A Validated Stability Indicating RP-HPLC Method for the Determination of Emtricitabine, Tenofovir Disoproxil Fumarate, Elvitegravir and Cobicistat in Pharmaceutical Dosage Form

PubMed Central

Runja, Chinnalalaiah; Ravi Kumar, Pigili; Avanapu, Srinivasa Rao

2016-01-01

A new simple, rapid stability indicating assay method has been developed and validated for the determination of emtricitabine, tenofovir disoproxil fumarate, elvitegravir and cobicistat using reverse-phase high-performance liquid chromatography in their pharmaceutical dosage form. The chromatographic separation was performed on an ODS column (250 × 4.6 mm, 5 µm) using mobile phase A (potassium dihydrogen orthophosphate, pH adjusted to 2.5) and mobile phase B (acetonitrile) in the ratio of 55:45% v/v at a flow rate of 1 mL/min. The analytes were detected at 250 nm. The method was found to be linear in the concentration range of 2–12 µg/mL for EMT, 3–18 µg/mL for TNDF, 1.5–9 µg/mL for ELV and COB, with the coefficient value (R2) of >0.9990. The accuracy was measured via recovery studies and found to be acceptable, and the percentage recoveries were found in the range of 99.93–100.08 ± 0.5%. Forced degradation studies were also conducted, and the drugs were subjected to various stress conditions such as acid hydrolysis, base hydrolysis, oxidative, photolytic and thermal degradation. The proposed method was successfully validated and applied for the quantitative estimation of these drugs in both bulk and tablet dosage forms. PMID:26865655

Preparation and stability evaluation of extemporaneous oral suspension of valsartan using commercially available tablets.

PubMed

Zaid, Abdel Naser; Assali, Mohyeddin; Qaddomi, Aiman; Ghanem, Mashhour; Zaaror, Yara Abu

2014-01-01

The aim of this study was to develop an extemporaneous valsartan suspension (80 mg valsartan/5 mL) starting from commercial tablets (80-mg/ tablet). A high-performance liquid chromatographic system was used for the analysis and quantification of valsartan in the samples studied. Samples of valsartan suspension for analysis were prepared as reported by the validated high-performance liquid chromatographic method and the dissolution tests were performed according to the U.S. Food and Drug Administration's method. The high-performance liquid chromatographic assay indicated that the 80-mg/5-mL valsartan suspension was stable for 30 days when stored at long-term and accelerated storage conditions. Valsartan release profile showed that approximately 85% of valsartan dissolved after 10 minutes and, accordingly, the calculation of similarity factor was not necessary. It is possible for the pharmacist to crush valsartan 80-mg tablets and prepare a suspension which has dosage flexibility that can be calculated according to body-surface area, kidney, and liver functions, without affecting the chemical stability of the active ingredient nor its dissolution profile and also have a cost-effective dosage form.

Analytical Method Validation of High-Performance Liquid Chromatography and Stability-Indicating Study of Medroxyprogesterone Acetate Intravaginal Sponges

PubMed Central

Batrawi, Nidal; Wahdan, Shorouq; Abualhasan, Murad

2017-01-01

Medroxyprogesterone acetate is widely used in veterinary medicine as intravaginal dosage for the synchronization of breeding cycle in ewes and goats. The main goal of this study was to develop reverse-phase high-performance liquid chromatography method for the quantification of medroxyprogesterone acetate in veterinary vaginal sponges. A single high-performance liquid chromatography/UV isocratic run was used for the analytical assay of the active ingredient medroxyprogesterone. The chromatographic system consisted of a reverse-phase C18 column as the stationary phase and a mixture of 60% acetonitrile and 40% potassium dihydrogen phosphate buffer as the mobile phase; the pH was adjusted to 5.6. The method was validated according to the International Council for Harmonisation (ICH) guidelines. Forced degradation studies were also performed to evaluate the stability-indicating properties and specificity of the method. Medroxyprogesterone was eluted at 5.9 minutes. The linearity of the method was confirmed in the range of 0.0576 to 0.1134 mg/mL (R2 > 0.999). The limit of quantification was shown to be 3.9 µg/mL. Precision and accuracy ranges were found to be %RSD <0.2 and 98% to 102%, respectively. Medroxyprogesterone capacity factor value of 2.1, tailing factor value of 1.03, and resolution value of 3.9 were obtained in accordance with ICH guidelines. Based on the obtained results, a rapid, precise, accurate, sensitive, and cost-effective analysis procedure was proposed for quantitative determination of medroxyprogesterone in vaginal sponges. This analytical method is the only available method to analyse medroxyprogesterone in veterinary intravaginal dosage form. PMID:28469407

Additional Evidence for the Reliability and Validity of the Student Risk Screening Scale at the High School Level: A Replication and Extension

ERIC Educational Resources Information Center

Lane, Kathleen Lynne; Oakes, Wendy P.; Ennis, Robin Parks; Cox, Meredith Lucille; Schatschneider, Christopher; Lambert, Warren

2013-01-01

This study reports findings from a validation study of the Student Risk Screening Scale for use with 9th- through 12th-grade students (N = 1854) attending a rural fringe school. Results indicated high internal consistency, test-retest stability, and inter-rater reliability. Predictive validity was established across two academic years, with Spring…

Development and validation of a stability-indicating capillary zone electrophoretic method for the assessment of entecavir and its correlation with liquid chromatographic methods.

PubMed

Dalmora, Sergio Luiz; Nogueira, Daniele Rubert; D'Avila, Felipe Bianchini; Souto, Ricardo Bizogne; Leal, Diogo Paim

2011-01-01

A stability-indicating capillary zone electrophoresis (CZE) method was validated for the analysis of entecavir in pharmaceutical formulations, using nimesulide as an internal standard. A fused-silica capillary (50 µm i.d.; effective length, 40 cm) was used while being maintained at 25°C; the applied voltage was 25 kV. A background electrolyte solution consisted of a 20 mM sodium tetraborate solution at pH 10. Injections were performed using a pressure mode at 50 mbar for 5 s, with detection at 216 nm. The specificity and stability-indicating capability were proven through forced degradation studies, evaluating also the in vitro cytotoxicity test of the degraded products. The method was linear over the concentration range of 1-200 µg mL(-1) (r(2) = 0.9999), and was applied for the analysis of entecavir in tablet dosage forms. The results were correlated to those of validated conventional and fast LC methods, showing non-significant differences (p > 0.05).

Synchrophasor-Assisted Prediction of Stability/Instability of a Power System

NASA Astrophysics Data System (ADS)

Saha Roy, Biman Kumar; Sinha, Avinash Kumar; Pradhan, Ashok Kumar

2013-05-01

This paper presents a technique for real-time prediction of stability/instability of a power system based on synchrophasor measurements obtained from phasor measurement units (PMUs) at generator buses. For stability assessment the technique makes use of system severity indices developed using bus voltage magnitude obtained from PMUs and generator electrical power. Generator power is computed using system information and PMU information like voltage and current phasors obtained from PMU. System stability/instability is predicted when the indices exceeds a threshold value. A case study is carried out on New England 10-generator, 39-bus system to validate the performance of the technique.

Development of an advanced pitch active control system for a wide body jet aircraft

NASA Technical Reports Server (NTRS)

Guinn, Wiley A.; Rising, Jerry J.; Davis, Walt J.

1984-01-01

An advanced PACS control law was developed for a commercial wide-body transport (Lockheed L-1011) by using modern control theory. Validity of the control law was demonstrated by piloted flight simulation tests on the NASA Langley visual motion simulator. The PACS design objective was to develop a PACS that would provide good flying qualities to negative 10 percent static stability margins that were equivalent to those of the baseline aircraft at a 15 percent static stability margin which is normal for the L-1011. Also, the PACS was to compensate for high-Mach/high-g instabilities that degrade flying qualities during upset recoveries and maneuvers. The piloted flight simulation tests showed that the PACS met the design objectives. The simulation demonstrated good flying qualities to negative 20 percent static stability margins for hold, cruise and high-speed flight conditions. Analysis and wind tunnel tests performed on other Lockheed programs indicate that the PACS could be used on an advanced transport configuration to provide a 4 percent fuel savings which results from reduced trim drag by flying at negative static stability margins.

Design of an unified chassis controller for rollover prevention, manoeuvrability and lateral stability

NASA Astrophysics Data System (ADS)

Yoon, Jangyeol; Yim, Seongjin; Cho, Wanki; Koo, Bongyeong; Yi, Kyongsu

2010-11-01

This paper describes a unified chassis control (UCC) strategy to prevent vehicle rollover and improve both manoeuvrability and lateral stability. Since previous researches on rollover prevention are only focused on the reduction of lateral acceleration, the manoeuvrability and lateral stability cannot be guaranteed. For this reason, it is necessary to design a UCC controller to prevent rollover and improve lateral stability by integrating electronic stability control, active front steering and continuous damping control. This integration is performed through switching among several control modes and a simulation is performed to validate the proposed method. Simulation results indicate that a significant improvement in rollover prevention, manoeuvrability and lateral stability can be expected from the proposed UCC system.

Degradation Kinetics Study of Alogliptin Benzoate in Alkaline Medium by Validated Stability-Indicating HPTLC Method.

PubMed

Bodiwala, Kunjan Bharatkumar; Shah, Shailesh; Thakor, Jeenal; Marolia, Bhavin; Prajapati, Pintu

2016-11-01

A rapid, sensitive, and stability-indicating high-performance thin-layer chromatographic method was developed and validated to study degradation kinetics of Alogliptin benzoate (ALG) in an alkaline medium. ALG was degraded under acidic, alkaline, oxidative, and thermal stress conditions. The degraded samples were chromatographed on silica gel 60F254-TLC plates, developed using a quaternary-solvent system (chloroform-methanol-ethyl acetate-triethyl amine, 9+1+1+0.5, v/v/v/v), and scanned at 278 nm. The developed method was validated per International Conference on Harmonization guidelines using validation parameters such as specificity, linearity and range, precision, accuracy, LOD, and LOQ. The linearity range for ALG was 100-500 ng/band (correlation coefficient = 0.9997) with an average recovery of 99.47%. The LOD and LOQ for ALG were 9.8 and 32.7 ng/band, respectively. The developed method was successfully applied for the quantitative estimation of ALG in its synthetic mixture with common excipients. Degradation kinetics of ALG in an alkaline medium was studied by degrading it under three different temperatures and three different concentrations of alkali. Degradation of ALG in the alkaline medium was found to follow first-order kinetics. Contour plots have been generated to predict degradation rate constant, half-life, and shelf life of ALG in various combinations of temperature and concentration of alkali using Design Expert software.

Stability of extemporaneously prepared preservative-free prochlorperazine nasal spray.

PubMed

Yellepeddi, Venkata K

2018-01-01

The stability of an extemporaneously prepared preservative-free prochlorperazine 5-mg/mL nasal spray was evaluated. The preservative-free prochlorperazine nasal spray was prepared by adding 250 mg of prochlorperazine edisylate to 50 mL of citrate buffer in a low-density polyethylene nasal spray bottle. A stability-indicating high-performance liquid chromatography (HPLC) method was developed and validated using the major degradant prochlorperazine sulfoxide and by performing forced-degradation studies. For chemical stability studies, 3 100-μL samples of the preservative-free prochlorperazine from 5 nasal spray bottles stored at room temperature were collected at days 0, 20, 30, 45, and 60 and were assayed in triplicate using the stability-indicating HPLC method. Microbiological testing involved antimicrobial effectiveness testing based on United States Pharmacopeia ( USP ) chapter 51 and quantitative microbiological enumeration of aerobic bacteria, yeasts, and mold based on USP chapter 61. Samples for microbiological testing were collected at days 0, 30, and 60. The stability-indicating HPLC method clearly identified the degradation product prochlorperazine sulfoxide without interference from prochlorperazine. All tested solutions retained over 90% of the initial prochlorperazine concentration for the 60-day study period. There were no detectable changes in color, pH, and viscosity in any sample. There was no growth of bacteria, yeast, and mold for 60 days in all samples tested. An extemporaneously prepared preservative-free nasal spray solution of prochlorperazine edisylate 5 mg/mL was physically, chemically, and microbiologically stable for 60 days when stored at room temperature in low-density polyethylene bottles. Copyright © 2018 by the American Society of Health-System Pharmacists, Inc. All rights reserved.

Development and Validation of High Precision Thermal, Mechanical, and Optical Models for the Space Interferometry Mission

NASA Technical Reports Server (NTRS)

Lindensmith, Chris A.; Briggs, H. Clark; Beregovski, Yuri; Feria, V. Alfonso; Goullioud, Renaud; Gursel, Yekta; Hahn, Inseob; Kinsella, Gary; Orzewalla, Matthew; Phillips, Charles

2006-01-01

SIM Planetquest (SIM) is a large optical interferometer for making microarcsecond measurements of the positions of stars, and to detect Earth-sized planets around nearby stars. To achieve this precision, SIM requires stability of optical components to tens of picometers per hour. The combination of SIM s large size (9 meter baseline) and the high stability requirement makes it difficult and costly to measure all aspects of system performance on the ground. To reduce risks, costs and to allow for a design with fewer intermediate testing stages, the SIM project is developing an integrated thermal, mechanical and optical modeling process that will allow predictions of the system performance to be made at the required high precision. This modeling process uses commercial, off-the-shelf tools and has been validated against experimental results at the precision of the SIM performance requirements. This paper presents the description of the model development, some of the models, and their validation in the Thermo-Opto-Mechanical (TOM3) testbed which includes full scale brassboard optical components and the metrology to test them at the SIM performance requirement levels.

Development and validation of a stability-indicating RP-HPLC method for assay of betamethasone and estimation of its related compounds.

PubMed

Fu, Qiang; Shou, Minshan; Chien, Dwight; Markovich, Robert; Rustum, Abu M

2010-02-05

Betamethasone (9alpha-fluoro-16beta-methylprednisolone) is one of the members of the corticosteriod family of active pharmaceutical ingredient (API), which is widely used as an anti-inflammatory agent and also as a starting material to manufacture various esters of betamethasone. A stability-indicating reverse-phase high performance liquid chromatography (RP-HPLC) method has been developed and validated which can separate and accurately quantitate low levels of 26 betamethasone related compounds. The stability-indicating capability of the method was demonstrated through adequate separation of all potential betamethasone related compounds from betamethasone and also from each other that are present in aged and stress degraded betamethasone stability samples. Chromatographic separation of betamethasone and its related compounds was achieved by using a gradient elution at a flow rate of 1.0mL/min on a ACE 3 C18 column (150mmx4.6mm, 3microm particle size, 100A pore size) at 40 degrees C. Mobile phase A of the gradient was 0.1% methanesulfonic acid in aqueous solution and mobile phase B was a mixture of tert-butanol and 1,4-dioxane (7:93, v/v). UV detection at 254nm was employed to monitor the analytes. For betamethasone 21-aldehyde, the QL and DL were 0.02% and 0.01% respectively. For betamethasone and the rest of the betamethasone related compounds, the QL and DL were 0.05% and 0.02%. The precision of betamethasone assay is 0.6% and the accuracy of betamethasone assay ranged from 98.1% to 99.9%.

Development and validation of a rapid stability indicating HPLC-method using monolithic stationary phase and two spectrophotometric methods for determination of antihistaminic acrivastine in capsules

NASA Astrophysics Data System (ADS)

Gouda, Ayman A.; Hashem, Hisham; Jira, Thomas

2014-09-01

Simple, rapid and accurate high performance liquid chromatographic (HPLC) and spectrophotometric methods are described for determination of antihistaminic acrivastine in capsules. The first method (method A) is based on accurate, sensitive and stability indicating chromatographic separation method. Chromolith® Performance RP-18e column, a relatively new packing material consisting of monolithic rods of highly porous silica, was used as stationary phase applying isocratic binary mobile phase of ACN and 25 mM NaH2PO4 pH 4.0 in the ratio of 22.5:77.5 at flow rate of 5.0 mL/min and 40 °C. A diode array detector was used at 254 nm for detection. The elution time of acrivastine was found to be 2.080 ± 0.032. The second and third methods (methods B and C) are based on the oxidation of acrivastine with excess N-bromosuccinimide (NBS) and determination of the unconsumed NBS with, metol-sulphanilic acid (λmax: 520 nm) or amaranth dye (λmax: 530 nm). The reacted oxidant corresponds to the drug content. Beer’s law is obeyed over the concentration range 1.563-50, 2.0-20 and 1.0-10 μg mL-1 for methods A, B and C, respectively. The limits of detection and quantitation were 0.40, 0.292 and 0.113 μg mL-1 and 0.782, 0.973 and 0.376 μg mL-1 for methods A, B and C, respectively. The HPLC method was validated for system suitability, linearity, precision, limits of detection and quantitation, specificity, stability and robustness. Stability tests were done through exposure of the analyte solution for four different stress conditions and the results indicate no interference of degradants with HPLC-method. The proposed methods was favorably applied for determination of acrivastine in capsules formulation. Statistical comparison of the obtained results from the analysis of the studied drug to those of the reported method using t- and F-tests showed no significant difference between them.

Development and validation of a stability-indicating high performance liquid chromatographic assay for benoxinate.

PubMed

Chorny, Michael; Levy, Daniel; Schumacher, Ilana; Lichaa, Chaim; Gruzman, Boris; Livshits, Oleg; Lomnicky, Yossi

2003-04-24

Benoxinate is a local anaesthetic used for ophthalmic applications. The aim of this study was to develop a rapid and simple stability-indicating method for the determination of benoxinate formulated for ophthalmic use, evaluate its long-term stability and identify its major degradation product. Benoxinate was eluted on a 10 microm Spherisorb phenyl column, 250 x 3.2 mm, with a mobile phase consisting of acetonitrile-buffer (pH 3.5) (35:65, v/v), pumped at 0.8 ml min(-1) flow rate. The buffer was composed of sodium dihydrogen phosphate (50 mM), sodium hydrogen sulfate (2.5 mM) and 1-heptanesulfonic acid sodium salt (5 mM). The analyte was quantified spectrophotometrically at 308 nm. The chromatograms of benoxinate formulations obtained by this method showed benoxinate (t = 4.5 min) well resolved from its degradation product (t = 2.3 min), which was separately identified by means of HPLC-MS as 4-amino-3-butoxybenzoic acid. The assay was demonstrated to have high accuracy, precision and linearity. The method was implemented in investigating the long-term stability of benoxinate 0.4% ophthalmic solutions. The method was found to be simple, quick and selective in determining benoxinate concentrations in fresh and aged preparations.

Rank Order Entropy: why one metric is not enough

PubMed Central

McLellan, Margaret R.; Ryan, M. Dominic; Breneman, Curt M.

2011-01-01

The use of Quantitative Structure-Activity Relationship models to address problems in drug discovery has a mixed history, generally resulting from the mis-application of QSAR models that were either poorly constructed or used outside of their domains of applicability. This situation has motivated the development of a variety of model performance metrics (r2, PRESS r2, F-tests, etc) designed to increase user confidence in the validity of QSAR predictions. In a typical workflow scenario, QSAR models are created and validated on training sets of molecules using metrics such as Leave-One-Out or many-fold cross-validation methods that attempt to assess their internal consistency. However, few current validation methods are designed to directly address the stability of QSAR predictions in response to changes in the information content of the training set. Since the main purpose of QSAR is to quickly and accurately estimate a property of interest for an untested set of molecules, it makes sense to have a means at hand to correctly set user expectations of model performance. In fact, the numerical value of a molecular prediction is often less important to the end user than knowing the rank order of that set of molecules according to their predicted endpoint values. Consequently, a means for characterizing the stability of predicted rank order is an important component of predictive QSAR. Unfortunately, none of the many validation metrics currently available directly measure the stability of rank order prediction, making the development of an additional metric that can quantify model stability a high priority. To address this need, this work examines the stabilities of QSAR rank order models created from representative data sets, descriptor sets, and modeling methods that were then assessed using Kendall Tau as a rank order metric, upon which the Shannon Entropy was evaluated as a means of quantifying rank-order stability. Random removal of data from the training set, also known as Data Truncation Analysis (DTA), was used as a means for systematically reducing the information content of each training set while examining both rank order performance and rank order stability in the face of training set data loss. The premise for DTA ROE model evaluation is that the response of a model to incremental loss of training information will be indicative of the quality and sufficiency of its training set, learning method, and descriptor types to cover a particular domain of applicability. This process is termed a “rank order entropy” evaluation, or ROE. By analogy with information theory, an unstable rank order model displays a high level of implicit entropy, while a QSAR rank order model which remains nearly unchanged during training set reductions would show low entropy. In this work, the ROE metric was applied to 71 data sets of different sizes, and was found to reveal more information about the behavior of the models than traditional metrics alone. Stable, or consistently performing models, did not necessarily predict rank order well. Models that performed well in rank order did not necessarily perform well in traditional metrics. In the end, it was shown that ROE metrics suggested that some QSAR models that are typically used should be discarded. ROE evaluation helps to discern which combinations of data set, descriptor set, and modeling methods lead to usable models in prioritization schemes, and provides confidence in the use of a particular model within a specific domain of applicability. PMID:21875058

Machine Learning methods for Quantitative Radiomic Biomarkers.

PubMed

Parmar, Chintan; Grossmann, Patrick; Bussink, Johan; Lambin, Philippe; Aerts, Hugo J W L

2015-08-17

Radiomics extracts and mines large number of medical imaging features quantifying tumor phenotypic characteristics. Highly accurate and reliable machine-learning approaches can drive the success of radiomic applications in clinical care. In this radiomic study, fourteen feature selection methods and twelve classification methods were examined in terms of their performance and stability for predicting overall survival. A total of 440 radiomic features were extracted from pre-treatment computed tomography (CT) images of 464 lung cancer patients. To ensure the unbiased evaluation of different machine-learning methods, publicly available implementations along with reported parameter configurations were used. Furthermore, we used two independent radiomic cohorts for training (n = 310 patients) and validation (n = 154 patients). We identified that Wilcoxon test based feature selection method WLCX (stability = 0.84 ± 0.05, AUC = 0.65 ± 0.02) and a classification method random forest RF (RSD = 3.52%, AUC = 0.66 ± 0.03) had highest prognostic performance with high stability against data perturbation. Our variability analysis indicated that the choice of classification method is the most dominant source of performance variation (34.21% of total variance). Identification of optimal machine-learning methods for radiomic applications is a crucial step towards stable and clinically relevant radiomic biomarkers, providing a non-invasive way of quantifying and monitoring tumor-phenotypic characteristics in clinical practice.

Validated stability-indicating densitometric thin-layer chromatography: application to stress degradation studies of minocycline.

PubMed

Jain, Nilu; Jain, Gaurav Kumar; Ahmad, Farhan Jalees; Khar, Roop Krishen

2007-09-19

A simple, stability-indicating high-performance thin-layer liquid chromatographic (HPTLC) method for analysis of minocycline was developed and validated. The densitometric analysis was carried out at 345 nm using methanol-acetonitrile-isopropyl alcohol-water (5:4:0.5:0.5, v/v/v/v) as mobile phase. The method employed TLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase. To achieve good result, plates were sprayed with a 10% (w/v) solution of disodium ethylene diaminetetraacetic acid (EDTA), the pH of which was adjusted to 9.0. Compact spots of minocycline were found at R(f) = 0.30+/-0.02. For proposed procedure, linearity (r = 0.9997), limit of detection (3.7 ng spot(-1)), recovery (99.23-100.16%), and precision (% R.S.D. < or = 0.364) was found to be satisfactory. The drug undergoes acidic and basic degradation, oxidation and photodegradation. All the peaks of degradation products were well resolved from the pure drug with significantly different R(f) values. The acidic and alkaline degradation kinetics of minocycline, evaluated using this method, is found to be of first order.

Stability of Prednisone in Oral Mix Suspending Vehicle.

PubMed

Friciu, Mihaela; Plourde, Kevin; Leclair, Grégoire; Danopoulos, Panagiota; Savji, Taslim

2015-01-01

The stability of prednisone (5 mg/mL) formulated as a suspension in Oral Mix vehicle was evaluated. Oral Mix is a novel oral, dye-free suspending vehicle developed by Medisca Pharmaceutique Inc. for preparation of extemporaneous dosage forms. This drug was chosen based on its high frequency of prescription among the pediatric population. Suspensions were prepared from both pure active and commercial tablets utilizing two different container closures: amber glass bottles and polypropylene syringes (PreciseDose Dispenser Medisca Pharmaceutique Inc.). Formulations were stored at 5°C or 25°C and organoleptic properties, pH, and concentration were evaluated at predetermined time points up to 90 days. Validated stability-indicating high-performance liquid chromatography methods were developed. Beyond-use date was evaluated by statistical analysis of the overall degradation trend. Prednisone was stable for at least 90 days at 25°C. No changes in organoleptic properties or pH were observed for either of the formulations, and the global stability was roughly equivalent and sometimes superior to the stability of the same drugs in other previously used vehicles. Thus, Oral Mix was found to be a suitable dye-free vehicle for extemporaneous formulations.

A novel adaptive finite time controller for bilateral teleoperation system

NASA Astrophysics Data System (ADS)

Wang, Ziwei; Chen, Zhang; Liang, Bin; Zhang, Bo

2018-03-01

Most bilateral teleoperation researches focus on the system stability within time-delays. However, practical teleoperation tasks require high performances besides system stability, such as convergence rate and accuracy. This paper investigates bilateral teleoperation controller design with transient performances. To ensure the transient performances and system stability simultaneously, an adaptive non-singular fast terminal mode controller is proposed to achieve practical finite-time stability considering system uncertainties and time delays. In addition, a novel switching scheme is introduced, in which way the singularity problem of conventional terminal sliding manifold is avoided. Finally, numerical simulations demonstrate the effectiveness and validity of the proposed method.

A validated stability-indicating RP-HPLC method for levofloxacin in the presence of degradation products, its process related impurities and identification of oxidative degradant.

PubMed

Lalitha Devi, M; Chandrasekhar, K B

2009-12-05

The objective of current study was to develop a validated specific stability indicating reversed-phase liquid chromatographic method for the quantitative determination of levofloxacin as well as its related substances determination in bulk samples, pharmaceutical dosage forms in the presence of degradation products and its process related impurities. Forced degradation studies were performed on bulk sample of levofloxacin as per ICH prescribed stress conditions using acid, base, oxidative, water hydrolysis, thermal stress and photolytic degradation to show the stability indicating power of the method. Significant degradation was observed during oxidative stress and the degradation product formed was identified by LCMS/MS, slight degradation in acidic stress and no degradation was observed in other stress conditions. The chromatographic method was optimized using the samples generated from forced degradation studies and the impurity spiked solution. Good resolution between the peaks corresponds to process related impurities and degradation products from the analyte were achieved on ACE C18 column using the mobile phase consists a mixture of 0.5% (v/v) triethyl amine in sodium dihydrogen orthophosphate dihydrate (25 mM; pH 6.0) and methanol using a simple linear gradient. The detection was carried out at 294 nm. The limit of detection and the limit of quantitation for the levofloxacin and its process related impurities were established. The stressed test solutions were assayed against the qualified working standard of levofloxacin and the mass balance in each case was in between 99.4 and 99.8% indicating that the developed LC method was stability indicating. Validation of the developed LC method was carried out as per ICH requirements. The developed LC method was found to be suitable to check the quality of bulk samples of levofloxacin at the time of batch release and also during its stability studies (long term and accelerated stability).

UPLC and LC-MS studies on degradation behavior of irinotecan hydrochloride and development of a validated stability-indicating ultra-performance liquid chromatographic method for determination of irinotecan hydrochloride and its impurities in pharmaceutical dosage forms.

PubMed

Kumar, Navneet; Sangeetha, Dhanaraj; Reddy, Sunil P

2012-10-01

The objective of the current investigation was to study the degradation behavior of irinotecan hydrochloride under different International Conference on Harmonization (ICH) recommended stress conditions using ultra-performance liquid chromatography and liquid chromatography-mass spectrometry and to establish a validated stability-indicating reverse-phase ultra-performance liquid chromatographic method for the quantitative determination of irinotecan hydrochloride and its seven impurities and degradation products in pharmaceutical dosage forms. Irinotecan hydrochloride was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Irinotecan hydrochloride was found to degrade significantly in oxidative and base hydrolysis and photolytic degradation conditions. The degradation products were well resolved from the main peak and its impurities, thus proving the stability-indicating power of the method. Chromatographic separation was achieved on a Waters Acquity BEH C8 (100 × 2.1 mm) 1.7-µm column with a mobile phase containing a gradient mixture of solvent A (0.02M KH(2)PO(4) buffer, pH 3.4) and solvent B (a mixture of acetonitrile and methanol in the ratio of 62:38 v/v). The mobile phase was delivered at a flow rate of 0.3 mL/min with ultraviolet detection at 220 nm. The run time was 8 min, within which irinotecan and its seven impurities and degradation products were satisfactorily separated. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness. This method was also suitable for the assay determination of irinotecan hydrochloride in pharmaceutical dosage forms.

A validated stability-indicating UPLC method for desloratadine and its impurities in pharmaceutical dosage forms.

PubMed

Rao, Dantu Durga; Satyanarayana, N V; Malleswara Reddy, A; Sait, Shakil S; Chakole, Dinesh; Mukkanti, K

2010-02-05

A novel stability-indicating gradient reverse phase ultra-performance liquid chromatographic (RP-UPLC) method was developed for the determination of purity of desloratadine in presence of its impurities and forced degradation products. The method was developed using Waters Aquity BEH C18 column with mobile phase containing a gradient mixture of solvents A and B. The eluted compounds were monitored at 280nm. The run time was 8min within which desloratadine and its five impurities were well separated. Desloratadine was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Desloratadine was found to degrade significantly in oxidative and thermal stress conditions and stable in acid, base, hydrolytic and photolytic degradation conditions. The degradation products were well resolved from main peak and its impurities, thus proved the stability-indicating power of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness. This method was also suitable for the assay determination of desloratadine in pharmaceutical dosage forms.

Psychometric properties of the motor diagnostics in the German football talent identification and development programme.

PubMed

HÖner, Oliver; Votteler, Andreas; Schmid, Markus; Schultz, Florian; Roth, Klaus

2015-01-01

The utilisation of motor performance tests for talent identification in youth sports is discussed intensively in talent research. This article examines the reliability, differential stability and validity of the motor diagnostics conducted nationwide by the German football talent identification and development programme and provides reference values for a standardised interpretation of the diagnostics results. Highly selected players (the top 4% of their age groups, U12-U15) took part in the diagnostics at 17 measurement points between spring 2004 and spring 2012 (N = 68,158). The heterogeneous test battery measured speed abilities and football-specific technical skills (sprint, agility, dribbling, ball control, shooting, juggling). For all measurement points, the overall score and the speed tests showed high internal consistency, high test-retest reliability and satisfying differential stability. The diagnostics demonstrated satisfying factorial-related validity with plausible and stable loadings on the two empirical factors "speed" and "technical skills". The score, and the technical skills dribbling and juggling, differentiated the most among players of different performance levels and thus showed the highest criterion-related validity. Satisfactory psychometric properties for the diagnostics are an important prerequisite for a scientifically sound rating of players' actual motor performance and for the future examination of the prognostic validity for success in adulthood.

Stability of cyclophosphamide in extemporaneous oral suspensions.

PubMed

Kennedy, Rachel; Groepper, Daniel; Tagen, Michael; Christensen, Robbin; Navid, Fariba; Gajjar, Amar; Stewart, Clinton F

2010-02-01

Cyclophosphamide, an alkylating agent, is widely used for the treatment of many adult and pediatric malignancies. The stability of cyclophosphamide in aqueous- and methylcellulose-based oral suspending vehicles is currently unknown. To develop and validate a stability-indicating high-performance liquid chromatography (HPLC) method to measure cyclophosphamide concentrations in simple syrup and Ora-Plus, and assess the 56-day chemical stability and physical appearance of cyclophosphamide in these suspensions at both room temperature (22 degrees C) and 4 degrees C. The intravenous formulation of cyclophosphamide was diluted to 20 mg/mL in NaCl 0.9%, compounded 1:1 with either suspending vehicle, and stored in the dark in 3-mL amber polypropylene oral syringes at 4 degrees C and 22 degrees C. Aliquots from each syringe were obtained on days 0, 3, 7, 14, 21, 28, 35, 42, 49, and 56 and assayed using the validated stability-indicating HPLC-UV method. A C18 analytical column was used to separate cyclophosphamide from the internal standard, ifosfamide, with a mobile phase of 21% acetonitrile in 79% sodium phosphate buffer. The suspension was examined for odor change, visually examined under normal fluorescent light for color change, and examined under a light microscope for evidence of microbial growth. Samples of cyclophosphamide in both simple syrup and Ora-Plus were stable when kept at 4 degrees C for at least 56 days. At room temperature, cyclophosphamide in simple syrup and Ora-Plus had a shelf life of 8 and 3 days, respectively. No changes in color or odor or evidence of microbial growth were observed. Cyclophosphamide can be extemporaneously prepared in simple syrup or Ora-Plus and stored for at least 2 months under refrigeration without significant degradation.

High-performance liquid chromatographic method optimization for ondansetron assay in extemporaneous topical gel and in marketed products.

PubMed

Quamrun, Masuda; Mamoon, Rashid; Nasheed, Shams; Randy, Mullins

2014-01-01

The compounding and evaluation of ondansetron hydrochloride dihydrate topical gel, 2.5% w/w, were conducted in this study. The gelling agent was Carbopol 940. Ethanol 70% in purified water was used to dissolve the drug and disperse the gelling agent. A gel was formed by adding drops of 0.1 N sodium hydroxide solution. To assay this gel, we developed a simple and reproducible stability--indicating high-performance liquid chromatographic method. This method was validated for specificity, accuracy, and precision. The compounded gel was assayed in triplicate, and the average recovery was 98.3%. Ondansetron marketed products were analyzed for comparison with the compounded formulation. Assay, accuracy, and precision data of the compounded topical gel were comparable to the marketed products.

Subjective sleepiness is a sensitive indicator of insufficient sleep and impaired waking function.

PubMed

Akerstedt, Torbjörn; Anund, Anna; Axelsson, John; Kecklund, Göran

2014-06-01

The main consequence of insufficient sleep is sleepiness. While measures of sleep latency, continuous encephalographical/electro-oculographical (EEG/EOG) recording and performance tests are useful indicators of sleepiness in the laboratory and clinic, they are not easily implemented in large, real-life field studies. Subjective ratings of sleepiness, which are easily applied and unobtrusive, are an alternative, but whether they measure sleepiness sensitively, reliably and validly remains uncertain. This review brings together research relevant to these issues. It is focused on the Karolinska Sleepiness Scale (KSS), which is a nine-point Likert-type scale. The diurnal pattern of sleepiness is U-shaped, with high KSS values in the morning and late evening, and with great stability across years. KSS values increase sensitively during acute total and repeated partial sleep deprivation and night work, including night driving. The effect sizes range between 1.5 and 3. The relation to driving performance or EEG/EOG indicators of sleepiness is highly significant, strongly curvilinear and consistent across individuals. High (>6) KSS values are associated particularly with impaired driving performance and sleep intrusions in the EEG. KSS values are also increased in many clinical conditions such as sleep apnea, depression and burnout. The context has a strong influence on KSS ratings. Thus, physical activity, social interaction and light exposure will reduce KSS values by 1-2 units. In contrast, time-on-task in a monotonous context will increase KSS values by 1-2 units. In summary, subjective ratings of sleepiness as described here is as sensitive and valid an indicator of sleepiness as objective measures, and particularly suitable for field studies. © 2014 European Sleep Research Society.

A validated specific stability-indicating RP-HPLC assay method for Ambrisentan and its related substances.

PubMed

Narayana, M B V; Chandrasekhar, K B; Rao, B M

2014-09-01

A validated specific stability-indicating reverse-phase liquid chromatographic method was developed for the quantitative determination of Ambrisentan as well as its related substances in bulk samples, pharmaceutical dosage forms in the presence of degradation products and its related impurities. Forced degradation studies were performed on bulk samples of Ambrisentan as per the ICH-prescribed stress conditions using acid, base, oxidative, thermal stress and photolytic degradation to show the stability-indicating power of the LC method. Significant degradation in acidic, basic stress conditions was observed and no degradation was observed in other stress conditions. The chromatographic method was optimized using the samples generated from the forced degradation studies and the impurity-spiked solution. Good resolution between the peaks corresponds to Ambrisentan-related impurities and degradation products from the analyte were achieved on a SunFire C18 column using a mobile phase consisting of a mixture of potassium dihydrogen orthophosphate at a pH adjusted to 2.5 with ortho-phosphoric acid in water and a mixture of acetonitrile:methanol using a simple linear gradient. The detection was carried out at 225 nm. The limit of detection and the limit of quantification for the Ambrisentan and its related impurities were established. The stressed test solutions were assayed against the qualified working standard of Ambrisentan and the mass balance in each case was between 98.9 and 100.3%, indicating that the developed LC method was stability indicating. Validation of the developed LC method was carried out as per the ICH requirements. The developed method was found to be suitable to check the quality of bulk samples of Ambrisentan at the time of batch release and also during its storage (long-term and accelerated stability). © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Development of RP-HPLC, Stability Indicating Method for Degradation Products of Linagliptin in Presence of Metformin HCl by Applying 2 Level Factorial Design; and Identification of Impurity-VII, VIII and IX and Synthesis of Impurity-VII.

PubMed

Jadhav, Sushant B; Reddy, P Sunil; Narayanan, Kalyanaraman L; Bhosale, Popatrao N

2017-06-27

The novel reverse phase-high performance liquid chromatography (RP-HPLC), stability indicating method was developed for determination of linagliptin (LGP) and its related substances in linagliptin and metformin HCl (MET HCl) tablets by implementing design of experiment to understand the critical method parameters and their relation with critical method attributes; to ensure robustness of the method. The separation of nine specified impurities was achieved with a Zorbax SB-Aq 250 × 4.6 mm, 5 µm column, using gradient elution and a detector wavelength of 225 nm, and validated in accordance with International Conference on Harmonization (ICH) guidelines and found to be accurate, precise, reproducible, robust, and specific . The drug was found to be degrading extensively in heat, humidity, basic, and oxidation conditions and was forming degradation products during stability studies. After slight modification in the buffer and the column, the same method was used for liquid chromatography-mass spectrometry (LC-MS) and ultra-performance liquid chromatography -time-of-flight/mass spectrometry UPLC-TOF/MS analysis, to identify m/z and fragmentation of maximum unspecified degradation products i.e., Impurity-VII ( 7 ), Impurity-VIII ( 8 ), and Impurity-IX ( 9 ) formed during stability studies. Based on the results, a degradation pathway for the drug has been proposed and synthesis of Impurity-VII ( 7 ) is also discussed to ensure an in-depth understanding of LGP and its related degradation products and optimum performance during the lifetime of the product.

The teamwork in assertive community treatment (TACT) scale: development and validation.

PubMed

Wholey, Douglas R; Zhu, Xi; Knoke, David; Shah, Pri; Zellmer-Bruhn, Mary; Witheridge, Thomas F

2012-11-01

Team design is meticulously specified for assertive community treatment (ACT) teams, yet performance can vary across ACT teams, even those with high fidelity. By developing and validating the Teamwork in Assertive Community Treatment (TACT) scale, investigators examined the role of team processes in ACT performance. The TACT scale measuring ACT teamwork was developed from a conceptual model grounded in organizational research and adapted for the ACT and mental health context. TACT subscales were constructed after exploratory and confirmatory factor analyses. The reliability, discriminant validity, predictive validity, temporal stability, internal consistency, and within-team agreement were established with surveys from approximately 300 members of 26 Minnesota ACT teams who completed the questionnaire three times, at six-month intervals. Nine TACT subscales emerged from the analyses: exploration, exploitation of new and existing knowledge, psychological safety, goal agreement, conflict, constructive controversy, information accessibility, encounter preparedness, and consumer-centered care. These nine subscales demonstrated fit and temporal stability (confirmatory factor analysis), high internal consistency (Cronbach's alpha), and within-team agreement and between-team differences (rwg and intraclass correlations). Correlational analyses of the subscales revealed that they measure related yet distinctive aspects of ACT team processes, and regression analyses demonstrated predictive validity (encounter preparedness is related to staff outcomes). The TACT scale demonstrated high reliability and validity and can be included in research and evaluation of teamwork in ACT and mental health teams.

Physicochemical and microbiological stability of azathioprine in InOrpha suspending agent studied under various conditions.

PubMed

Amin, Alexandre; Bourget, Philippe; Vidal, Fabrice; Cartier, François; Beauvais, Raphaëlle; Afonso, Veronica Do Nascimento

2015-01-01

Azathioprine is an antineoplastic antimetabolite drug currently used as an immunosuppressive agent after organ transplantation and for several dysimmunitary diseases. The usual daily dose ranges from 1 to 5 mg/kg orally. Azathioprine is marketed in France under the trade name Imurel in tablet form for oral administration that contains either 25 mg or 50 mg of the active ingredient. This Galenic formulation is not suitable for pediatric use and often requires a grinding operation or a dose fractionation to facilitate administration. In addition to a potential risk of imprecision in the administered dose, tablet grinding might unnecessarily expose nurses and families to a toxic compound. To overcome this problem, the objective of this study was to develop and evaluate the physicochemical and microbiological stabilities of azathioprine in a sugar-free, alcohol-free, and paraben-free InOrpha suspending agent. The studied samples were formulated into a 10-mg/mL suspension and stored in 24 plastic bottles of 60 mL at two different temperature conditions (between 2 degrees C to 8 degrees C and room temperature). Two series of 12 samples were tested for physicochemical stability using high-performance liquid chromatography as well as for a microbiological status for 35 days (daily opening of the bottles from day 0 of compounding) and for 56 days, upon daily flask opening (first opening at day 28 from compounding and daily opening for 28 consecutive days). The high-performance liquid chromatography method developed is linear, accurate, precise, and robust. In addition, a forced degradation study validated the selectivity and the specificity requirements of the method validated as stability indicating. At room temperature storage, high-performance liquid chromatography analysis showed that tested samples had concentrations ranging from 90% to 110% of the initial concentration throughout the course of the study. Microbiological status remained stable during the 56 days of investigation. Based on the data collected, the study led to the development of a new Galenic formulation of azathioprine that is suitable for pediatric use and can be safely stored at room temperature for 28 days (before and after opening for a maximum of 56 consecutive days).

Simultaneous determination of some water-soluble vitamins and preservatives in multivitamin syrup by validated stability-indicating high-performance liquid chromatography method.

PubMed

Vidović, Stojanka; Stojanović, Biljana; Veljković, Jelena; Prazić-Arsić, Ljiljana; Roglić, Goran; Manojlović, Dragan

2008-08-22

HPLC stability-indicating method has been developed for the simultaneous determination of some water-soluble vitamins (ascorbic acid, thiamine hydrochloride, riboflavin-5'-phosphate sodium, pyridoxine hydrochloride, nicotinamide, D(+)-panthenol) and two preservatives (methylparaben and sodium benzoate) in multivitamin syrup preparation. Water-soluble vitamins, preservatives and their degradants were separated on Zorbax SB-Aq (C(18)) (250 mm x 4.6 mm, 5 microm) column at an ambient temperature. Combined isocratic and gradient elution was performed with a mobile phase consisting of 0.0125 M hexane-1-sulfonic acid sodium salt in 0.1% (m/v) o-phosphoric acid, pH 2.4-2.5 (solvent A) and acetonitrile (solvent B) at the flow-rate 1 ml min(-1). Starting with solvent A an isocratic elution was performed for 15 min, then the composition was changed to 85% of A and 15% of B during the next 20 min and it was constant for 5 min, then the composition was changed to 70% of A and 30% of B during next 15 min and it was constant for 5 min and finally was changed to 100% of A as at the beginning of the elution. Detection was performed with diode array detector at 210, 230 and 254 nm. Multivitamin syrup preparation was subjected to stress testing (forced degradation) in order to demonstrate that degradants from the vitamins, preservatives and/or product excipients do not interfere with the quantification of vitamins and preservatives. Typical validation characteristics: selectivity, accuracy, precision, linearity, range, limit of quantification and limit of detection were evaluated for vitamins and preservatives.

Storage stability study of porcine hepatic and intestinal cytochrome P450 isoenzymes by use of a newly developed and fully validated highly sensitive HPLC-MS/MS method.

PubMed

Schelstraete, Wim; Devreese, Mathias; Croubels, Siska

2018-02-01

Microsomes are an ideal medium to investigate cytochrome P450 (CYP450) enzyme-mediated drug metabolism. However, before microsomes are prepared, tissues can be stored for a long time. Studies about the stability of these enzymes in porcine hepatic and intestinal tissues upon storage are lacking. To be able to investigate CYP450 stability in microsomes prepared from these tissues, a highly sensitive and rapid HPLC-MS/MS method for the simultaneous determination of six CYP450 metabolites in incubation medium was developed and validated. The metabolites, paracetamol (CYP1A), 7-hydroxy-coumarin (CYP2A), 1-hydroxy-midazolam (CYP3A), 4-hydroxy-tolbutamide (CYP2C), dextrorphan (CYP2D), and 6-hydroxy-chlorzoxazone (CYP2E) were extracted with ethyl acetate at pH 1.0, followed by evaporation and separation on an Agilent Zorbax Eclipse Plus C18 column. The method was fully validated in a GLP-compliant laboratory according to European guidelines and was highly sensitive (LOQ = 0.25-2.5 ng/mL), selective, had good precision (RSD-within, 1.0-9.1%; RSD-between, 1.0-18.4%) and accuracy (within-run, 83.3-102%; between-run, 78.5-102%), and showed no relative signal suppression and enhancement. Consequently, this method was applied to study the stability of porcine hepatic and intestinal CYP450 isoenzymes when tissues were stored at - 80 °C. The results indicate that porcine CYP450 isoenzymes are stable in tissues at least up to 4 months when snap frozen and stored at - 80 °C. Moreover, the results indicate differences in porcine CYP450 stability compared to rat, rabbit, and fish CYP450, as observed by other research groups, hence stressing the importance to investigate the CYP450 stability of a specific species.

Application of a validated stability-indicating densitometric thin-layer chromatographic method to stress degradation studies on moxifloxacin.

PubMed

Motwani, Sanjay K; Khar, Roop K; Ahmad, Farhan J; Chopra, Shruti; Kohli, K; Talegaonkar, S

2007-01-16

A simple, sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for densitometric determination of moxifloxacin both as a bulk drug and from pharmaceutical formulation was developed and validated as per the International Conference on Harmonization (ICH) guidelines. The method employed TLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase and the mobile phase consisted of n-propanol-ethanol-6M ammonia solution (4:1:2, v/v/v). Densitometric analysis of moxifloxacin was carried out in the absorbance mode at 298 nm. Compact spots for moxifloxacin were found at R(f) value of 0.58+/-0.02. The linear regression analysis data for the calibration plots showed good linear relationship with r=0.9925 in the working concentration range of 100-800 ng spot(-1). The method was validated for precision, accuracy, ruggedness, robustness, specificity, recovery, limit of detection (LOD) and limit of quantitation (LOQ). The LOD and LOQ were 3.90 and 11.83 ng spot(-1), respectively. Drug was subjected to acid and alkali hydrolysis, oxidation, dry heat, wet heat treatment and photodegradation. All the peaks of degradation products were well resolved from the standard drug with significantly different R(f) values. Statistical analysis proves that the developed HPTLC method is reproducible and selective. As the method could effectively separate the drug from its degradation products, it can be employed as stability-indicating one. Moreover, the proposed HPTLC method was utilized to investigate the kinetics of the acidic and alkaline degradation processes at different temperatures. Arrhenius plot was constructed and apparent pseudo-first-order rate constant, half-life and activation energy were calculated. In addition the pH-rate profile for degradation of moxifloxacin in constant ionic strength buffer solutions within the pH range 1.2-10.8 was studied.

[Psychometric properties of a self-efficacy scale for physical activity in Brazilian adults].

PubMed

Rech, Cassiano Ricardo; Sarabia, Tais Taiana; Fermino, Rogério César; Hallal, Pedro Curi; Reis, Rodrigo Siqueira

2011-04-01

To test the validity and reliability of a self-efficacy scale for physical activity (PA) in Brazilian adults. A self-efficacy scale was applied jointly with a multidimensional questionnaire through face-to-face interviews with 1,418 individuals (63.4% women) aged ≥ 18 years. The scale was submitted to validity (factorial and construct) and reliability analysis (internal consistency and temporal stability). A test-retest procedure was conducted with 74 individuals to evaluate temporal stability. Exploratory factor analyses revealed two independent factors: self-efficacy for walking and self-efficacy for moderate and vigorous PA (MVPA). Together, these two factors explained 65.4% of the total variance of the scale (20.9% and 44.5% for walking and MVPA, respectively). Cronbach's alpha values were 0.83 for walking and 0.90 for MVPA, indicating high internal consistency. Both factors were significantly and positively correlated (rho ≥ 0.17, P < 0.001) with quality of life indicators (health perception, self-satisfaction, and energy for daily activities), indicating an adequate construct validity. The scale's validity, internal consistency, and reliability were adequate to evaluate self-efficacy for PA in Brazilian adults.

The Reliability, Validity, and Evaluation of the Objective Structured Clinical Examination in Podiatry (Chiropody).

ERIC Educational Resources Information Center

Woodburn, Jim; Sutcliffe, Nick

1996-01-01

The Objective Structured Clinical Examination (OSCE), initially developed for undergraduate medical education, has been adapted for assessment of clinical skills in podiatry students. A 12-month pilot study found the test had relatively low levels of reliability, high construct and criterion validity, and good stability of performance over time.…

A simple, rapid and stability indicating validated method for quantification of lamotrigine in human plasma and dry plasma spot using LC-ESI-MS/MS: Application in clinical study.

PubMed

Namdev, Kuldeep Kumar; Dwivedi, Jaya; Chilkoti, Deepak Chandra; Sharma, Swapnil

2018-01-01

Lamotrigine (LTZ) is a phenyltriazine derivative which belongs to anti-epileptic drugs (AEDs) class and prescribed as mono- or adjunctive-therapy in treatment of epilepsy. Therapeutic drug monitoring (TDM) of AEDs provides a valid clinical tool in optimization of overall therapy. However, TDM is challenging due to the high biological samples (plasma/blood) storage/shipment costs and the limited availability of laboratories providing TDM services. Sampling in the form of dry plasma spot (DPS) or dry blood spot (DBS) are suitable alternative to overcome these issues. We developed and validated a new method for quantification of LTZ in human plasma and DPS. The extraction of LTZ from plasma and DPS was performed using liquid-liquid extraction with diethyl ether and an extraction solution composed of diethyl ether- methyl tert-butyl ether- acetone (50:30:20, v/v/v), respectively. Lamotrigine- 13C3, d3 was used as internal standard (ISTD) and the chromatographic separation was achieved on Hypurity Advance C18 column (150×4.6mm, 5μm). Quantitative estimation of LTZ and ISTD was performed on a liquid chromatography tandem mass spectrometer coupled with electrospray ionization interface operated under positive mode of ionization. Calibration curves were linear (r 2 >0.99) over the concentration range of 10-3020ng/mL for both plasma and DPS. Statistical analysis provides insignificant difference between LTZ concentration extracted from plasma and DPS samples. The method is found suitable for application in clinical study and in therapeutic monitoring of LTZ. To the best of our knowledge this is the first report which describing a validated stability indicating assay for quantification of LTZ in dry plasma spot. Copyright © 2017 Elsevier B.V. All rights reserved.

Test Score Stability and Construct Validity of the Adult Manifest Anxiety Scale-College Version Scores among College Students: A Brief Report

ERIC Educational Resources Information Center

Lowe, Patricia A.; Papanastasiou, Elena C.; DeRuyck, Kimberly A.; Reynolds, Cecil R.

2005-01-01

In this study, the authors investigated the temporal stability and construct validity of the Adult Manifest Anxiety Scale-College Version (AMAS-C; C. R. Reynolds, B. O. Richmond, & P. A. Lowe, 2003b) scores. Results indicated that the AMAS-C scores had adequate to excellent test score stability, and evidence supported the construct validity of the…

Stability of Metronidazole Suspensions.

PubMed

Donnelly, Ronald F; Ying, James

2015-01-01

Metronidazole is an antiprotozoal agent used in the treatment of bacterial and protozoal anaerobic infections. The objectives of this study were to develop concentrated metronidazole suspensions that are inexpensive and easy to prepare and determine the stability of these suspensions after storage in amber polyvinyl chloride bottles at room temperature (23°C) and under refrigeration (5°C). Metronidazole suspensions (50 mg/mL) were prepared from powder using Ora-Blend or simple syrup as the vehicles. Samples were collected in triplicate from each container on days 0, 7, 14, 28, 56, and 93. Samples were assayed using a high-performance liquid chromatography method that had been validated as stability indicating. Color, change in physical appearance, and pH were also monitored at each time interval. There was no apparent change in color or physical appearance. The pH values changed by less than 0.20 units over the 93 days. The stability of metronidazole suspensions compounded from United States Pharmacopeia powder using Ora-Blend or simple syrup and packaged in amber polyvinyl chloride bottles was determined to be 93 days when stored at either room temperature or under refrigeration.

Changes in performance: a 5-year longitudinal study of participants in a multi-source feedback programme.

PubMed

Violato, Claudio; Lockyer, Jocelyn M; Fidler, Herta

2008-10-01

Multi-source feedback (MSF) enables performance data to be provided to doctors from patients, co-workers and medical colleagues. This study examined the evidence for the validity of MSF instruments for general practice, investigated changes in performance for doctors who participated twice, 5 years apart, and determined the association between change in performance and initial assessment and socio-demographic characteristics. Data for 250 doctors included three datasets per doctor from, respectively, 25 patients, eight co-workers and eight medical colleagues, collected on two occasions. There was high internal consistency (alpha > 0.90) and adequate generalisability (Ep(2) > 0.70). D study results indicate adequate generalisability coefficients for groups of eight assessors (medical colleagues, co-workers) and 25 patient surveys. Confirmatory factor analyses provided evidence for the validity of factors that were theoretically expected, meaningful and cohesive. Comparative fit indices were 0.91 for medical colleague data, 0.87 for co-worker data and 0.81 for patient data. Paired t-test analysis showed significant change between the two assessments from medical colleagues and co-workers, but not between the two patient surveys. Multiple linear regressions explained 2.1% of the variance at time 2 for medical colleagues, 21.4% of the variance for co-workers and 16.35% of the variance for patient assessments, with professionalism a key variable in all regressions. There is evidence for the construct validity of the instruments and for their stability over time. Upward changes in performance will occur, although their effect size is likely to be small to moderate.

Stability, reliability and cross-mode correlations of tests in a recommended 8-minute performance assessment battery

NASA Technical Reports Server (NTRS)

Wilkes, R. L.; Kennedy, R. S.; Dunlap, W. P.; Lane, N. E.

1986-01-01

A need exists for an automated performance test system to study drugs, agents, treatments, and stresses of interest to the aviation, space, and environmental medical community. The purpose of this present study is to evaluate tests for inclusion in the NASA-sponsored Automated Performance Test System (APTS). Twenty-one subjects were tested over 10 replications with tests previously identified as good candidates for repeated-measure research. The tests were concurrently administered in paper-and-pencil and microcomputer modes. Performance scores for the two modes were compared. Data from trials 1 to 10 were examined for indications of test stability and reliability. Nine of the ten APT system tests achieved stability. Reliabilities were generally high. Cross-correlation of microbased tests with traditional paper-and-pencil versions revealed similarity of content within tests in the different modes, and implied at least three cognition and two motor factors. This protable, inexpensive, rugged, computerized battery of tests is recommended for use in repeated-measures studies of environmental and drug effects on performance. Identification of other tests compatible with microcomputer testing and potentially capable of tapping previously unidentified factors is recommended. Documentation of APTS sensitivity to environmental agents is available for more than a dozen facilities and is reported briefly. Continuation of such validation remains critical in establishing the efficacy of APTS tests.

Stability indicating RP-HPLC method development and validation for the simultaneous determination of aminexil and minoxidil in pharmaceutical dosage form.

PubMed

Siddiraju, S; Sahithi, M

2015-03-01

The objective of the present work is to develop stability indicating high-performance liquid chromatographic method for the simultaneous determination of aminexil and minoxidil in pharmaceutical dosage form. The chromatographic separation was achieved with BDS Hypersil C18 column (250 mm×4.6 mm×5 μ) as stationary phase and phosphate buffer and acetonitrile (78:22) as mobile phase. The method was employed by using a flow rate of 1.1 mL/min kept at 30°C. The detection wavelength was kept at 238 nm by using photo-diode array detector. The retention times of the aminexil and minoxidil were found to be 2.3 min and 3.9 min, respectively. The method developed was validated in accordance with ICH guidelines with respect to the stability indicating capacity of the method including system suitability, accuracy, precision, linearity, range, limit of detection, limit of quantification and robustness. The linearity responses of aminexil and minoxidil were found to be in the concentration ranges of 18.75-112.5 μg/mL and 25-150 μg/mL, respectively. The LOD and LOQ values for aminexil were found to be 0.31 and 0.92 μg/mL and minoxidil were found to be 0.03 and 0.10 μg/mL respectively. The percentage recoveries for both the drugs were found in the range of 98-101%. This method is accurate, precise and sensitive; hence, it can be employed for routine quality control of aminexil and minoxidil in pharmaceutical industries and drug testing laboratories. Copyright © 2014 Elsevier Masson SAS. All rights reserved.

Best Practices in Stability Indicating Method Development and Validation for Non-clinical Dose Formulations.

PubMed

Henry, Teresa R; Penn, Lara D; Conerty, Jason R; Wright, Francesca E; Gorman, Gregory; Pack, Brian W

2016-11-01

Non-clinical dose formulations (also known as pre-clinical or GLP formulations) play a key role in early drug development. These formulations are used to introduce active pharmaceutical ingredients (APIs) into test organisms for both pharmacokinetic and toxicological studies. Since these studies are ultimately used to support dose and safety ranges in human studies, it is important to understand not only the concentration and PK/PD of the active ingredient but also to generate safety data for likely process impurities and degradation products of the active ingredient. As such, many in the industry have chosen to develop and validate methods which can accurately detect and quantify the active ingredient along with impurities and degradation products. Such methods often provide trendable results which are predictive of stability, thus leading to the name; stability indicating methods. This document provides an overview of best practices for those choosing to include development and validation of such methods as part of their non-clinical drug development program. This document is intended to support teams who are either new to stability indicating method development and validation or who are less familiar with the requirements of validation due to their position within the product development life cycle.

Development and validation of a stability-indicating RP-HPLC-FLD method for determination of 5-[(4-chlorophenoxy) methyl]-1, 3, 4-oxadiazole-2-thiol; A novel drug candidate.

PubMed

Shehzadi, Naureen; Hussain, Khalid; Islam, Muhammad; Bukhari, Nadeem Irfan; Asif, Noman; Khan, Muhammad Tanveer; Salman, Muhammad; Qamar, Shaista; Parveen, Sajida; Zahid, Fakhra; Shah, Arshad Ali; Bilal, Abida; Abbasi, Muhammad Athar; Siddiqui, Sabahat Zahra; Rehman, Azizur

2018-03-01

The present study describes the development and validation of a simple high performance liquid chromatographic method for the determination of a novel drug candidate, 5-[(4-chlorophenoxy) methyl]-1, 3, 4-oxadiazole-2-thiol. The stability-indicating capacity of the method was evaluated by subjecting the compound's solution to hydrolytic, oxidative, photolytic, transition metal- and thermal- stress. The chromatographic separation was achieved over a C18 column (Promosil, 5 µm, 4.60 × 250 mm), maintained at 25°C, using an isocratic mobile phase comprising a mixture of acetonitrile and acidified water of pH 2.67 (1:1, v/v), at a flow rate of 1.00 mL/min and detection using a fluorescent light detector (excitation at 250 nm and emission at 410 nm). The Beer's law was followed over the concentration range 2.50-50.00 μg/ml. The recovery (98.56-100.19%, SD <5%), intraday accuracy and precision (97.31-100.81%, RSD <5%), inter-day accuracy and precision (97.50-100.75%, RSD <5%) and intermediate accuracy and precision (98.10-99.91%, RSD <5%) indicated that the method was reliable, repeatable, reproducible and rugged. The resolution and selectivity factors of the compound's peak from the nearest resolving peak, particularly in case of dry heat and copper metal stress, were found to be greater than 2 and 1, respectively, which indicated specificity and selectivity. The compound was extensively decomposed in alkaline-hydrolytic, oxidative, metal- and dry heat- stress. However, the compound in acidic and neutral conditions was resistant to photolysis. The results of the present study indicate that the developed method is specific, selective, sensitive and suitable, hence, may be used for quality control, stability testing and preformulation studies.

The influence of validity criteria on Immediate Post-Concussion Assessment and Cognitive Testing (ImPACT) test-retest reliability among high school athletes.

PubMed

Brett, Benjamin L; Solomon, Gary S

2017-04-01

Research findings to date on the stability of Immediate Post-Concussion Assessment and Cognitive Testing (ImPACT) Composite scores have been inconsistent, requiring further investigation. The use of test validity criteria across these studies also has been inconsistent. Using multiple measures of stability, we examined test-retest reliability of repeated ImPACT baseline assessments in high school athletes across various validity criteria reported in previous studies. A total of 1146 high school athletes completed baseline cognitive testing using the online ImPACT test battery at two time periods of approximately two-year intervals. No participant sustained a concussion between assessments. Five forms of validity criteria used in previous test-retest studies were applied to the data, and differences in reliability were compared. Intraclass correlation coefficients (ICCs) ranged in composite scores from .47 (95% confidence interval, CI [.38, .54]) to .83 (95% CI [.81, .85]) and showed little change across a two-year interval for all five sets of validity criteria. Regression based methods (RBMs) examining the test-retest stability demonstrated a lack of significant change in composite scores across the two-year interval for all forms of validity criteria, with no cases falling outside the expected range of 90% confidence intervals. The application of more stringent validity criteria does not alter test-retest reliability, nor does it account for some of the variation observed across previously performed studies. As such, use of the ImPACT manual validity criteria should be utilized in the determination of test validity and in the individualized approach to concussion management. Potential future efforts to improve test-retest reliability are discussed.

Stability-indicating RP-HPLC method for the simultaneous determination of escitalopram oxalate and clonazepam.

PubMed

Kakde, Rajendra B; Satone, Dinesh D; Gadapayale, Kamalesh K; Kakde, Megha G

2013-07-01

The objective of the current study was to develop a validated, specific stability-indicating reversed-phase liquid chromatographic (LC) method for the quantitative determination of escitalopram oxalate and clonazepam and their related substances in bulk drugs and pharmaceutical dosage forms in the presence of degradation products. Forced degradation studies were performed on the pure drugs of escitalopram oxalate and clonazepam, as per the stress conditions prescribed by the International Conference on Harmonization (ICH) using acid, base, oxidation, thermal stress and photolytic degradation to show the stability-indicating power of the method. Significant degradation was observed during acid and alkaline hydrolysis and no degradation was observed in other stress conditions. The chromatographic method was optimized using the samples generated from forced degradation studies. Good resolution between the peaks corresponded to the active pharmaceutical ingredients, escitalopram oxalate and clonazepam, and degradation products from the analyte were achieved on an ODS Hypersil C18 column (250 × 4.6 mm) using a mobile phase consisting of a mixture of acetonitrile-50 mM phosphate buffer + 10 mM triethylamine (70:30, v/v). The detection was conducted at 268 nm. The limit of detection and the limit of quantitation for escitalopram oxalate and clonazepam were established. The stress test solutions were assayed against the qualified working standards of escitalopram oxalate and clonazepam, which indicated that the developed LC method was stability-indicating. Validation of the developed LC method was conducted as per ICH requirements. The developed LC method was found to be suitable to check the quality of bulk samples of escitalopram oxalate and clonazepam.

Simultaneous determination of aliskiren and hydrochlorothiazide from their pharmaceutical preparations using a validated stability-indicating MEKC method.

PubMed

Sangoi, Maximiliano S; Wrasse-Sangoi, Micheli; Oliveira, Paulo R; Rolim, Clarice M B; Steppe, Martin

2011-08-01

A stability-indicating MEKC method was developed and validated for the simultaneous determination of aliskiren (ALI) and hydrochlorothiazide (HCTZ) in pharmaceutical formulations using ranitidine as an internal standard (IS). Optimal conditions for the separation of ALI, HCTZ and its major impurity chlorothiazide (CTZ), IS and degradation products were investigated. The method employed 47 mM Tris buffer and 47 mM anionic detergent SDS solution at pH 10.2 as the background electrolyte. MEKC method was performed on a fused-silica capillary (40 cm) at 28°C. Applied voltage was 26 kV (positive polarity) and photodiode array (PDA) detector was set at 217 nm. The method was validated in accordance with the ICH requirements. The method was linear over the concentration range of 5-100 and 60-1200 μg/mL for HCTZ and ALI, respectively (r(2) >0.9997). The stability-indicating capability of the method was established by enforced degradation studies combined with peak purity assessment using the PDA detection. Precision and accuracy evaluated by RSD were lower than 2%. The method proved to be robust by a fractional factorial design evaluation. The proposed MEKC method was successfully applied for the quantitative analysis of ALI and HCTZ both individually and in a combined dosage tablet formulation to support the quality control. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Validated Stability-Indicating RP-UPLC Method for Simultaneous Determination of Desloratadine and Sodium Benzoate in Oral Liquid Pharmaceutical Formulations.

PubMed

Kumar, Navneet; Sangeetha, Dhanaraj; Reddy, Pingili Sunil; Prakash, Lakkireddy

2012-01-01

A novel, sensitive and selective stability-indicating gradient reverse phase ultra performance liquid chromatographic method was developed and validated for the quantitative determination of desloratadine and sodium benzoate in pharmaceutical oral liquid formulation. The chromatographic separation was achieved on Acquity BEH C8 (100 mm × 2.1 mm) 1.7 μm column by using mobile phase containing a gradient mixture of solvent A (0.05 M KH(2)PO(4) and 0.07 M triethylamine, pH 3.0) and B (50:25:25 v/v/v mixture of acetonitrile, methanol and water) at flow rate of 0.4 mL/min. Column temperature was maintained at 40°C and detection was carried out at a wavelength of 272 nm. The described method shows excellent linearity over a range of 0.254 μg/mL to 76.194 μg/mL for desloratadine and 1.006 μg/mL to 301.67 μg/mL for sodium benzoate. The correlation coefficient for desloratadine and sodium benzoate was more than 0.999. To establish stability-indicating capability of the method, drug product was subjected to the stress conditions of acid, base, oxidative, hydrolytic, thermal and photolytic degradation. The degradation products were well resolved from desloratadine and sodium benzoate. The developed method was validated as per international ICH guidelines with respect to specificity, linearity, LOD, LOQ, accuracy, precision and robustness.

Influence of sodium metabisulfite and glutathione on the stability of vitamin C in O/W emulsion and extemporaneous aqueous gel.

PubMed

Maia, Adriana M; Baby, André Rolim; Pinto, Claudinéia A S O; Yasaka, Wilson J; Suenaga, Eunice; Kaneko, Telma M; Velasco, Maria Valéria Robles

2006-09-28

Vitamin C exerts several functions on skin as collagen synthesis, depigmentant and antioxidant activity. Vitamin C is unstable in the presence of oxygen, luminosity, humidity, high temperatures and heavy metals, which presents a significant challenge to the development of cosmetic formulations. Therefore, the utilization of an effective antioxidant system is required to maintain the vitamin C stability. The purpose of this research work was to develop prototypes of cosmetic formulations, as O/W emulsion and extemporaneous aqueous gel, containing vitamin C and to evaluate the influence of sodium metabisulfite (SMB) and glutathione (GLT), as antioxidants, on the stability of the active substance. A HPLC stability-indicating method was developed and validated for this study and stability assays were performed in 90 and 26 days and storage conditions were 5.0+/-0.5, 24+/-2 and 40.0+/-0.5 degrees C. The HPLC stability-indicating method showed linearity (r(2)>0.99), specificity, R.S.D.<1.22% and accuracy/recovery ranging from 95.46 to 101.54%. Preparations with SMB or GLT and the antioxidant-free presented results statistically distinct, demonstrating the necessity of the antioxidant system addition. O/W emulsions with SMB or GLT retained the vitamin C content >90.38% stored at 5.0+/-0.5 and 24+/-2 degrees C. For the aqueous gel with SMB or GLT, the active substance concentration was maintained >94.03%. Considering the vitamin C stability, the SMB and the GLT showed to be statistically adequate, as antioxidants, for the cosmetic formulations.

Simultaneous quantification of five major active components in capsules of the traditional Chinese medicine ‘Shu-Jin-Zhi-Tong’ by high performance liquid chromatography

PubMed Central

Yang, Xing-Xin; Zhang, Xiao-Xia; Chang, Rui-Miao; Wang, Yan-Wei; Li, Xiao-Ni

2011-01-01

A simple and reliable high performance liquid chromatography (HPLC) method has been developed for the simultaneous quantification of five major bioactive components in ‘Shu-Jin-Zhi-Tong’ capsules (SJZTC), for the purposes of quality control of this commonly prescribed traditional Chinese medicine. Under the optimum conditions, excellent separation was achieved, and the assay was fully validated in terms of linearity, precision, repeatability, stability and accuracy. The validated method was applied successfully to the determination of the five compounds in SJZTC samples from different production batches. The HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of SJZTC. PMID:29403711

A reliability of the prototype trunk training system for sitting balance.

PubMed

Jeong, Juri; Park, Dae-Sung; Lee, Hyelim; Eun, Seondeok

2014-11-01

[Purpose] Cerebral palsy is a disorder that affects balance in the sitting position. Cerebral palsy patients need trunk muscle strengthening and balance training. In order to improve trunk control sensory-motor control training is carried out on an unstable surface. We have developed a Trunk Training System (TTS) that can provide visual feedback using a tilt sensor for balance training in the sitting position. Before using the TTS for training children with cerebral palsy experiments were conducted with healthy adult subjects and the TTS to gather basic data for its improvement. [Subjects] The subjects were 11 healthy men (n=3) and women (n=8). [Methods] Subjects trained at two levels (5°, 10°), in four different directions (anterior, posterior, left, right), three times each. TTS outcome indices (stability index, performance time) were measured. [Results] The stability index and performance time showed high correlation (-0.6

Validation of a liquid chromatography method for the simultaneous determination of sulfadimethoxine and trimethoprim and application to a stability study.

PubMed

Louati, K; Mistiri, F; Kallel, M; Safta, F

2010-03-01

A liquid chromatography method is described for the simultaneous determination of sulfadimetoxine and trimethoprim from a veterinary formulation at the proportion of 187 mg and 40 mg respectively in presence of some excipient. The solution was subjected to different International Conference On Harmonisation prescribed stress conditions (hydrolysis, oxidation and photolysis). A stability-indicating high-performance liquid chromatography method was developed for the analysis of active substances in presence of their major degradation products. It involved a Knauer Eurospher C18 thermostated column at 25 degrees C, and 9.57 mM phosphate buffer (pH adjusted to 2.0 with orthophosphoric acid)-acetonitrile (70:30 v/v) as mobile phase. The mobile phase flow rate and sample volume injected were 1.2 mL/min and 20 microL, respectively. The selected wavelength for the determination was 248 nm. The method was validated for linearity, precision, accuracy and specificity, and then applied to a stability study of sulfadimetoxine and trimethoprim in the veterinary solution packaged in high density polyethylene plastic bottles of 1 L and 100 mL thermosealed and no thermosealed and corked by a white cap, at both accelerated and long-term conditions required by the International Conference On Harmonisation. The method developed, which separates all of the most degradation products formed under variety of conditions, proved to be simple, accurate, precise and specific. The results of the stress degradation show that the solution is more sensitive to hydrolysis. The stability studies carried out on three batches of each presentation show that the finished product remains stable for six months. Copyright 2010 Elsevier Masson SAS. All rights reserved.

Integrating a Motion Base into a CAVE Automatic Virtual Environment: Phase 1

DTIC Science & Technology

2001-07-01

this, a CAVE system must perform well in the following motion-related areas: visual gaze stability, simulator sickness, realism (or face validity...and performance validity. Visual Gaze Stability Visual gaze stability, the ability to maintain eye fixation on a particular target, depends upon human...reflexes such as the vestibulo-ocular reflex (VOR) and the optokinetic nystagmus (OKN). VOR is a reflex that counter-rotates the eye relative to the

Stability-Indicating HPLC Determination of Gemcitabine in Pharmaceutical Formulations

PubMed Central

Singh, Rahul; Shakya, Ashok K.; Naik, Rajashri; Shalan, Naeem

2015-01-01

A simple, sensitive, inexpensive, and rapid stability indicating high performance liquid chromatographic method has been developed for determination of gemcitabine in injectable dosage forms using theophylline as internal standard. Chromatographic separation was achieved on a Phenomenex Luna C-18 column (250 mm × 4.6 mm; 5μ) with a mobile phase consisting of 90% water and 10% acetonitrile (pH 7.00 ± 0.05). The signals of gemcitabine and theophylline were recorded at 275 nm. Calibration curves were linear in the concentration range of 0.5–50 μg/mL. The correlation coefficient was 0.999 or higher. The limit of detection and limit of quantitation were 0.1498 and 0.4541 μg/mL, respectively. The inter- and intraday precision were less than 2%. Accuracy of the method ranged from 100.2% to 100.4%. Stability studies indicate that the drug was stable to sunlight and UV light. The drug gives 6 different hydrolytic products under alkaline stress and 3 in acidic condition. Aqueous and oxidative stress conditions also degrade the drug. Degradation was higher in the alkaline condition compared to other stress conditions. The robustness of the methods was evaluated using design of experiments. Validation reveals that the proposed method is specific, accurate, precise, reliable, robust, reproducible, and suitable for the quantitative analysis. PMID:25838825

Stability-indicating RP-HPLC Method for the Simultaneous Determination of Sitagliptin and Simvastatin in Tablets

PubMed Central

Ramalingam, P.; Bhaskar, V. Udaya; Reddy, Y. Padmanabha; Kumar, K. Vinod

2014-01-01

A new stability-indicating high-performance liquid chromatographic method for simultaneous analysis of sitagliptin and simvastatin in pharmaceutical dosage form was developed and validated. The mobile phase consisted of methanol and water (70:30, v/v) with 0.2 % of n-heptane sulfonic acid adjusted to pH 3.0 with ortho phosphoric acid was used. Retentions of sitagliptin and simvastatin were 4.3 min and 30.4 min, respectively with a flow rate of 1 ml/min on C8 (Qualisil BDS, 250×4.6 mm, 5 μ). Eluents were detected at 253 nm using photodiode diode array detector. The linear regression analysis data for the linearity plot showed correlation coefficient values of 0.9998 and 0.9993 for sitagliptin and simvastatin, with respective concentration ranges of 20-150 μg/ml and 8-60 μg/ml. The relative standard deviation for inter-day precision was lower than 2.0%. The assay of sitagliptin and simvastatin was determined in tablet dosage form was found to be within limits. Both drugs were subjected to a variety of stress conditions such as acidic, basic, oxidation, photolytic, neutral and thermal stress in order to achieve adequate degradation. Results revealed that considerable degradation was found in all stress conditions except oxidative degradations. The method has proven specificity for stability indicating assay method. PMID:25425754

Quantitative determination of multi markers in five varieties of Withania somnifera using ultra-high performance liquid chromatography with hybrid triple quadrupole linear ion trap mass spectrometer combined with multivariate analysis: Application to pharmaceutical dosage forms.

PubMed

Chandra, Preeti; Kannujia, Rekha; Saxena, Ankita; Srivastava, Mukesh; Bahadur, Lal; Pal, Mahesh; Singh, Bhim Pratap; Kumar Ojha, Sanjeev; Kumar, Brijesh

2016-09-10

An ultra-high performance liquid chromatography electrospray ionization tandem mass spectrometry method has been developed and validated for simultaneous quantification of six major bioactive compounds in five varieties of Withania somnifera in various plant parts (leaf, stem and root). The analysis was accomplished on Waters ACQUITY UPLC BEH C18 column with linear gradient elution of water/formic acid (0.1%) and acetonitrile at a flow rate of 0.3mLmin(-1). The proposed method was validated with acceptable linearity (r(2), 0.9989-0.9998), precision (RSD, 0.16-2.01%), stability (RSD, 1.04-1.62%) and recovery (RSD ≤2.45%), under optimum conditions. The method was also successfully applied for the simultaneous determination of six marker compounds in twenty-six marketed formulations. Hierarchical cluster analysis and principal component analysis were applied to discriminate these twenty-six batches based on characteristics of the bioactive compounds. The results indicated that this method is advance, rapid, sensitive and suitable to reveal the quality of Withania somnifera and also capable of performing quality evaluation of polyherbal formulations having similar markers/raw herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

Validation of the Filovirus Plaque Assay for Use in Preclinical Studies

PubMed Central

Shurtleff, Amy C.; Bloomfield, Holly A.; Mort, Shannon; Orr, Steven A.; Audet, Brian; Whitaker, Thomas; Richards, Michelle J.; Bavari, Sina

2016-01-01

A plaque assay for quantitating filoviruses in virus stocks, prepared viral challenge inocula and samples from research animals has recently been fully characterized and standardized for use across multiple institutions performing Biosafety Level 4 (BSL-4) studies. After standardization studies were completed, Good Laboratory Practices (GLP)-compliant plaque assay method validation studies to demonstrate suitability for reliable and reproducible measurement of the Marburg Virus Angola (MARV) variant and Ebola Virus Kikwit (EBOV) variant commenced at the United States Army Medical Research Institute of Infectious Diseases (USAMRIID). The validation parameters tested included accuracy, precision, linearity, robustness, stability of the virus stocks and system suitability. The MARV and EBOV assays were confirmed to be accurate to ±0.5 log10 PFU/mL. Repeatability precision, intermediate precision and reproducibility precision were sufficient to return viral titers with a coefficient of variation (%CV) of ≤30%, deemed acceptable variation for a cell-based bioassay. Intraclass correlation statistical techniques for the evaluation of the assay’s precision when the same plaques were quantitated by two analysts returned values passing the acceptance criteria, indicating high agreement between analysts. The assay was shown to be accurate and specific when run on Nonhuman Primates (NHP) serum and plasma samples diluted in plaque assay medium, with negligible matrix effects. Virus stocks demonstrated stability for freeze-thaw cycles typical of normal usage during assay retests. The results demonstrated that the EBOV and MARV plaque assays are accurate, precise and robust for filovirus titration in samples associated with the performance of GLP animal model studies. PMID:27110807

A Study of Method Development, Validation, and Forced Degradation for Simultaneous Quantification of Paracetamol and Ibuprofen in Pharmaceutical Dosage Form by RP-HPLC Method

PubMed Central

Jahan, Md. Sarowar; Islam, Md. Jahirul; Begum, Rehana; Kayesh, Ruhul; Rahman, Asma

2014-01-01

A rapid and stability-indicating reversed phase high-performance liquid chromatography (RP-HPLC) method was developed for simultaneous quantification of paracetamol and ibuprofen in their combined dosage form especially to get some more advantages over other methods already developed for this combination. The method was validated according to United States Pharmacopeia (USP) guideline with respect to accuracy, precision, specificity, linearity, solution stability, robustness, sensitivity, and system suitability. Forced degradation study was validated according to International Conference on Harmonisation (ICH). For this, an isocratic condition of mobile phase comprising phosphate buffer (pH 6.8) and acetonitrile in a ratio of 65:35, v/v at a flow rate of 0.7 mL/minute over RP C18 (octadecylsilane (ODS), 150 × 4.6 mm, 5 μm, Phenomenex Inc.) column at ambient temperature was maintained. The method showed excellent linear response with correlation coefficient (R2) values of 0.999 and 1.0 for paracetamol and ibuprofen respectively, which were within the limit of correlation coefficient (R2 > 0.995). The percent recoveries for two drugs were found within the acceptance limit of (97.0–103.0%). Intra-and inter-day precision studies of the new method were less than the maximum allowable limit percentage of relative standard deviation (%RSD) ≤ 2.0. Forced degradation of the drug product was carried out as per the ICH guidelines with a view to establishing the stability-indicating property of this method and providing useful information about the degradation pathways, degradation products, and how the quality of a drug substance and drug product changes with time under the influence of various stressing conditions. The degradation of ibuprofen was within the limit (5–20%, according to the guideline of ICH), while paracetamol showed <20% degradation in oxidation and basic condition. PMID:25452691

A Study of Method Development, Validation, and Forced Degradation for Simultaneous Quantification of Paracetamol and Ibuprofen in Pharmaceutical Dosage Form by RP-HPLC Method.

PubMed

Jahan, Md Sarowar; Islam, Md Jahirul; Begum, Rehana; Kayesh, Ruhul; Rahman, Asma

2014-01-01

A rapid and stability-indicating reversed phase high-performance liquid chromatography (RP-HPLC) method was developed for simultaneous quantification of paracetamol and ibuprofen in their combined dosage form especially to get some more advantages over other methods already developed for this combination. The method was validated according to United States Pharmacopeia (USP) guideline with respect to accuracy, precision, specificity, linearity, solution stability, robustness, sensitivity, and system suitability. Forced degradation study was validated according to International Conference on Harmonisation (ICH). For this, an isocratic condition of mobile phase comprising phosphate buffer (pH 6.8) and acetonitrile in a ratio of 65:35, v/v at a flow rate of 0.7 mL/minute over RP C18 (octadecylsilane (ODS), 150 × 4.6 mm, 5 μm, Phenomenex Inc.) column at ambient temperature was maintained. The method showed excellent linear response with correlation coefficient (R (2)) values of 0.999 and 1.0 for paracetamol and ibuprofen respectively, which were within the limit of correlation coefficient (R (2) > 0.995). The percent recoveries for two drugs were found within the acceptance limit of (97.0-103.0%). Intra-and inter-day precision studies of the new method were less than the maximum allowable limit percentage of relative standard deviation (%RSD) ≤ 2.0. Forced degradation of the drug product was carried out as per the ICH guidelines with a view to establishing the stability-indicating property of this method and providing useful information about the degradation pathways, degradation products, and how the quality of a drug substance and drug product changes with time under the influence of various stressing conditions. The degradation of ibuprofen was within the limit (5-20%, according to the guideline of ICH), while paracetamol showed <20% degradation in oxidation and basic condition.

Development and validation of a stability indicating HPLC method for determination of lisinopril, lisinopril degradation product and parabens in the lisinopril extemporaneous formulation.

PubMed

Beasley, Christopher A; Shaw, Jessica; Zhao, Zack; Reed, Robert A

2005-03-09

The purpose of the research described herein was to develop and validate a stability-indicating HPLC method for lisinopril, lisinopril degradation product (DKP), methyl paraben and propyl paraben in a lisinopril extemporaneous formulation. The method developed in this report is selective for the components listed above, in the presence of the complex and chromatographically rich matrix presented by the Bicitra and Ora-Sweet SF formulation diluents. The method was also shown to have adequate sensitivity with a detection limit of 0.0075 microg/mL (0.03% of lisinopril method concentration). The validation elements investigated showed that the method has acceptable specificity, recovery, linearity, solution stability, and method precision. Acceptable robustness indicates that the assay method remains unaffected by small but deliberate variations, which are described in ICH Q2A and Q2B guidelines.

Examining the validity of AHRQ's patient safety indicators (PSIs): is variation in PSI composite score related to hospital organizational factors?

PubMed

Shin, Marlena H; Sullivan, Jennifer L; Rosen, Amy K; Solomon, Jeffrey L; Dunn, Edward J; Shimada, Stephanie L; Hayes, Jennifer; Rivard, Peter E

2014-12-01

Increasing use of Agency for Healthcare Research and Quality's Patient Safety Indicators (PSIs) for hospital performance measurement intensifies the need to critically assess their validity. Our study examined the extent to which variation in PSI composite score is related to differences in hospital organizational structures or processes (i.e., criterion validity). In site visits to three Veterans Health Administration hospitals with high and three with low PSI composite scores ("low performers" and "high performers," respectively), we interviewed a cross-section of hospital staff. We then coded interview transcripts for evidence in 13 safety-related domains and assessed variation across high and low performers. Evidence of leadership and coordination of work/communication (organizational process domains) was predominantly favorable for high performers only. Evidence in the other domains was either mixed, or there were insufficient data to rate the domains. While we found some evidence of criterion validity, the extent to which variation in PSI rates is related to differences in hospitals' organizational structures/processes needs further study. © The Author(s) 2014.

Design of an adaptive super-twisting decoupled terminal sliding mode control scheme for a class of fourth-order systems.

PubMed

Ashtiani Haghighi, Donya; Mobayen, Saleh

2018-04-01

This paper proposes an adaptive super-twisting decoupled terminal sliding mode control technique for a class of fourth-order systems. The adaptive-tuning law eliminates the requirement of the knowledge about the upper bounds of external perturbations. Using the proposed control procedure, the state variables of cart-pole system are converged to decoupled terminal sliding surfaces and their equilibrium points in the finite time. Moreover, via the super-twisting algorithm, the chattering phenomenon is avoided without affecting the control performance. The numerical results demonstrate the high stabilization accuracy and lower performance indices values of the suggested method over the other ones. The simulation results on the cart-pole system as well as experimental validations demonstrate that the proposed control technique exhibits a reasonable performance in comparison with the other methods. Copyright © 2018 ISA. Published by Elsevier Ltd. All rights reserved.

Aeroservoelastic Modeling and Validation of a Thrust-Vectoring F/A-18 Aircraft

NASA Technical Reports Server (NTRS)

Brenner, Martin J.

1996-01-01

An F/A-18 aircraft was modified to perform flight research at high angles of attack (AOA) using thrust vectoring and advanced control law concepts for agility and performance enhancement and to provide a testbed for the computational fluid dynamics community. Aeroservoelastic (ASE) characteristics had changed considerably from the baseline F/A-18 aircraft because of structural and flight control system amendments, so analyses and flight tests were performed to verify structural stability at high AOA. Detailed actuator models that consider the physical, electrical, and mechanical elements of actuation and its installation on the airframe were employed in the analysis to accurately model the coupled dynamics of the airframe, actuators, and control surfaces. This report describes the ASE modeling procedure, ground test validation, flight test clearance, and test data analysis for the reconfigured F/A-18 aircraft. Multivariable ASE stability margins are calculated from flight data and compared to analytical margins. Because this thrust-vectoring configuration uses exhaust vanes to vector the thrust, the modeling issues are nearly identical for modem multi-axis nozzle configurations. This report correlates analysis results with flight test data and makes observations concerning the application of the linear predictions to thrust-vectoring and high-AOA flight.

Evaluation of the stability of fluoxetine in pluronic lecithin organogel and the determination of an appropriate beyond-use date.

PubMed

Peacock, Gina F; Sauvageot, Jurgita

2014-01-01

Fluoxetine is a commonly prescribed psychotropic medication for a variety of behavioral diagnoses in veterinary practice, and fluoxetine in Pluronic lecithin organogel has been used successfully in treating inappropriate urine spraying in felines. Historically, pharmacists have assigned a variety of beyond-use dates to extemporaneously compound drugs in Pluronic lecithin organogel. The objective of this study was to evaluate the stability of fluoxetine in Pluronic lecithin organogel over a period of six months and to determine an appropriate beyond-use date. A stability-indicating high-performance liquid chromatography method for fluoxetine in Pluronic lecithin organogel was validated in our laboratory. Fluoxetine-Pluronic lecithin organogel 50 mg/mL was prepared by a local compounding pharmacy and analyzed by high-performance liquid chromatograph at 0, 7, 14, 21, 28, 45, 60, 90, and 180 days. Physical stability was also assessed by visual observation. At each time point percent of initial concentration was calculated. The beyond-use date was determined as the time period that the samples maintained at least 90 percent of the initial concentration. At 180 days, the mean percent of initial concentration was 99 +/- 1.5 and, visually, the fluoxetine-Pluronic lecithin organogel retained the original color and consistency, without detectable separation of the different phases of Pluronic lecithin organogel. Since fluoxetine was physically stable and retained greater than 90 percent of initial concentration in Pluronic lecithin organogel for 180 days when stored at room temperature and protected from light, a beyond-use date of 180 days is appropriate.

Stability-indicating UPLC method for determining related substances and degradants in dronedarone.

PubMed

Pydimarry, Surya Prakash Rao; Cholleti, Vijay Kumar; Vangala, Ranga Reddy

2014-08-01

A simple, sensitive and reproducible method was developed on ultra-performance liquid chromatography coupled with photodiode array detection for the quantitative determination of dronedarone hydrochloride (DRO) in drug substance and pharmaceutical dosage forms. The method is applicable for the quantification of related substances and assays of drug substances. Chromatographic separation was achieved on Acquity UPLC BEH C8 100 mm, 2.1 mm and 1.7 µm columns, using gradient elution within a short run time of 10.0 min. The eluted compounds were monitored at 288 nm, the flow rate was 0.5 mL/min and the column oven temperature was maintained at 40°C. The resolution of DRO and 11 impurities (potentials and by-products) was greater than 2.0 for all pairs of components. The high correlation coefficient value (>0.9995) indicates the clear correlations between the concentrations of investigated compound and their peak areas within the test ranges. The repeatability and intermediate precision, expressed by the relative standard deviation, were less than 2.5%. The accuracy and validity of the method were further ascertained by performing recovery studies via a spike method. The accuracy of the method, expressed as relative error, was satisfactory. No interference was observed from concomitant substances normally added to the tablets. DRO was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. DRO was found to degrade significantly in acid and base stress conditions and to remain stable in thermal, photolytic degradation, oxidative and hydrolytic conditions. The degradation products were well resolved from primary peak and its impurities, proving that the method is stability indicating. The developed method was validated as per International Conference on Harmonization guidelines with respect to specificity, limit of detection, limit of quantification, linearity, accuracy, precision, solution stability and robustness. This method is also suitable for the determination of DRO drug substance and pharmaceutical dosage forms. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

LOX/hydrocarbon rocket engine analytical design methodology development and validation. Volume 1: Executive summary and technical narrative

NASA Technical Reports Server (NTRS)

Pieper, Jerry L.; Walker, Richard E.

1993-01-01

During the past three decades, an enormous amount of resources were expended in the design and development of Liquid Oxygen/Hydrocarbon and Hydrogen (LOX/HC and LOX/H2) rocket engines. A significant portion of these resources were used to develop and demonstrate the performance and combustion stability for each new engine. During these efforts, many analytical and empirical models were developed that characterize design parameters and combustion processes that influence performance and stability. Many of these models are suitable as design tools, but they have not been assembled into an industry-wide usable analytical design methodology. The objective of this program was to assemble existing performance and combustion stability models into a usable methodology capable of producing high performing and stable LOX/hydrocarbon and LOX/hydrogen propellant booster engines.

Stability of florfenicol in drinking water.

PubMed

Hayes, John M; Eichman, Jonathan; Katz, Terry; Gilewicz, Rosalia

2003-01-01

Florfenicol, a broad-spectrum antibiotic, is being developed for veterinary application as an oral concentrate intended for dilution with drinking water. When a drug product is dosed via drinking water in a farm setting, a number of variables, including pH, chlorine content, hardness of the water used for dilution, and container material, may affect its stability, leading to a decrease in drug potency. The stability of florfenicol after dilution of Florfenicol Drinking Water Concentrate Oral Solution, 23 mg/mL, with drinking water was studied. A stability-indicating, validated liquid chromatographic method was used to evaluate florfenicol stability at 25 degrees C at 5, 10, and 24 h after dilution. The results indicate that florfenicol is stable under a range of simulated field conditions, including various pipe materials and conditions of hard or soft and chlorinated or nonchlorinated water at low or high pH. Significant degradation (> 10%) was observed only for isolated combinations in galvanized pipes. Analysis indicated that the florfenicol concentration in 8 of the 12 water samples stored in galvanized pipes remained above 90% of the initial concentration (100 mg/L) for 24 h after dilution.

Fundamental Movement Skills Are More than Run, Throw and Catch: The Role of Stability Skills.

PubMed

Rudd, James R; Barnett, Lisa M; Butson, Michael L; Farrow, Damian; Berry, Jason; Polman, Remco C J

2015-01-01

In motor development literature fundamental movement skills are divided into three constructs: locomotive, object control and stability skills. Most fundamental movement skills research has focused on children's competency in locomotor and object control skills. The first aim of this study was to validate a test battery to assess the construct of stability skills, in children aged 6 to 10 (M age = 8.2, SD = 1.2). Secondly we assessed how the stability skills construct fitted into a model of fundamental movement skill. The Delphi method was used to select the stability skill battery. Confirmatory factor analysis (CFA) was used to assess if the skills loaded onto the same construct and a new model of FMS was developed using structural equation modelling. Three postural control tasks were selected (the log roll, rock and back support) because they had good face and content validity. These skills also demonstrated good predictive validity with gymnasts scoring significantly better than children without gymnastic training and children from a high SES school performing better than those from a mid and low SES schools and the mid SES children scored better than the low SES children (all p < .05). Inter rater reliability tests were excellent for all three skills (ICC = 0.81, 0.87, 0.87) as was test re-test reliability (ICC 0.87-0.95). CFA provided good construct validity, and structural equation modelling revealed stability skills to be an independent factor in an overall FMS model which included locomotor (r = .88), object control (r = .76) and stability skills (r = .81). This study provides a rationale for the inclusion of stability skills in FMS assessment. The stability skills could be used alongside other FMS assessment tools to provide a holistic assessment of children's fundamental movement skills.

The validity and reliability of a dynamic neuromuscular stabilization-heel sliding test for core stability.

PubMed

Cha, Young Joo; Lee, Jae Jin; Kim, Do Hyun; You, Joshua Sung H

2017-10-23

Core stabilization plays an important role in the regulation of postural stability. To overcome shortcomings associated with pain and severe core instability during conventional core stabilization tests, we recently developed the dynamic neuromuscular stabilization-based heel sliding (DNS-HS) test. The purpose of this study was to establish the criterion validity and test-retest reliability of the novel DNS-HS test. Twenty young adults with core instability completed both the bilateral straight leg lowering test (BSLLT) and DNS-HS test for the criterion validity study and repeated the DNS-HS test for the test-retest reliability study. Criterion validity was determined by comparing hip joint angle data that were obtained from BSLLT and DNS-HS measures. The test-retest reliability was determined by comparing hip joint angle data. Criterion validity was (ICC2,3) = 0.700 (p< 0.05), suggesting a good relationship between the two core stability measures. Test-retest reliability was (ICC3,3) = 0.953 (p< 0.05), indicating excellent consistency between the repeated DNS-HS measurements. Criterion validity data demonstrated a good relationship between the gold standard BSLLT and DNS-HS core stability measures. Test-retest reliability data suggests that DNS-HS core stability was a reliable test for core stability. Clinically, the DNS-HS test is useful to objectively quantify core instability and allow early detection and evaluation.

Comparison of thunderstorm simulations from WRF-NMM and WRF-ARW models over East Indian Region.

PubMed

Litta, A J; Mary Ididcula, Sumam; Mohanty, U C; Kiran Prasad, S

2012-01-01

The thunderstorms are typical mesoscale systems dominated by intense convection. Mesoscale models are essential for the accurate prediction of such high-impact weather events. In the present study, an attempt has been made to compare the simulated results of three thunderstorm events using NMM and ARW model core of WRF system and validated the model results with observations. Both models performed well in capturing stability indices which are indicators of severe convective activity. Comparison of model-simulated radar reflectivity imageries with observations revealed that NMM model has simulated well the propagation of the squall line, while the squall line movement was slow in ARW. From the model-simulated spatial plots of cloud top temperature, we can see that NMM model has better captured the genesis, intensification, and propagation of thunder squall than ARW model. The statistical analysis of rainfall indicates the better performance of NMM than ARW. Comparison of model-simulated thunderstorm affected parameters with that of the observed showed that NMM has performed better than ARW in capturing the sharp rise in humidity and drop in temperature. This suggests that NMM model has the potential to provide unique and valuable information for severe thunderstorm forecasters over east Indian region.

An Integrated Study on a Novel High Temperature High Entropy Alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Shizhong

2016-12-31

This report summarizes our recent works of theoretical modeling, simulation, and experimental validation of the simulation results on the new refractory high entropy alloy (HEA) design and oxide doped refractory HEA research. The simulation of the stability and thermal dynamics simulation on potential thermal stable candidates were performed and related HEA with oxide doped samples were synthesized and characterized. The HEA ab initio density functional theory and molecular dynamics physical property simulation methods and experimental texture validation techniques development, achievements already reached, course work development, students and postdoc training, and future improvement research directions are briefly introduced.

Nonclinical dose formulation analysis method validation and sample analysis.

PubMed

Whitmire, Monica Lee; Bryan, Peter; Henry, Teresa R; Holbrook, John; Lehmann, Paul; Mollitor, Thomas; Ohorodnik, Susan; Reed, David; Wietgrefe, Holly D

2010-12-01

Nonclinical dose formulation analysis methods are used to confirm test article concentration and homogeneity in formulations and determine formulation stability in support of regulated nonclinical studies. There is currently no regulatory guidance for nonclinical dose formulation analysis method validation or sample analysis. Regulatory guidance for the validation of analytical procedures has been developed for drug product/formulation testing; however, verification of the formulation concentrations falls under the framework of GLP regulations (not GMP). The only current related regulatory guidance is the bioanalytical guidance for method validation. The fundamental parameters for bioanalysis and formulation analysis validations that overlap include: recovery, accuracy, precision, specificity, selectivity, carryover, sensitivity, and stability. Divergence in bioanalytical and drug product validations typically center around the acceptance criteria used. As the dose formulation samples are not true "unknowns", the concept of quality control samples that cover the entire range of the standard curve serving as the indication for the confidence in the data generated from the "unknown" study samples may not always be necessary. Also, the standard bioanalytical acceptance criteria may not be directly applicable, especially when the determined concentration does not match the target concentration. This paper attempts to reconcile the different practices being performed in the community and to provide recommendations of best practices and proposed acceptance criteria for nonclinical dose formulation method validation and sample analysis.

Prospective, Head-to-Head Study of Three Computerized Neurocognitive Assessment Tools (CNTs): Reliability and Validity for the Assessment of Sport-Related Concussion.

PubMed

Nelson, Lindsay D; LaRoche, Ashley A; Pfaller, Adam Y; Lerner, E Brooke; Hammeke, Thomas A; Randolph, Christopher; Barr, William B; Guskiewicz, Kevin; McCrea, Michael A

2016-01-01

Limited data exist comparing the performance of computerized neurocognitive tests (CNTs) for assessing sport-related concussion. We evaluated the reliability and validity of three CNTs-ANAM, Axon Sports/Cogstate Sport, and ImPACT-in a common sample. High school and collegiate athletes completed two CNTs each at baseline. Concussed (n=165) and matched non-injured control (n=166) subjects repeated testing within 24 hr and at 8, 15, and 45 days post-injury. Roughly a quarter of each CNT's indices had stability coefficients (M=198 day interval) over .70. Group differences in performance were mostly moderate to large at 24 hr and small by day 8. The sensitivity of reliable change indices (RCIs) was best at 24 hr (67.8%, 60.3%, and 47.6% with one or more significant RCIs for ImPACT, Axon, and ANAM, respectively) but diminished to near the false positive rates thereafter. Across time, the CNTs' sensitivities were highest in those athletes who became asymptomatic within 1 day before neurocognitive testing but was similar to the tests' false positive rates when including athletes who became asymptomatic several days earlier. Test-retest reliability was similar among these three CNTs and below optimal standards for clinical use on many subtests. Analyses of group effect sizes, discrimination, and sensitivity and specificity suggested that the CNTs may add incrementally (beyond symptom scores) to the identification of clinical impairment within 24 hr of injury or within a short time period after symptom resolution but do not add significant value over symptom assessment later. The rapid clinical recovery course from concussion and modest stability probably jointly contribute to limited signal detection capabilities of neurocognitive tests outside a brief post-injury window. (JINS, 2016, 22, 24-37).

Prospective, Head-to-Head Study of Three Computerized Neurocognitive Assessment Tools (CNTs): Reliability and Validity for the Assessment of Sport-Related Concussion

PubMed Central

Nelson, Lindsay D.; LaRoche, Ashley A.; Pfaller, Adam Y.; Lerner, E. Brooke; Hammeke, Thomas A.; Randolph, Christopher; Barr, William B.; Guskiewicz, Kevin; McCrea, Michael A.

2016-01-01

Limited data exist comparing the performance of computerized neurocognitive tests (CNTs) for assessing sport-related concussion. We evaluated the reliability and validity of three CNTs—ANAM, Axon Sports/Cogstate Sport, and ImPACT—in a common sample. High school and collegiate athletes completed two CNTs each at baseline. Concussed (n = 165) and matched non-injured control (n = 166) subjects repeated testing within 24 hr and at 8, 15, and 45 days post-injury. Roughly a quarter of each CNT's indices had stability coefficients (M = 198 day interval) over .70. Group differences in performance were mostly moderate to large at 24 hr and small by day 8. The sensitivity of reliable change indices (RCIs) was best at 24 hr (67.8%, 60.3%, and 47.6% with one or more significant RCIs for ImPACT, Axon, and ANAM, respectively) but diminished to near the false positive rates thereafter. Across time, the CNTs' sensitivities were highest in those athletes who became asymptomatic within 1 day before neurocognitive testing but was similar to the tests' false positive rates when including athletes who became asymptomatic several days earlier. Test–retest reliability was similar among these three CNTs and below optimal standards for clinical use on many subtests. Analyses of group effect sizes, discrimination, and sensitivity and specificity suggested that the CNTs may add incrementally (beyond symptom scores) to the identification of clinical impairment within 24 hr of injury or within a short time period after symptom resolution but do not add significant value over symptom assessment later. The rapid clinical recovery course from concussion and modest stability probably jointly contribute to limited signal detection capabilities of neurocognitive tests outside a brief post-injury window. PMID:26714883

Development of a validated HPLC method for the quantitative determination of trelagliptin succinate and its related substances in pharmaceutical dosage forms.

PubMed

Luo, Zhiqiang; Chen, Xinjing; Wang, Guopeng; Du, Zhibo; Ma, Xiaoyun; Wang, Hao; Yu, Guohua; Liu, Aoxue; Li, Mengwei; Peng, Wei; Liu, Yang

2018-01-01

Trelagliptin succinate is a dipeptidyl peptidase IV (DPP-4) inhibitor which is used as a new long-acting drug for once-weekly treatment of type 2 diabetes mellitus (DM). In the present study, a rapid, sensitive and accurate high-performance liquid chromatography (HPLC) method was developed and validated for separation and determination of trelagliptin succinate and its eight potential process-related impurities. The chromatographic separation was achieved on a Waters Xselect CSH™ C 18 (250mm×4.6mm, 5.0μm) column. The mobile phases comprised of 0.05% trifluoroacetic acid in water as well as acetonitrile containing 0.05% trifluoroacetic acid. The compounds of interest were monitored at 224nm and 275nm. The stability-indicating capability of this method was evaluated by performing stress test studies. Trelagliptin succinate was found to degrade significantly in acid, base, oxidative and thermal stress conditions and only stable in photolytic degradation condition. The degradation products were well resolved from the main peak and its impurities. In addition, the major degradation impurities formed under acid, base, oxidative and thermal stress conditions were characterized by ultra-high-performance liquid chromatography coupled with linear ion trap-Orbitrap tandem mass spectrometry (UHPLC-LTQ-Orbitrap). The method was validated to fulfill International Conference on Harmonisation (ICH) requirements and this validation included specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision and robustness. The developed method in this study could be applied for routine quality control analysis of trelagliptin succinate tablets, since there is no official monograph. Copyright © 2017 Elsevier B.V. All rights reserved.

Development and validation of an abbreviated version of the Trust in Oncologist Scale-the Trust in Oncologist Scale-short form (TiOS-SF).

PubMed

Hillen, Marij A; Postma, Rosa-May; Verdam, Mathilde G E; Smets, Ellen M A

2017-03-01

The original 18-item, four-dimensional Trust in Oncologist Scale assesses cancer patients' trust in their oncologist. The current aim was to develop and validate a short form version of the scale to enable more efficient assessment of cancer patients' trust. Existing validation data of the full-length Trust in Oncologist Scale were used to create a short form of the Trust in Oncologist Scale. The resulting short form was validated in a new sample of cancer patients (n = 92). Socio-demographics, medical characteristics, trust in the oncologist, satisfaction with communication, trust in healthcare, willingness to recommend the oncologist to others and to contact the oncologist in case of questions were assessed. Internal consistency, reliability, convergent and structural validity were tested. The five-item Trust in Oncologist Scale Short Form was created by selecting the statistically best performing item from each dimension of the original scale, to ensure content validity. Mean trust in the oncologist was high in the validation sample (response rate 86%, M = 4.30, SD = 0.98). Exploratory factor analyses supported one-dimensionality of the short form. Internal consistency was high, and temporal stability was moderate. Initial convergent validity was suggested by moderate correlations between trust scores with associated constructs. The Trust in Oncologist Scale Short Form appears to efficiently, reliably and validly measures cancer patients' trust in their oncologist. It may be used in research and as a quality indicator in clinical practice. More thorough validation of the scale is recommended to confirm this initial evidence of its validity.

Nursing Intensive-Care Satisfaction Scale [NICSS]: Development and validation of a patient-centred instrument.

PubMed

Romero-García, Marta; de la Cueva-Ariza, Laura; Benito-Aracil, Llucia; Lluch-Canut, Teresa; Trujols-Albet, Joan; Martínez-Momblan, Maria Antonia; Juvé-Udina, Maria-Eulàlia; Delgado-Hito, Pilar

2018-06-01

The aim of this study was to develop and validate the Nursing Intensive-Care Satisfaction Scale to measures satisfaction with nursing care from the critical care patient's perspective. Instruments that measure satisfaction with nursing cares have been designed and validated without taking the patient's perspective into consideration. Despite the benefits and advances in measuring satisfaction with nursing care, none instrument is specifically designed to assess satisfaction in intensive care units. Instrument development. The population were all discharged patients (January 2013 - January 2015) from three Intensive Care Units of a third level hospital (N = 200). All assessment instruments were given to discharged patients and 48 hours later, to analyse the temporal stability, only the questionnaire was given again. The validation process of the scale included the analysis of internal consistency, temporal stability; validity of construct through a confirmatory factor analysis; and criterion validity. Reliability was 0.95. The intraclass correlation coefficient for the total scale was 0.83 indicating a good temporal stability. Construct validity showed an acceptable fit and factorial structure with four factors, in accordance with the theoretical model, being Consequences factor the best correlated with other factors. Criterion validity, presented a correlation between low and high (range: 0.42-0.68). The scale has been designed and validated incorporating the perspective of critical care patients. Thanks to its reliability and validity, this questionnaire can be used both in research and in clinical practice. The scale offers a possibility to assess and develop interventions to improve patient satisfaction with nursing care. © 2018 John Wiley & Sons Ltd.

Development and Validation of Stability-Indicating Derivative Spectrophotometric Methods for Determination of Dronedarone Hydrochloride

NASA Astrophysics Data System (ADS)

Chadha, R.; Bali, A.

2016-05-01

Rapid, sensitive, cost effective and reproducible stability-indicating derivative spectrophotometric methods have been developed for the estimation of dronedarone HCl employing peak-zero (P-0) and peak-peak (P-P) techniques, and their stability-indicating potential assessed in forced degraded solutions of the drug. The methods were validated with respect to linearity, accuracy, precision and robustness. Excellent linearity was observed in concentrations 2-40 μg/ml ( r 2 = 0.9986). LOD and LOQ values for the proposed methods ranged from 0.42-0.46 μg/ml and 1.21-1.27 μg/ml, respectively, and excellent recovery of the drug was obtained in the tablet samples (99.70 ± 0.84%).

Analytical Stability-Indicating Methods for Alogliptin in Tablets by LC-CAD and LC-UV.

PubMed

Bertol, Charise Dallazem; Friedrich, Maria Tereza; Carlos, Graciela; Froehlich, Pedro Eduardo

2017-03-01

Stability-indicating LC methods using a UV detector and a charged aerosol detector (CAD) simultaneously were validated for the assessment of alogliptin (ALG) in tablets. The analysis was performed on a C8 column (250 × 4.6 mm, 5 μm) at a flow of 0.8 mL/min, using acetonitrile-10 mM ammonium acetate buffer (pH 3.5; 90 + 10, v/v) as mobile phase and UV detection at 275 nm. Validation followed the International Conference on Harmonization guidelines. The method was linear over the range of 25-200 μg/mL. Normality of the residuals showed a normal distribution, no autocorrelation, and homoscedasticity. LODs were 6.25 and 2.65 µg/mL and LOQs were 20.85 and 8.84 µg/mL for the CAD and the UV detector, respectively. The methods were precise and accurate. Excipients and degradation products did not interfere in the methods in studies of specificity. None of the factors studied in the analysis of robustness had a significant effect on the quantification of the ALG by the Pareto chart. The results of the assay obtained with LC-CAD and LC-UV were similar. The methods could be considered interchangeable and stability-indicating, and can be applied as an appropriate QC tool for analysis of ALG in tablets.

Development and validation of a novel stability-indicating HPLC method for the quantitative determination of eleven related substances in ezetimibe drug substance and drug product.

PubMed

Luo, Zhiqiang; Deng, Zhongqing; Liu, Yang; Wang, Guopeng; Yang, Wenning; Hou, Chengbo; Tang, Minming; Yang, Ruirui; Zhou, Huaming

2015-07-01

Ezetimibe is a novel lipid-lowering agent that inhibits intestinal absorption of dietary and biliary cholesterol. In the present work, a simple, sensitive and reproducible gradient reverse phase high performance liquid chromatographic (RP-HPLC) method for separation and determination of the related substances of ezetimibe was developed and validated. Eleven potential process-related impurities (starting materials, (3S,4S,3'S)-isomer, degradants and byproducts) were identified in the crude samples. Tentative structures for all the impurities were assigned primarily based on comparison of their retention time and mass spectrometric data with that of available standards and references. This method can be applied to routine analysis in quality control of both bulk drugs and commercial tablets. Separation of all these compounds was performed on a Phenomenex Luna Phenyl-Hexyl (100mm×4.6mm, 5μm) analytical column. The mobile phase-A consists of acetonitrile-water (pH adjusted to 4.0 with phosphoric acid)-methanol at 15:75:10 (v/v/v), and mobile phase-B contains acetonitrile. The eluted compounds were monitored at 210nm. Ezetimibe was subjected to hydrolytic, acid, base, oxidative, photolytic and thermal stress conditions as per ICH serves to generate degradation products that can be used as a worst case to assess the analytical method performance. The drug showed extensive degradation in thermal, acid, oxidative, base and hydrolytic stress conditions, while it was stable to photolytic degradation conditions. The main degradation product formed under thermal, acid, oxidative, base and hydrolytic stress conditions corresponding to (2R,3R,6S)-N, 6-bis(4-fluorophenyl)-2-(4-hydroxyphenyl)-oxane-3-carboxamide (Ezetimibe tetrahydropyran impurity) was characterized by LC-MS/MS analysis. The degradation products were well resolved from the main peak and its impurities, thus proved the stability-indicating power of the method. The developed method was validated as per international conference on harmonization (ICH) guidelines with respect to specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision and robustness. Copyright © 2015 Elsevier B.V. All rights reserved.

Validation of the solidifying soil process using laser-induced breakdown spectroscopy

NASA Astrophysics Data System (ADS)

Lin, Zhao-Xiang; Liu, Lin-Mei; Liu, Lu-Wen

2016-09-01

Although an Ionic Soil Stabilizer (ISS) has been widely used in landslide control, it is desirable to effectively monitor the stabilization process. With the application of laser-induced breakdown spectroscopy (LIBS), the ion contents of K, Ca, Na, Mg, Al, and Si in the permeable fluid are detected after the solidified soil samples have been permeated. The processes of the Ca ion exchange are analyzed at pressures of 2 and 3 atm, and it was determined that the cation exchanged faster as the pressure increased. The Ca ion exchanges were monitored for different stabilizer mixtures, and it was found that a ratio of 1:200 of ISS to soil is most effective. The investigated plasticity and liquidity indexes also showed that the 1:200 ratio delivers the best performance. The research work indicates that it is possible to evaluate the engineering performances of soil solidified by ISS in real time and online by LIBS.

Early Identification of Children at Risk for Academic Difficulties Using Standardized Assessment: Stability and Predictive Validity of Preschool Math and Language Scores

ERIC Educational Resources Information Center

Frans, Niek; Post, Wendy J.; Huisman, Mark; Oenema-Mostert, Ineke C. E.; Keegstra, Anne L.; Minnaert, Alexander E. M. G.

2017-01-01

Despite the claim by several researchers that variability in performance may complicate the identification of "at-risk" children, variability in the academic performance of young children remains an undervalued area of research. The goal of this study is to examine the predictive validity for future scores and the score stability of two…

Determination of vitamin C in foods: current state of method validation.

PubMed

Spínola, Vítor; Llorent-Martínez, Eulogio J; Castilho, Paula C

2014-11-21

Vitamin C is one of the most important vitamins, so reliable information about its content in foodstuffs is a concern to both consumers and quality control agencies. However, the heterogeneity of food matrixes and the potential degradation of this vitamin during its analysis create enormous challenges. This review addresses the development and validation of high-performance liquid chromatography methods for vitamin C analysis in food commodities, during the period 2000-2014. The main characteristics of vitamin C are mentioned, along with the strategies adopted by most authors during sample preparation (freezing and acidification) to avoid vitamin oxidation. After that, the advantages and handicaps of different analytical methods are discussed. Finally, the main aspects concerning method validation for vitamin C analysis are critically discussed. Parameters such as selectivity, linearity, limit of quantification, and accuracy were studied by most authors. Recovery experiments during accuracy evaluation were in general satisfactory, with usual values between 81 and 109%. However, few methods considered vitamin C stability during the analytical process, and the study of the precision was not always clear or complete. Potential future improvements regarding proper method validation are indicated to conclude this review. Copyright © 2014. Published by Elsevier B.V.

Short- and longtime stability of therapeutic ultrasound reference sources for dosimetry and exposimetry purposes

NASA Astrophysics Data System (ADS)

Haller, J.; Wilkens, V.

2017-03-01

The objective of this work was to create highly stable therapeutic ultrasound fields with well-known exposimetry and dosimetry parameters that are reproducible and hence predictable with well-known uncertainties. Such well- known and reproducible fields would allow validation and secondary calibrations of different measuring capabilities, which is already a widely accepted strategy for diagnostic fields. For this purpose, a reference setup was established that comprises two therapeutic ultrasound sources (one High-Intensity Therapeutic Ultrasound (HITU) source and one physiotherapy-like source), standard rf electronics for signal creation, and computer-controlled feedback to stabilize the input voltage. The short- and longtime stability of the acoustic output were evaluated - for the former, measurements over typical laboratory measurement time periods (i.e. some seconds or minutes) of the input voltage stability with and without feedback control were performed. For the latter, measurements of typical acoustical exposimetry parameters were performed bimonthly over one year. The measurement results show that the short- and the longtime stability of the reference setup are very good and that it is especially significantly improved in comparison to a setup without any feedback control.

Euclidean distance and Kolmogorov-Smirnov analyses of multi-day auditory event-related potentials: a longitudinal stability study

NASA Astrophysics Data System (ADS)

Durato, M. V.; Albano, A. M.; Rapp, P. E.; Nawang, S. A.

2015-06-01

The validity of ERPs as indices of stable neurophysiological traits is partially dependent on their stability over time. Previous studies on ERP stability, however, have reported diverse stability estimates despite using the same component scoring methods. This present study explores a novel approach in investigating the longitudinal stability of average ERPs—that is, by treating the ERP waveform as a time series and then applying Euclidean Distance and Kolmogorov-Smirnov analyses to evaluate the similarity or dissimilarity between the ERP time series of different sessions or run pairs. Nonlinear dynamical analysis show that in the absence of a change in medical condition, the average ERPs of healthy human adults are highly longitudinally stable—as evaluated by both the Euclidean distance and the Kolmogorov-Smirnov test.

Validation of a high performance liquid chromatography method for the stabilization of epigallocatechin gallate.

PubMed

Fangueiro, Joana F; Parra, Alexander; Silva, Amélia M; Egea, Maria A; Souto, Eliana B; Garcia, Maria L; Calpena, Ana C

2014-11-20

Epigallocatechin gallate (EGCG) is a green tea catechin with potential health benefits, such as anti-oxidant, anti-carcinogenic and anti-inflammatory effects. In general, EGCG is highly susceptible to degradation, therefore presenting stability problems. The present paper was focused on the study of EGCG stability in HEPES (N-2-hydroxyethylpiperazine-N'-2-ethanesulfonic acid) medium regarding the pH dependency, storage temperature and in the presence of ascorbic acid a reducing agent. The evaluation of EGCG in HEPES buffer has demonstrated that this molecule is not able of maintaining its physicochemical properties and potential beneficial effects, since it is partially or completely degraded, depending on the EGCG concentration. The storage temperature of EGCG most suitable to maintain its structure was shown to be the lower values (4 or -20 °C). The pH 3.5 was able to provide greater stability than pH 7.4. However, the presence of a reducing agent (i.e., ascorbic acid) was shown to provide greater protection against degradation of EGCG. A validation method based on RP-HPLC with UV-vis detection was carried out for two media: water and a biocompatible physiological medium composed of Transcutol®P, ethanol and ascorbic acid. The quantification of EGCG for purposes, using pure EGCG, requires a validated HPLC method which could be possible to apply in pharmacokinetic and pharmacodynamics studies. Copyright © 2014. Published by Elsevier B.V.

Stability of alemtuzumab solutions at room temperature.

PubMed

Goldspiel, Justin T; Goldspiel, Barry R; Grimes, George J; Yuan, Peng; Potti, Gopal

2013-03-01

The 24-hour stability of alemtuzumab solutions prepared at concentrations not included in the product label and stored in glass or polyolefin containers at room temperature was evaluated. Triplicate solutions of alemtuzumab (6.67, 40, and 120 μg/mL) in 0.9% sodium chloride were prepared in either glass bottles or polyolefin containers and stored at room temperature under normal fluorescent lighting conditions. The solutions were analyzed by a validated stability-indicating high-performance liquid chromatography (HPLC) assay at time zero and 8, 14, and 24 hours after preparation; solution pH values were measured and the containers visually inspected at all time points. Stability was defined as the retention of ≥90% of the initial alemtuzumab concentration. HPLC analysis indicated that the percentage of the initial alemtuzumab concentration retained was >90% for all solutions evaluated, with no significant changes over the study period. The most dilute alemtuzumab solution (6.67 μg/mL) showed some degradation (91% of the initial concentration retained at hour 24), whereas the retained concentration was >99% for all other preparations throughout the study period. Solution pH values varied by drug concentration but did not change significantly over 24 hours. No evidence of particle formation was detected in any solution by visual inspection at any time during the study. Solutions of alemtuzumab 6.67 μg/mL stored in glass bottles and solutions of 40 and 120 μg/mL stored in polyolefin containers were stable for at least 24 hours at room temperature.

High-resolution computational algorithms for simulating offshore wind turbines and farms: Model development and validation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Calderer, Antoni; Yang, Xiaolei; Angelidis, Dionysios

2015-10-30

The present project involves the development of modeling and analysis design tools for assessing offshore wind turbine technologies. The computational tools developed herein are able to resolve the effects of the coupled interaction of atmospheric turbulence and ocean waves on aerodynamic performance and structural stability and reliability of offshore wind turbines and farms. Laboratory scale experiments have been carried out to derive data sets for validating the computational models.

How do Stability Corrections Perform in the Stable Boundary Layer Over Snow?

NASA Astrophysics Data System (ADS)

Schlögl, Sebastian; Lehning, Michael; Nishimura, Kouichi; Huwald, Hendrik; Cullen, Nicolas J.; Mott, Rebecca

2017-10-01

We assess sensible heat-flux parametrizations in stable conditions over snow surfaces by testing and developing stability correction functions for two alpine and two polar test sites. Five turbulence datasets are analyzed with respect to, (a) the validity of the Monin-Obukhov similarity theory, (b) the model performance of well-established stability corrections, and (c) the development of new univariate and multivariate stability corrections. Using a wide range of stability corrections reveals an overestimation of the turbulent sensible heat flux for high wind speeds and a generally poor performance of all investigated functions for large temperature differences between snow and the atmosphere above (>10 K). Applying the Monin-Obukhov bulk formulation introduces a mean absolute error in the sensible heat flux of 6 W m^{-2} (compared with heat fluxes calculated directly from eddy covariance). The stability corrections produce an additional error between 1 and 5 W m^{-2}, with the smallest error for published stability corrections found for the Holtslag scheme. We confirm from previous studies that stability corrections need improvements for large temperature differences and wind speeds, where sensible heat fluxes are distinctly overestimated. Under these atmospheric conditions our newly developed stability corrections slightly improve the model performance. However, the differences between stability corrections are typically small when compared to the residual error, which stems from the Monin-Obukhov bulk formulation.

Adaptability and stability of soybean genotypes in off-season cultivation.

PubMed

Batista, R O; Hamawaki, R L; Sousa, L B; Nogueira, A P O; Hamawaki, O T

2015-08-14

The oil and protein contents of soybean grains are important quantitative traits for use in breeding. However, few breeding programs perform selection based on these traits in different environments. This study assessed the adaptability and stability of 14 elite early soybean breeding lines in off-season cultivation with respect to yield, and oil and protein contents. A range of statistical methods was applied and these analyses indicated that for off-season cultivation, the lines UFUS 5 and UFUS 10 could be recommended due to their superior performance in grain yield, oil content, and specific adaptability to unfavorable environments along with high stability in these characteristics. Also recommended were UFUS 06, which demonstrated superior performance in all three tested characteristics and showed adaptation to favorable environments, and UFUS 13, which showed high adaptability and stability and a superior performance for protein content.

Development and validation of a reversed-phase ion-pair high-performance liquid chromatographic method for the determination of risedronate in pharmaceutical preparations.

PubMed

Kyriakides, Demetra; Panderi, Irene

2007-02-12

A stability indicating, reversed-phase ion-pair high-performance liquid chromatographic method was developed and validated for the determination of risedronate in pharmaceutical dosage forms. The determination was performed on a BDS C(18) analytical column (250 mm x 4.6 mm i.d., 5 microm particle size); the mobile phase consisted of 0.005 M tetrabutylammonium hydroxide and 0.005 M pyrophosphate sodium (pH 7.0) mixed with acetonitrile in a ratio (78:22, v/v) and pumped at a flow rate 1.00 mL min(-1). The ultraviolet (UV) detector was operated at 262 nm. The retention times of magnesium ascorbyl phosphate, which was used as internal standard and risedronate were 4.94 and 5.95 min, respectively. The calibration graph was ranged from 2.50 to 20.00 microg mL(-1), while detection and quantitation limits were found to be 0.48 and 1.61 microg mL(-1), respectively. The intra- and inter-day percentage relative standard deviations, %R.S.D., were less than 5.9%, while the relative percentage error, %E(r), was less than 0.4%. The method was applied to the quality control of commercial tablets and content uniformity test and proved to be suitable for rapid and reliable quality control.

[Maslach Burnout Inventory - Student Survey: Portugal-Brazil cross-cultural adaptation].

PubMed

Campos, Juliana Alvares Duarte Bonini; Maroco, João

2012-10-01

To perform a cross-cultural adaptation of the Portuguese version of the Maslach Burnout Inventory for students (MBI-SS), and investigate its reliability, validity and cross-cultural invariance. The face validity involved the participation of a multidisciplinary team. Content validity was performed. The Portuguese version was completed in 2009, on the internet, by 958 Brazilian and 556 Portuguese university students from the urban area. Confirmatory factor analysis was carried out using as fit indices: the χ²/df, the Comparative Fit Index (CFI), the Goodness of Fit Index (GFI) and the Root Mean Square Error of Approximation (RMSEA). To verify the stability of the factor solution according to the original English version, cross-validation was performed in 2/3 of the total sample and replicated in the remaining 1/3. Convergent validity was estimated by the average variance extracted and composite reliability. The discriminant validity was assessed, and the internal consistency was estimated by the Cronbach's alpha coefficient. Concurrent validity was estimated by the correlational analysis of the mean scores of the Portuguese version and the Copenhagen Burnout Inventory, and the divergent validity was compared to the Beck Depression Inventory. The invariance of the model between the Brazilian and the Portuguese samples was assessed. The three-factor model of Exhaustion, Disengagement and Efficacy showed good fit (c 2/df = 8.498, CFI = 0.916, GFI = 0.902, RMSEA = 0.086). The factor structure was stable (λ:χ²dif = 11.383, p = 0.50; Cov: χ²dif = 6.479, p = 0.372; Residues: χ²dif = 21.514, p = 0.121). Adequate convergent validity (VEM = 0.45;0.64, CC = 0.82;0.88), discriminant (ρ² = 0.06;0.33) and internal consistency (α = 0.83;0.88) were observed. The concurrent validity of the Portuguese version with the Copenhagen Inventory was adequate (r = 0.21, 0.74). The assessment of the divergent validity was impaired by the approach of the theoretical concept of the dimensions Exhaustion and Disengagement of the Portuguese version with the Beck Depression Inventory. Invariance of the instrument between the Brazilian and Portuguese samples was not observed (λ:χ²dif = 84.768, p<0.001; Cov: χ²dif = 129.206, p < 0.001; Residues: χ²dif = 518.760, p < 0.001). The Portuguese version of the Maslach Burnout Inventory for students showed adequate reliability and validity, but its factor structure was not invariant between the countries, indicating the absence of cross-cultural stability.

The Stroop test as a measure of performance validity in adults clinically referred for neuropsychological assessment.

PubMed

Erdodi, Laszlo A; Sagar, Sanya; Seke, Kristian; Zuccato, Brandon G; Schwartz, Eben S; Roth, Robert M

2018-06-01

This study was designed to develop performance validity indicators embedded within the Delis-Kaplan Executive Function Systems (D-KEFS) version of the Stroop task. Archival data from a mixed clinical sample of 132 patients (50% male; M Age = 43.4; M Education = 14.1) clinically referred for neuropsychological assessment were analyzed. Criterion measures included the Warrington Recognition Memory Test-Words and 2 composites based on several independent validity indicators. An age-corrected scaled score ≤6 on any of the 4 trials reliably differentiated psychometrically defined credible and noncredible response sets with high specificity (.87-.94) and variable sensitivity (.34-.71). An inverted Stroop effect was less sensitive (.14-.29), but comparably specific (.85-90) to invalid performance. Aggregating the newly developed D-KEFS Stroop validity indicators further improved classification accuracy. Failing the validity cutoffs was unrelated to self-reported depression or anxiety. However, it was associated with elevated somatic symptom report. In addition to processing speed and executive function, the D-KEFS version of the Stroop task can function as a measure of performance validity. A multivariate approach to performance validity assessment is generally superior to univariate models. (PsycINFO Database Record (c) 2018 APA, all rights reserved).

A comparative pharmacokinetic study of three flavonoids and three anthraquinones in normal and gastrointestinal motility disorders rat plasma after the oral administration of Wei-Chang-Shu tablet using high-performance liquid chromatography-tandem mass spectrometry.

PubMed

Ren, Yan; Zhao, Weiwei; Zhao, Juanjuan; Chen, Xiangming; Yu, Chen; Liu, Mengan

2017-11-01

A simple, fast and reliable high-performance liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous quantification and pharmacokinetic study of three flavonoids (liquiritigenin, isoliquiritigenin and formononetin) and three anthraquinones (emodin, rhein and aloe-emodin), which are the bioactive ingredients of Wei-Chang-Shu tablet found in rat plasma. After extraction by liquid-liquid extraction with ethyl acetate, chromatographic separation was achieved on an Agilent Zorbax SB-C 18 column (4.6 × 150 mm, 5 μm) at a flow rate of 1 mL/min by gradient elution using 0.1% aqueous acetic acid and acetonitrile. The detection was performed using a triple quadrupole mass spectrometer equipped with electrospray ionization source in the negative ionization and selected reaction monitoring mode. Method validation was performed in terms of specificity, carryover, linearity (r > 0.99), intra-/inter-day precision (1.0-10.1%), accuracy (relative error, <7.6%), stability (0.6-13.2%), extract recovery (74.9-91.9%) and matrix effect (89.1-109%). The lower limits of quantification of the six analytes varied from 0.92 to 10.4 ng/mL. The validated method was successfully applied to compare the pharmacokinetic properties of Wei-Chang-Shu tablet in normal rats and in rats with gastrointestinal motility disorders. The results indicated that there were obvious differences in the pharmacokinetic behavior between normal and model rats. This study will be helpful in the clinical application of Wei-Chang-Shu tablet. Copyright © 2017 John Wiley & Sons, Ltd.

Longitudinal data analysis in support of functional stability concepts for leachate management at closed municipal landfills

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gibbons, Robert D., E-mail: rdg@uchicago.edu; Morris, Jeremy W.F., E-mail: jmorris@geosyntec.com; Prucha, Christopher P., E-mail: cprucha@wm.com

2014-09-15

Highlights: • Longitudinal data analysis using a mixed-effects regression model. • Dataset consisted of a total of 1402 samples from 101 closed municipal landfills. • Target analytes and classes generally showed predictable degradation trends. • Validates historical studies focused on macro organic indicators such as BOD. • BOD can serve as “gateway” indicator for planning leachate management. - Abstract: Landfill functional stability provides a target that supports no environmental threat at the relevant point of exposure in the absence of active control systems. With respect to leachate management, this study investigates “gateway” indicators for functional stability in terms of themore » predictability of leachate characteristics, and thus potential threat to water quality posed by leachate emissions. Historical studies conducted on changes in municipal solid waste (MSW) leachate concentrations over time (longitudinal analysis) have concentrated on indicator compounds, primarily chemical oxygen demand (COD) and biochemical oxygen demand (BOD). However, validation of these studies using an expanded database and larger constituent sets has not been performed. This study evaluated leachate data using a mixed-effects regression model to determine the extent to which leachate constituent degradation can be predicted based on waste age or operational practices. The final dataset analyzed consisted of a total of 1402 samples from 101 MSW landfills. Results from the study indicated that all leachate constituents exhibit a decreasing trend with time in the post-closure period, with 16 of the 25 target analytes and aggregate classes exhibiting a statistically significant trend consistent with well-studied indicators such as BOD. Decreasing trends in BOD concentration after landfill closure can thus be considered representative of trends for many leachate constituents of concern.« less

Development and validation of a ultra high performance liquid chromatography-tandem mass spectrometric method for the direct detection of formoterol in human urine.

PubMed

Sardela, V F; Deventer, K; Pereira, H M G; de Aquino Neto, F R; Van Eenoo, P

2012-11-01

Formoterol is a long acting β(2)-agonist and has proven to be a very effective bronchodilating agent. Hence it is frequently applied therapeutically for the treatment of asthma. Because β(2)-agonists might be misused in sports for the stimulatory effects and for growth-promoting action their use is restricted. Since January 2012, formoterol is prohibited in urinary concentrations higher than 30 ng/mL. The objective of this study was to develop and validate a simple and robust ultra high performance liquid chromatographic-tandem mass spectrometric (UHPLC-MS/MS) method for the direct quantification of formoterol in urine. Sample preparation was limited to an enzymatic hydrolysis step after which 2 μL was injected in the chromatographic system. Chromatography was performed on a C(8)-column using gradient conditions. The mobile phase consisted of water/methanol (H(2)O/MeOH) both containing 0.1% acetic acid (HOAc) and 1mM ammonium acetate (NH(4)OAc). Calibration curve were constructed between 15 and 60 ng/mL. Validation data showed bias of 1.3% and imprecision of 5.4% at the threshold. Ion suppression/enhancement never exceeded 7%. Calculating measurement uncertainty showed proof of applicability of the method. Stability of formoterol was also investigated at 56 °C (accelerated stability test) at pH 1.0/5.2/7.0 and 9.5. At the physiological pH values of 5.2 and 7.0, formoterol showed good stability. At pH 1.0 and 9.5 significant degradation was observed. Copyright © 2012 Elsevier B.V. All rights reserved.

Cultural adaptation of an instrument to assess physical fitness in cardiac patients.

PubMed

Domingues, Gabriela de Barros Leite; Gallani, Maria Cecília; Gobatto, Claudio Alexandre; Miura, Cinthya Tamie Passos; Rodrigues, Roberta Cunha Matheus; Myers, Jonathan

2011-04-01

To validate the content and to evaluate the reliability of the Veterans Specific Activity Questionnaire instrument, culturally adapted for use in the Brazilian population of cardiac patients. The instrument was translated and back-translated and subsequently analyzed by a committee of judges to evaluate its semantic-idiomatic and cultural equivalences. Physical activities were replaced when indicated in the instrument, but uncommon in the daily life of the target population. Another committee of specialists analyzed the metabolic equivalence of replaced activities. The proportion of agreement of evaluation of the judges was quantified by the Content Validity Index. The pre-test was performed in two stages (n1 and n2=15). Reliability was assessed using the test-retest (interval of 7-15 days, n = 50). In the evaluation of semantic-idiomatic and cultural equivalences, items with a Content Validity Index < 1 were reviewed until consensus among the judges was obtained. The second committee found 100% of agreement in the analysis of metabolic equivalence between original and replaced activities. Test-retest analysis indicated a Kappa coefficient of agreement (k = 0.86; (p<0.001), suggesting temporal stability of the instrument. The Brazilian version of the Veterans Specific Activity Questionnaire showed evidence of reliability, according to the temporal stability criterion and adequate cultural content.

Development of a job stressor scale for nurses caring for patients with intractable neurological diseases.

PubMed

Ando, Yukako; Kataoka, Tsuyoshi; Okamura, Hitoshi; Tanaka, Katsutoshi; Kobayashi, Toshio

2013-12-01

The purpose of this research is to verify the reliability and validity of a job stressor scale for nurses caring for patients with intractable neurological diseases. A mail survey was conducted using a self-report questionnaire. The subjects were 263 nurses and assistant nurses working in wards specializing in intractable neurological diseases. The response rate was 71.9% (valid response rate, 66.2%). With regard to reliability, internal consistency and stability were assessed. Internal consistency was examined via Cronbach's alpha. For stability, the test-retest method was performed and stability was examined via intraclass correlation coefficients. With regard to validity, factor validity, criterion-related validity, and content validity were assessed. Exploratory factor analysis was used for factor validity. For criterion-related validity, an existing scale was used as an external criterion; concurrent validity was examined via Spearman's rank correlation coefficients. As a result of analysis, there were 26 items in the scale created with an eight factor structure. Cronbach's a for the 26 items was 0.90; with the exception of two factors, alpha for all of the individual sub-factors was high at 0.7 or higher. The intraclass correlation coefficient for the 26 items was 0.89 (p < 0.001). With regard to criterion-related validity, concurrent validity was confirmed and the correlation coefficient with an external criterion was 0.73 (p < 0.001). For content validity, subjects who responded that "The questionnaire represents a stressor well or to a degree" accounted for 81% of the total responses. Reliability and validity were confirmed, so the scale created in the current research is a usable scale.

Nonlinear stability and control study of highly maneuverable high performance aircraft, phase 2

NASA Technical Reports Server (NTRS)

Mohler, R. R.

1992-01-01

Research leading to the development of new nonlinear methodologies for the adaptive control and stability analysis of high angle of attack aircraft such as the F-18 is discussed. The emphasis has been on nonlinear adaptive control, but associated model development, system identification, stability analysis, and simulation were studied in some detail as well. Studies indicated that nonlinear adaptive control can outperform linear adaptive control for rapid maneuvers with large changes in angle of attack. Included here are studies on nonlinear model algorithmic controller design and an analysis of nonlinear system stability using robust stability analysis for linear systems.

Application of quality by design concept to develop a dual gradient elution stability-indicating method for cloxacillin forced degradation studies using combined mixture-process variable models.

PubMed

Zhang, Xia; Hu, Changqin

2017-09-08

Penicillins are typical of complex ionic samples which likely contain large number of degradation-related impurities (DRIs) with different polarities and charge properties. It is often a challenge to develop selective and robust high performance liquid chromatography (HPLC) methods for the efficient separation of all DRIs. In this study, an analytical quality by design (AQbD) approach was proposed for stability-indicating method development of cloxacillin. The structures, retention and UV characteristics rules of penicillins and their impurities were summarized and served as useful prior knowledge. Through quality risk assessment and screen design, 3 critical process parameters (CPPs) were defined, including 2 mixture variables (MVs) and 1 process variable (PV). A combined mixture-process variable (MPV) design was conducted to evaluate the 3 CPPs simultaneously and a response surface methodology (RSM) was used to achieve the optimal experiment parameters. A dual gradient elution was performed to change buffer pH, mobile-phase type and strength simultaneously. The design spaces (DSs) was evaluated using Monte Carlo simulation to give their possibility of meeting the specifications of CQAs. A Plackett-Burman design was performed to test the robustness around the working points and to decide the normal operating ranges (NORs). Finally, validation was performed following International Conference on Harmonisation (ICH) guidelines. To our knowledge, this is the first study of using MPV design and dual gradient elution to develop HPLC methods and improve separations for complex ionic samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Stability of steviol glycosides in several food matrices.

PubMed

Jooken, Etienne; Amery, Ruis; Struyf, Tom; Duquenne, Barbara; Geuns, Jan; Meesschaert, Boudewijn

2012-10-24

As steviol glycosides are now allowed as a food additive in the European market, it is important to assess the stability of these steviol glycosides after they have been added to different food matrices. We analyzed and tested the stability of steviol glycosides in semiskimmed milk, soy drink, fermented milk drink, ice cream, full-fat and skimmed set yogurt, dry biscuits, and jam. The fat was removed by centrifugation from the dairy and soy drink samples. Proteins were precipitated by the addition of acetonitrile and also removed by centrifugation. Samples of jam were extracted with water. Dry biscuits were extracted with ethanol. The resulting samples were concentrated with solid-phase extraction and analyzed by high-performance liquid chromatography on a C18 stationary phase and a gradient of acetonitrile/aqueous 25 mM phosphoric acid. The accuracy was checked using a standard addition on some samples. For assessing the stability of the steviol glycosides, samples were stored in conditions relevant to each food matrix and analyzed periodically. The results indicate that steviol glycosides can be analyzed with good precision and accuracy in these food categories. The recovery was between 96 and 103%. The method was also validated by standard addition, which showed excellent agreement with the external calibration curve. No sign of decomposition of steviol glycosides was found in any of the samples.

An Improved LC-ESI-MS/MS Method to Quantify Pregabalin in Human Plasma and Dry Plasma Spot for Therapeutic Monitoring and Pharmacokinetic Applications.

PubMed

Dwivedi, Jaya; Namdev, Kuldeep K; Chilkoti, Deepak C; Verma, Surajpal; Sharma, Swapnil

2018-06-06

Therapeutic drug monitoring (TDM) of anti-epileptic drugs provides a valid clinical tool in optimization of overall therapy. However, TDM is challenging due to the high biological samples (plasma/blood) storage/shipment costs and the limited availability of laboratories providing TDM services. Sampling in the form of dry plasma spot (DPS) or dry blood spot (DBS) is a suitable alternative to overcome these issues. An improved, simple, rapid, and stability indicating method for quantification of pregabalin in human plasma and DPS has been developed and validated. Analyses were performed on liquid chromatography tandem mass spectrometer under positive ionization mode of electrospray interface. Pregabain-d4 was used as internal standard, and the chromatographic separations were performed on Poroshell 120 EC-C18 column using an isocratic mobile phase flow rate of 1 mL/min. Stability of pregabalin in DPS was evaluated under simulated real-time conditions. Extraction procedures from plasma and DPS samples were compared using statistical tests. The method was validated considering the FDA method validation guideline. The method was linear over the concentration range of 20-16000 ng/mL and 100-10000 ng/mL in plasma and DPS, respectively. DPS samples were found stable for only one week upon storage at room temperature and for at least four weeks at freezing temperature (-20 ± 5 °C). Method was applied for quantification of pregabalin in over 600 samples of a clinical study. Statistical analyses revealed that two extraction procedures in plasma and DPS samples showed statistically insignificant difference and can be used interchangeably without any bias. Proposed method involves simple and rapid steps of sample processing that do not require a pre- or post-column derivatization procedure. The method is suitable for routine pharmacokinetic analysis and therapeutic monitoring of pregabalin.

Polymer stabilized liquid crystals: Topology-mediated electro-optical behavior and applications

NASA Astrophysics Data System (ADS)

Weng, Libo

There has been a wide range of liquid crystal polymer composites that vary in polymer concentration from as little as 3 wt.% (polymer stabilized liquid crystal) to as high as 60 wt.% (polymer dispersed liquid crystals). In this dissertation, an approach of surface polymerization based on a low reactive monomer concentration about 1 wt.% is studied in various liquid crystal operation modes. The first part of dissertation describes the development of a vertical alignment (VA) mode with surface polymer stabilization, and the effects of structure-performance relationship of reactive monomers (RMs) and polymerization conditions on the electro-optical behaviors of the liquid crystal device has been explored. The polymer topography plays an important role in modifying and enhancing the electro-optical performance of stabilized liquid crystal alignment. The enabling surface-pinned polymer stabilized vertical alignment (PSVA) approach has led to the development of high-performance and fast-switching displays with controllable pretilt angle, increase in surface anchoring energy, high optical contrast and fast response time. The second part of the dissertation explores a PSVA mode with in-plane switching (IPS) and its application for high-efficiency and fast-switching phase gratings. The diffraction patterns and the electro-optical behaviors including diffraction efficiency and response time are characterized. The diffraction grating mechanism and performance have been validated by computer simulation. Finally, the advantages of surface polymerization approach such as good optical contrast and fast response time have been applied to the fringe-field switching (FFS) system. The concentration of reactive monomer on the electro-optical behavior of the FFS cells is optimized. The outstanding electro-optical results and mechanism of increase in surface anchoring strength are corroborated by the director field simulation. The density and topology of nanoscale polymer protrusions are analyzed and confirmed by morphological study. The developed high-performance polymer-stabilized fringe-field-switching (PS-FFS) could open new types of device applications.

Quality indicators for eye bank.

PubMed

Acharya, Manisha; Biswas, Saurabh; Das, Animesh; Mathur, Umang; Dave, Abhishek; Singh, Ashok; Dubey, Suneeta

2018-03-01

The aim of this study is to identify quality indicators of the eye bank and validate their effectivity. Adverse reaction rate, discard rate, protocol deviation rate, and compliance rate were defined as Quality Indicators of the eye bank. These were identified based on definition of quality that captures two dimensions - "result quality" and "process quality." The indicators were measured and tracked as part of quality assurance (QA) program of the eye bank. Regular audits were performed to validate alignment of standard operating procedures (SOP) with regulatory and surgeon acceptance standards and alignment of activities performed in the eye bank with the SOP. Prospective study of the indicators was performed by comparing their observed values over the period 2011-2016. Adverse reaction rate decreased more than 8-fold (from 0.61% to 0.07%), discard rate decreased and stabilized at 30%, protocol deviation rate decreased from 1.05% to 0.08%, and compliance rate reported by annual quality audits improved from 59% to 96% at the same time. In effect, adverse reaction rate, discard rate, and protocol deviation rate were leading indicators, and compliance rate was the trailing indicator. These indicators fulfill an important gap in available literature on QA in eye banking. There are two ways in which these findings can be meaningful. First, eye banks which are new to quality measurement can adopt these indicators. Second, eye banks which are already deeply engaged in quality improvement can test these indicators in their eye bank, thereby incorporating them widely and improving them over time.

End-stage renal disease adherence questionnaire: translation and validation to the portuguese language.

PubMed

Poveda, Verónica; Amado, Leonilde; Filgueiras, Madalena; Teixeira, Laetitia; Miranda, Vasco; Santos-Silva, Alice; Paúl, Constança; Costa, Elísio

2016-11-01

Non-adherence to medical plans is recognized as an important problem in dialysis patients, since it has been associated with increased morbidity and mortality, resulting in disproportionately high costs of care. The success of renal replacement therapy depends on the adherence of patients to the different aspects of the therapeutic strategy, which includes a complex drug regimen involving a wide variety of drugs and doses, several prescribed dialysis sessions with different durations, dietetic recommendations and restriction of fluid intake. In this work, we aimed to translate and validate a previously described self-reported end-stage renal disease questionnaire (ESRD-AQ) to the Portuguese language (PESRD-AQ). After ESRD-AQ translation, a validation was performed by experts and by using a cohort of 185 Portuguese dialysis patients. PESRD-AQ reliability analysis showed strong test-retest stability across all items, with an intra-class correlation of 0.931. The average of the item-level content validity index by experts for the 46 items was 0.98, ranging from 0.94 to 1. Moreover, we found that PESRD-AQ scores indicative of non-adherence were associated with alterations in some biological and biochemical markers of non-adherence, including interdialytic weight gain. In conclusion, our results showed that PESRD-AQ, which presented an acceptable reliability and validity, is a valid tool to be used for adherence evaluation by Portuguese-speaking dialysis patients.

Fundamental Movement Skills Are More than Run, Throw and Catch: The Role of Stability Skills

PubMed Central

Rudd, James R.; Barnett, Lisa M.; Butson, Michael L.; Farrow, Damian; Berry, Jason; Polman, Remco C. J.

2015-01-01

Introduction In motor development literature fundamental movement skills are divided into three constructs: locomotive, object control and stability skills. Most fundamental movement skills research has focused on children’s competency in locomotor and object control skills. The first aim of this study was to validate a test battery to assess the construct of stability skills, in children aged 6 to 10 (M age = 8.2, SD = 1.2). Secondly we assessed how the stability skills construct fitted into a model of fundamental movement skill. Method The Delphi method was used to select the stability skill battery. Confirmatory factor analysis (CFA) was used to assess if the skills loaded onto the same construct and a new model of FMS was developed using structural equation modelling. Results Three postural control tasks were selected (the log roll, rock and back support) because they had good face and content validity. These skills also demonstrated good predictive validity with gymnasts scoring significantly better than children without gymnastic training and children from a high SES school performing better than those from a mid and low SES schools and the mid SES children scored better than the low SES children (all p < .05). Inter rater reliability tests were excellent for all three skills (ICC = 0.81, 0.87, 0.87) as was test re-test reliability (ICC 0.87–0.95). CFA provided good construct validity, and structural equation modelling revealed stability skills to be an independent factor in an overall FMS model which included locomotor (r = .88), object control (r = .76) and stability skills (r = .81). Discussion This study provides a rationale for the inclusion of stability skills in FMS assessment. The stability skills could be used alongside other FMS assessment tools to provide a holistic assessment of children’s fundamental movement skills. PMID:26468644

Comparison of Thunderstorm Simulations from WRF-NMM and WRF-ARW Models over East Indian Region

PubMed Central

Litta, A. J.; Mary Ididcula, Sumam; Mohanty, U. C.; Kiran Prasad, S.

2012-01-01

The thunderstorms are typical mesoscale systems dominated by intense convection. Mesoscale models are essential for the accurate prediction of such high-impact weather events. In the present study, an attempt has been made to compare the simulated results of three thunderstorm events using NMM and ARW model core of WRF system and validated the model results with observations. Both models performed well in capturing stability indices which are indicators of severe convective activity. Comparison of model-simulated radar reflectivity imageries with observations revealed that NMM model has simulated well the propagation of the squall line, while the squall line movement was slow in ARW. From the model-simulated spatial plots of cloud top temperature, we can see that NMM model has better captured the genesis, intensification, and propagation of thunder squall than ARW model. The statistical analysis of rainfall indicates the better performance of NMM than ARW. Comparison of model-simulated thunderstorm affected parameters with that of the observed showed that NMM has performed better than ARW in capturing the sharp rise in humidity and drop in temperature. This suggests that NMM model has the potential to provide unique and valuable information for severe thunderstorm forecasters over east Indian region. PMID:22645480

Stability of suxamethonium in pharmaceutical solution for injection by validated stability-indicating chromatographic method.

PubMed

Beck, William; Kabiche, Sofiane; Balde, Issa-Bella; Carret, Sandra; Fontan, Jean-Eudes; Cisternino, Salvatore; Schlatter, Joël

2016-12-01

To assess the stability of pharmaceutical suxamethonium (succinylcholine) solution for injection by validated stability-indicating chromatographic method in vials stored at room temperature. The chromatographic assay was achieved by using a detector wavelength set at 218 nm, a C18 column, and an isocratic mobile phase (100% of water) at a flow rate of 0.6 mL/min for 5 minutes. The method was validated according to the International Conference on Harmonization guidelines with respect to the stability-indicating capacity of the method including linearity, limits of detection and quantitation, precision, accuracy, system suitability, robustness, and forced degradations. Linearity was achieved in the concentration range of 5 to 40 mg/mL with a correlation coefficient higher than 0.999. The limits of detection and quantification were 0.8 and 0.9 mg/mL, respectively. The percentage relative standard deviation for intraday (1.3-1.7) and interday (0.1-2.0) precision was found to be less than 2.1%. Accuracy was assessed by the recovery test of suxamethonium from solution for injection (99.5%-101.2%). Storage of suxamethonium solution for injection vials at ambient temperature (22°C-26°C) for 17 days demonstrated that at least 95% of original suxamethonium concentration remained stable. Copyright © 2016 Elsevier Inc. All rights reserved.

Transport and stability analyses supporting disruption prediction in high beta KSTAR plasmas

NASA Astrophysics Data System (ADS)

Ahn, J.-H.; Sabbagh, S. A.; Park, Y. S.; Berkery, J. W.; Jiang, Y.; Riquezes, J.; Lee, H. H.; Terzolo, L.; Scott, S. D.; Wang, Z.; Glasser, A. H.

2017-10-01

KSTAR plasmas have reached high stability parameters in dedicated experiments, with normalized beta βN exceeding 4.3 at relatively low plasma internal inductance li (βN/li>6). Transport and stability analyses have begun on these plasmas to best understand a disruption-free path toward the design target of βN = 5 while aiming to maximize the non-inductive fraction of these plasmas. Initial analysis using the TRANSP code indicates that the non-inductive current fraction in these plasmas has exceeded 50 percent. The advent of KSTAR kinetic equilibrium reconstructions now allows more accurate computation of the MHD stability of these plasmas. Attention is placed on code validation of mode stability using the PEST-3 and resistive DCON codes. Initial evaluation of these analyses for disruption prediction is made using the disruption event characterization and forecasting (DECAF) code. The present global mode kinetic stability model in DECAF developed for low aspect ratio plasmas is evaluated to determine modifications required for successful disruption prediction of KSTAR plasmas. Work supported by U.S. DoE under contract DE-SC0016614.

Pressure ulcers: development and psychometric evaluation of the attitude towards pressure ulcer prevention instrument (APuP).

PubMed

Beeckman, D; Defloor, T; Demarré, L; Van Hecke, A; Vanderwee, K

2010-11-01

Pressure ulcers continue to be a significant problem in hospitals, nursing homes and community care settings. Pressure ulcer incidence is widely accepted as an indicator for the quality of care. Negative attitudes towards pressure ulcer prevention may result in suboptimal preventive care. A reliable and valid instrument to assess attitudes towards pressure ulcer prevention is lacking. Development and psychometric evaluation of the Attitude towards Pressure ulcer Prevention instrument (APuP). Prospective psychometric instrument validation study. A literature review was performed to design the instrument. Content validity was evaluated by nine European pressure ulcer experts and five experts in psychometric instrument validation in a double Delphi procedure. A convenience sample of 258 nurses and 291 nursing students from Belgium and The Netherlands participated in order to evaluate construct validity and stability reliability of the instrument. The data were collected between February and May 2008. A factor analysis indicated the construct of a 13 item instrument in a five factor solution: (1) attitude towards personal competency to prevent pressure ulcers (three items); (2) attitude towards the priority of pressure ulcer prevention (three items); (3) attitude towards the impact of pressure ulcers (three items); (4) attitude towards personal responsibility in pressure ulcer prevention (two items); and (5) attitude towards confidence in the effectiveness of prevention (two items). This five factor solution accounted for 61.4% of the variance in responses related to attitudes towards pressure ulcer prevention. All items demonstrated factor loadings over 0.60. The instrument produced similar results during stability testing [ICC=0.88 (95% CI=0.84-0.91, P<0.001)]. For the total instrument, the internal consistency (Cronbachs alpha) was 0.79. The APuP is a psychometrically sound instrument that can be used to effectively assess attitudes towards pressure ulcer prevention in patient care, education, and research. In further research, the association between attitude, knowledge and clinical performance should be explored. Copyright 2010 Elsevier Ltd. All rights reserved.

Development and validation of a stability-indicating size-indicating size-exclusion LC method for the determination of rhIFN-alpha2a in pharmaceutical formulations.

PubMed

Zimmermann, Estevan Sonego; da Silva, Lucélia Magalhães; Calegari, Guilherme Zanini; Stamm, Fernanda Pavani; Souto, Ricardo Bizogne; Dalmora, Sérgio Luiz

2013-01-01

A size-exclusion LC method was validated for the determination of interferon-a2a (rhlFN-alpha2a) in pharmaceutical formulations without interference from human serum albumin. Chromatographic separation was performed on a BioSep-SEC-S 2000 column (300 x 7.8 mm id). The mobile phase consisted of 0.001 M monobasic potassium phosphate, 0.008 M sodium phosphate dibasic; 0.2 M sodium chloride buffer, pH 7.4, run at a gradient flow rate and using photodiode array detection at 214 nm, was used. Chromatographic separation was achieved with a retention time of 17.2 min, and the analysis was linear over the concentration range of 1.98 to 198 microg/mL (r2 = 0.9996). The accuracy was 101.39%, with bias lower than 1.67%. The LOD and LOQ were 0.87 and 1.98 microg/mL, respectively. Moreover, method validation demonstrated acceptable results for precision and robustness. The method was applied to the assessment of rhlFN-alpha2a and related proteins in biopharmaceutical dosage forms, and the content/potencies were correlated to those given by a validated RP-LC method and an in vitro bioassay. It was concluded that use of the methods in conjunction allows a great improvement in monitoring stability and QC, thereby ensuring the therapeutic efficacy of the biotechnology-derived medicine.

Familiarization, validity and smallest detectable difference of the isometric squat test in evaluating maximal strength.

PubMed

Drake, David; Kennedy, Rodney; Wallace, Eric

2018-02-06

Isometric multi-joint tests are considered reliable and have strong relationships with 1RM performance. However, limited evidence is available for the isometric squat in terms of effects of familiarization and reliability. This study aimed to assess, the effect of familiarization, stability reliability, determine the smallest detectible difference, and the correlation of the isometric squat test with 1RM squat performance. Thirty-six strength-trained participants volunteered to take part in this study. Following three familiarization sessions, test-retest reliability was evaluated with a 48-hour window between each time point. Isometric squat peak, net and relative force were assessed. Results showed three familiarizations were required, isometric squat had a high level of stability reliability and smallest detectible difference of 11% for peak and relative force. Isometric strength at a knee angle of ninety degrees had a strong significant relationship with 1RM squat performance. In conclusion, the isometric squat is a valid test to assess multi-joint strength and can discriminate between strong and weak 1RM squat performance. Changes greater than 11% in peak and relative isometric squat performance should be considered as meaningful in participants who are familiar with the test.

Development and Testing of a High Stability Engine Control (HISTEC) System

NASA Technical Reports Server (NTRS)

Orme, John S.; DeLaat, John C.; Southwick, Robert D.; Gallops, George W.; Doane, Paul M.

1998-01-01

Flight tests were recently completed to demonstrate an inlet-distortion-tolerant engine control system. These flight tests were part of NASA's High Stability Engine Control (HISTEC) program. The objective of the HISTEC program was to design, develop, and flight demonstrate an advanced integrated engine control system that uses measurement-based, real-time estimates of inlet airflow distortion to enhance engine stability. With improved stability and tolerance of inlet airflow distortion, future engine designs may benefit from a reduction in design stall-margin requirements and enhanced reliability, with a corresponding increase in performance and decrease in fuel consumption. This paper describes the HISTEC methodology, presents an aircraft test bed description (including HISTEC-specific modifications) and verification and validation ground tests. Additionally, flight test safety considerations, test plan and technique design and approach, and flight operations are addressed. Some illustrative results are presented to demonstrate the type of analysis and results produced from the flight test program.

A bioanalytical HPLC method for coumestrol quantification in skin permeation tests followed by UPLC-QTOF/HDMS stability-indicating method for identification of degradation products.

PubMed

Bianchi, Sara E; Teixeira, Helder F; Kaiser, Samuel; Ortega, George G; Schneider, Paulo Henrique; Bassani, Valquiria L

2016-05-01

Coumestrol is present in several species of the Fabaceae family widely distributed in plants. The estrogenic and antioxidant activities of this molecule show its potential as skin anti-aging agent. These characteristics reveal the interest in developing analytical methodology for permeation studies, as well as to know the stability of coumestrol identifying the major degradation products. Thus, the present study was designed, first, to develop and validate a versatile liquid chromatography (HPLC) method to quantify coumestrol in a hydrogel formulation in different porcine skin layers (stratum corneum, epidermis, and dermis) in permeation tests. In the stability-indicating test coumestrol samples were exposed to stress conditions: temperature, UVC light, oxidative, acid and alkaline media. The degradation products, as well as the constituents extracted from the hydrogel, adhesive tape or skin were not eluted in the retention time of the coumestrol. Hence, the HPLC method showed to be versatile, specific, accurate, precise and robust showing excellent performance for quantifying coumestrol in complex matrices involving skin permeation studies. Coumestrol recovery from porcine ear skin was found to be in the range of 97.07-107.28 μg/mL; the intra-day precision (repeatability) and intermediate precision (inter-day precision), respectively lower than 4.71% and 2.09%. The analysis using ultra-performance liquid chromatography coupled to a quadrupole time-of-flight high definition mass spectrometry detector (UPLC-QTOF/HDMS) suggest the MS fragmentation patterns and the chemical structure of the main degradation products. These results represent new and relevant findings for the development of coumestrol pharmaceutical and cosmetic products. Copyright © 2016 Elsevier B.V. All rights reserved.

New support for high-performance liquid chromatography based on silica coated with alumina particles.

PubMed

Silveira, José Leandro R; Dib, Samia R; Faria, Anizio M

2014-01-01

A new material based on silica coated with alumina nanoparticles was proposed for use as a chromatographic support for reversed-phase high-performance liquid chromatography. Alumina nanoparticles were synthesized by a sol-gel process in reversed micelles composed of sodium bis(2-ethylhexyl)sulfosuccinate, and the support material was formed by the self-assembly of alumina layers on silica spheres. Spectroscopic and (29)Si nuclear magnetic resonance results showed evidence of chemical bonds between the alumina nanoparticles and the silica spheres, while morphological characterizations showed that the aluminized silica maintained the morphological properties of silica desired for chromatographic purposes after alumina incorporation. Stability studies indicated that bare silica showed high dissolution (~83%), while the aluminized silica remained practically unchanged (99%) after passing one liter of the alkaline mobile phase, indicating high stability under alkaline conditions. The C18 bonded aluminized silica phase showed great potential for use in high-performance liquid chromatography to separate basic molecules in the reversed-phase mode.

Quantitative determination and validation of octreotide acetate using 1 H-NMR spectroscopy with internal standard method.

PubMed

Yu, Chen; Zhang, Qian; Xu, Peng-Yao; Bai, Yin; Shen, Wen-Bin; Di, Bin; Su, Meng-Xiang

2018-01-01

Quantitative nuclear magnetic resonance (qNMR) is a well-established technique in quantitative analysis. We presented a validated 1 H-qNMR method for assay of octreotide acetate, a kind of cyclic octopeptide. Deuterium oxide was used to remove the undesired exchangeable peaks, which was referred to as proton exchange, in order to make the quantitative signals isolated in the crowded spectrum of the peptide and ensure precise quantitative analysis. Gemcitabine hydrochloride was chosen as the suitable internal standard. Experimental conditions, including relaxation delay time, the numbers of scans, and pulse angle, were optimized first. Then method validation was carried out in terms of selectivity, stability, linearity, precision, and robustness. The assay result was compared with that by means of high performance liquid chromatography, which is provided by Chinese Pharmacopoeia. The statistical F test, Student's t test, and nonparametric test at 95% confidence level indicate that there was no significant difference between these two methods. qNMR is a simple and accurate quantitative tool with no need for specific corresponding reference standards. It has the potential of the quantitative analysis of other peptide drugs and standardization of the corresponding reference standards. Copyright © 2017 John Wiley & Sons, Ltd.

Physical and Chemical Stability of Urapidil in 0.9% Sodium Chloride in Elastomeric Infusion Pump.

PubMed

Tomasello, Cristina; Leggieri, Anna; Rabbia, Franco; Veglio, Franco; Baietto, Lorena; Fulcheri, Chiara; De Nicolò, Amedeo; De Perri, Giovanni; D'Avolio, Antonio

2016-01-01

Urapidil is an antihypertensive agent, usually administered through intravenous bolus injection, slow-intravenous infusion, or continuous-drug infusion by perfusor. Since to date no evidences are available on drug stability in elastomeric pumps, patients have to be hospitalized. The purpose of this study was to validate an ultra-performance liquid chromatographic method to evaluate urapidil stability in an elastomeric infusion pump, in order to allow continuous infusion as home-care treatment. Analyses were conducted by diluting urapidil in an elastomeric pump. Two concentrations were evaluated: 1.6 mg/mL and 3.3 mg/mL. For the analyses, a reverse-phase ultra-performance liquid chromatographic- photodiode array detection instrument was used. Stressed degradation, pH changes, and visual clarity were used as stability indicators up to 10 days after urapidil solution preparation. The drug showed no more than 5% degradation during the test period at room temperature. No pH changes and no evidences of incompatibility were observed. Stress tests resulted in appreciable observation of degradation products. Considering the observed mean values, urapidil hydrochloride in sodium chloride 0.9% in elastomeric infusion pumps is stable for at least 10 days. These results indicate that this treatment could be administered at home for a prolonged duration (at least 7 days) with a satisfactory response. Copyright© by International Journal of Pharmaceutical Compounding, Inc.

Evaluation of the reliability and validity for X16 balance testing scale for the elderly.

PubMed

Ju, Jingjuan; Jiang, Yu; Zhou, Peng; Li, Lin; Ye, Xiaolei; Wu, Hongmei; Shen, Bin; Zhang, Jialei; He, Xiaoding; Niu, Chunjin; Xia, Qinghua

2018-05-10

Balance performance is considered as an indicator of functional status in the elderly, a large scale population screening and evaluation in the community context followed by proper interventions would be of great significance at public health level. However, there has been no suitable balance testing scale available for large scale studies in the unique community context of urban China. A balance scale named X16 balance testing scale was developed, which was composed of 3 domains and 16 items. A total of 1985 functionally independent and active community-dwelling elderly adults' balance abilities were tested using the X16 scale. The internal consistency, split-half reliability, content validity, construct validity, discriminant validity of X16 balance testing scale were evaluated. Factor analysis was performed to identify alternative factor structure. The Eigenvalues of factors 1, 2, and 3 were 8.53, 1.79, and 1.21, respectively, and their cumulative contribution to the total variance reached 72.0%. These 3 factors mainly represented domains static balance, postural stability, and dynamic balance. The Cronbach alpha coefficient for the scale was 0.933. The Spearman correlation coefficients between items and its corresponding domains were ranged from 0.538 to 0.964. The correlation coefficients between each item and its corresponding domain were higher than the coefficients between this item and other domains. With the increase of age, the scores of balance performance, domains static balance, postural stability, and dynamic balance in the elderly declined gradually (P < 0.001). With the increase of age, the proportion of the elderly with intact balance performance decreased gradually (P < 0.001). The reliability and validity of the X16 balance testing scale is both adequate and acceptable. Due to its simple and quick use features, it is practical to be used repeatedly and routinely especially in community setting and on large scale screening.

Development and co-validation of porcine insulin certified reference material by high-performance liquid chromatography-isotope dilution mass spectrometry.

PubMed

Wu, Liqing; Takatsu, Akiko; Park, Sang-Ryoul; Yang, Bin; Yang, Huaxin; Kinumi, Tomoya; Wang, Jing; Bi, Jiaming; Wang, Yang

2015-04-01

This article concerns the development and co-validation of a porcine insulin (pINS) certified reference material (CRM) produced by the National Institute of Metrology, People's Republic of China. Each CRM unit contained about 15 mg of purified solid pINS. The moisture content, amount of ignition residue, molecular mass, and purity of the pINS were measured. Both high-performance liquid chromatography-isotope dilution mass spectrometry and a purity deduction method were used to determine the mass fraction of the pINS. Fifteen units were selected to study the between-bottle homogeneity, and no inhomogeneity was observed. A stability study concluded that the CRM was stable for at least 12 months at -20 °C. The certified value of the CRM was (0.892 ± 0.036) g/g. A co-validation of the CRM was performed among Chinese, Japanese, and Korean laboratories under the framework of the Asian Collaboration on Reference Materials. The co-validation results agreed well with the certified value of the CRM. Consequently, the pINS CRM may be used as a calibration material or as a validation standard for pharmaceutical purposes to improve the quality of pharmaceutical products.

Stability of an ophthalmic formulation of polyhexamethylene biguanide in gamma-sterilized and ethylene oxide sterilized low density polyethylene multidose eyedroppers

PubMed Central

Wasiak, Mathieu; Jouannet, Mireille; Sautou, Valérie

2018-01-01

Background Polyhexamethylene biguanide (PHMB) eye drops are a frequently used medication to treat Acanthamoeba keratitis. In the absence of marketed PHMB eye drops, pharmacy-compounding units are needed to prepare this much needed treatment, but the lack of validated PHMB stability data severely limits their conservation by imposing short expiration dates after preparation. In this study we aim to assess the physicochemical and microbiological stability of a 0.2 mg/mL PHMB eye drop formulation stored in two kinds of polyethylene bottles at two different temperatures. Methods A liquid chromatography coupled with diode array detector stability-indicating method was validated to quantify PHMB, using a cyanopropyl bonded phase (Agilent Zorbax Eclipse XDB-CN column 4.6 × 75 mm with particle size of 3.5 μm) and isocratic elution consisting of acetonitrile/deionized water (3/97 v/v) at a flow rate of 1.3 mL/min. PHMB eye drops stability was assessed for 90 days of storage at 5 and 25 °C in ethylene oxide sterilized low density polyethylene (EOS-LDPE) and gamma sterilized low density polyethylene (GS-LDPE) bottles. The following analyses were performed: visual inspection, PHMB quantification and breakdown products (BPs) screening, osmolality and pH measurements, and sterility assessment. PHMB quantification and BP screening was also performed on the drops emitted from the multidose eyedroppers to simulate in-use condition. Results The analytical method developed meets all the qualitative and quantitative criteria for validation with an acceptable accuracy and good linearity, and is stability indicating. During 90 days of storage, no significant decrease of PHMB concentration was found compared to initial concentration in all stored PHMB eye drops. However, BP were found at day 30 and at day 90 of monitoring in both kind of bottles, stored at 5 and 25 °C, respectively. Although no significant variation of osmolality was found and sterility was maintained during 90 days of monitoring, a significant decrease of pH in GS-LDPE PHMB eye drops was noticed reaching 4 and 4.6 at 25 °C and 5 °C respectively, compared to initial pH of 6.16. Discussion Although no significant decrease in PHMB concentration was found during 90 days of monitoring in all conditions, the appearance of BPs and their unknown toxicities let us believe that 0.2 mg/mL PHMB solution should be conserved for no longer than 60 days in EOS-LDPE bottles at 25 °C. PMID:29682408

A novel automated hydrophilic interaction liquid chromatography method using diode-array detector/electrospray ionization tandem mass spectrometry for analysis of sodium risedronate and related degradation products in pharmaceuticals.

PubMed

Bertolini, Tiziana; Vicentini, Lorenza; Boschetti, Silvia; Andreatta, Paolo; Gatti, Rita

2014-10-24

A simple, sensitive and fast hydrophilic interaction liquid chromatography (HILIC) method using ultraviolet diode-array detector (UV-DAD)/electrospray ionization tandem mass spectrometry was developed for the automated high performance liquid chromatography (HPLC) determination of sodium risedronate (SR) and its degradation products in new pharmaceuticals. The chromatographic separations were performed on Ascentis Express HILIC 2.7μm (150mm×2.1mm, i.d.) stainless steel column (fused core). The mobile phase consisted of formate buffer solution (pH 3.4; 0.03M)/acetonitrile 42:58 and 45:55 (v/v) for granules for oral solution and effervescent tablet analysis, respectively, at a flow-rate of 0.2mL/min, setting the wavelength at 262nm. Stability characteristics of SR were evaluated by performing stress test studies. The main degradation product formed under oxidation conditions corresponding to sodium hydrogen (1-hydroxy-2-(1-oxidopyridin-3-yl)-1-phosphonoethyl)phosphonate was characterized by high performance liquid chromatography-electrospray ionization-mass tandem mass spectrometry (HPLC-ESI-MS/MS). The validation parameters such as linearity, sensitivity, accuracy, precision and selectivity were found to be highly satisfactory. Linear responses were observed in standard and in fortified placebo solutions. Intra-day precision (relative standard deviation, RSD) was ≤1.1% for peak area and ≤0.2% for retention times (tR) without significant differences between intra- and inter-day data. Recovery studies showed good results for all the examined compounds (from 98.7 to 101.0%) with RSD ranging from 0.6 to 0.7%. The limits of detection (LOD) and quantitation (LOQ) were 1 and 3ng/mL, respectively. The high stability of standard and sample solutions at room temperature means an undoubted advantage of the method allowing the simultaneous preparation of many samples and consecutive chromatographic analyses by using an autosampler. The developed stability indicating method is suitable for the quality control of SR in new and commercial pharmaceutical formulations. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of degradation products and process related impurities of asenapine maleate in asenapine sublingual tablets by UPLC

NASA Astrophysics Data System (ADS)

Kumar, Nitin; Sangeetha, D.; Kalyanraman, L.

2017-11-01

For determination of process related impurities and degradation products of asenapine maleate in asenapine sublingual Tablets, a reversed phase, stability indicating UPLC method was developed. Acetonitrile, methanol and potassium dihydrogen phosphate buffer with tetra-n- butyl ammonium hydrogen sulphate as ion pair (pH 2.2; 0.01 M) at flow rate of 0.2 ml/min were used in gradient elution mode. Separation was achieved by using acquity BEH Shield RP18 column (1.7 μm, 2.1 mm×100 mm) at 35 ºC. UV detection was performed at 228 nm. Subsequently the liquid chromatography method was validated as per ICH. The drug product was exposed to the stress conditions of acid hydrolysis, base hydrolysis, water hydrolysis, oxidative, thermal, and photolytic. In oxidative stress and thermal stress significant degradation was observed. All the degradation products were well separated from analyte peak and its impurities. Stability indicating nature of the method was proved by demonstrating the peak purity of Asenapine peak in all the stressed samples. The mass balance was found >95% for all the stress conditions. Based on method validation, the method was found specific, linear, accurate, precise, rugged and robust.

Determination of three steroidal saponins from Ophiopogon japonicus (Liliaceae) via high-performance liquid chromatography with mass spectrometry.

PubMed

Wang, Yongyi; Xu, Jinzhong; Qu, Haibin

2013-01-01

A simple and accurate analytical method was developed for simultaneous quantification of three steroidal saponins in the roots of Ophiopogon japonicus via high-performance liquid chromatography (HPLC) with mass spectrometry (MS) in this study. Separation was performed on a Tigerkin C(18) column and detection was performed by mass spectrometry. A mobile phase consisted of 0.02% formic acid in water (v/v) and 0.02% formic acid in acetonitrile (v/v) was used with a flow rate of 0.5 mL min(-1). The quantitative HPLC-MS method was validated for linearity, precision, repeatability, stability, recovery, limits of detection and quantification. This developed method provides good linearity (r >0.9993), intra- and inter-day precisions (RSD <4.18%), repeatability (RSD <5.05%), stability (RSD <2.08%) and recovery (93.82-102.84%) for three steroidal saponins. It could be considered as a suitable quality control method for O. japonicus.

Development of Advanced Verification and Validation Procedures and Tools for the Certification of Learning Systems in Aerospace Applications

NASA Technical Reports Server (NTRS)

Jacklin, Stephen; Schumann, Johann; Gupta, Pramod; Richard, Michael; Guenther, Kurt; Soares, Fola

2005-01-01

Adaptive control technologies that incorporate learning algorithms have been proposed to enable automatic flight control and vehicle recovery, autonomous flight, and to maintain vehicle performance in the face of unknown, changing, or poorly defined operating environments. In order for adaptive control systems to be used in safety-critical aerospace applications, they must be proven to be highly safe and reliable. Rigorous methods for adaptive software verification and validation must be developed to ensure that control system software failures will not occur. Of central importance in this regard is the need to establish reliable methods that guarantee convergent learning, rapid convergence (learning) rate, and algorithm stability. This paper presents the major problems of adaptive control systems that use learning to improve performance. The paper then presents the major procedures and tools presently developed or currently being developed to enable the verification, validation, and ultimate certification of these adaptive control systems. These technologies include the application of automated program analysis methods, techniques to improve the learning process, analytical methods to verify stability, methods to automatically synthesize code, simulation and test methods, and tools to provide on-line software assurance.

Validation of a Reversed-Phase High Performance Liquid Chromatography Method for the Simultaneous Analysis of Cysteine and Reduced Glutathione in Mouse Organs

PubMed Central

Brundu, Serena; Nencioni, Lucia; Celestino, Ignacio; Coluccio, Paolo; Palamara, Anna Teresa; Fraternale, Alessandra

2016-01-01

A depletion of reduced glutathione (GSH) has been observed in pathological conditions and in aging. Measuring GSH in tissues using mouse models is an excellent way to assess GSH depletion and the potential therapeutic efficacy of drugs used to maintain and/or restore cellular redox potential. A high performance liquid chromatography (HPLC) method for the simultaneous determination of GSH and cysteine (Cys) in mouse organs was validated according to USA and European standards. The method was based on separation coupled with ultraviolet detection and precolumn derivatization with 5,5′-dithiobis-(2-nitrobenzoic acid) (DTNB). The required validation parameters, that are, selectivity, linearity, lower limit of quantification, precision, accuracy, recovery, and stability, were studied for spleen, lymph nodes, pancreas, and brain. The results showed that the lower limits of quantification were 0.313 μM and 1.25 μM for Cys and GSH, respectively. Intraday and interday precisions were less than 11% and 14%, respectively, for both compounds. The mean extraction recoveries of Cys and GSH from all organs were more than 93% and 86%, respectively. Moreover, the stability of both analytes during sample preparation and storage was demonstrated. The method was accurate, reliable, consistent, and reproducible and it was useful to determine Cys and GSH in the organs of different mouse strains. PMID:26885246

Validated and longitudinally stable asthma phenotypes based on cluster analysis of the ADEPT study.

PubMed

Loza, Matthew J; Djukanovic, Ratko; Chung, Kian Fan; Horowitz, Daniel; Ma, Keying; Branigan, Patrick; Barnathan, Elliot S; Susulic, Vedrana S; Silkoff, Philip E; Sterk, Peter J; Baribaud, Frédéric

2016-12-15

Asthma is a disease of varying severity and differing disease mechanisms. To date, studies aimed at stratifying asthma into clinically useful phenotypes have produced a number of phenotypes that have yet to be assessed for stability and to be validated in independent cohorts. The aim of this study was to define and validate, for the first time ever, clinically driven asthma phenotypes using two independent, severe asthma cohorts: ADEPT and U-BIOPRED. Fuzzy partition-around-medoid clustering was performed on pre-specified data from the ADEPT participants (n = 156) and independently on data from a subset of U-BIOPRED asthma participants (n = 82) for whom the same variables were available. Models for cluster classification probabilities were derived and applied to the 12-month longitudinal ADEPT data and to a larger subset of the U-BIOPRED asthma dataset (n = 397). High and low type-2 inflammation phenotypes were defined as high or low Th2 activity, indicated by endobronchial biopsies gene expression changes downstream of IL-4 or IL-13. Four phenotypes were identified in the ADEPT (training) cohort, with distinct clinical and biomarker profiles. Phenotype 1 was "mild, good lung function, early onset", with a low-inflammatory, predominantly Type-2, phenotype. Phenotype 2 had a "moderate, hyper-responsive, eosinophilic" phenotype, with moderate asthma control, mild airflow obstruction and predominant Type-2 inflammation. Phenotype 3 had a "mixed severity, predominantly fixed obstructive, non-eosinophilic and neutrophilic" phenotype, with moderate asthma control and low Type-2 inflammation. Phenotype 4 had a "severe uncontrolled, severe reversible obstruction, mixed granulocytic" phenotype, with moderate Type-2 inflammation. These phenotypes had good longitudinal stability in the ADEPT cohort. They were reproduced and demonstrated high classification probability in two subsets of the U-BIOPRED asthma cohort. Focusing on the biology of the four clinical independently-validated easy-to-assess ADEPT asthma phenotypes will help understanding the unmet need and will aid in developing tailored therapies. NCT01274507 (ADEPT), registered October 28, 2010 and NCT01982162 (U-BIOPRED), registered October 30, 2013.

Stability-indicating method for simultaneous estimation of olmesartan medoxomile, amlodipine besylate and hydrochlorothiazide by RP-HPLC in tablet dosage form.

PubMed

Jain, P S; Patel, M K; Gorle, A P; Chaudhari, A J; Surana, S J

2012-09-01

A simple, specific, accurate and precise stability-indicating reversed-phase high-performance liquid chromatographic method was developed for simultaneous estimation of olmesartan medoxomile (OLME), amlodipine besylate (AMLO) and hydrochlorothiazide (HCTZ) in tablet dosage form. The method was developed using an RP C18 base deactivated silica column (250 × 4.6 mm, 5 µm) with a mobile phase consisting of triethylamine (pH 3.0) adjusted with orthophosphoric acid (A) and acetonitrile (B), with a timed gradient program of T/%B: 0/30, 7/70, 8/30, 10/30 with a flow rate of 1.4 mL/min. Ultraviolet detection was used at 236 nm. The retention times for OLME, AMLO and HCTZ were found to be 6.72, 4.28 and 2.30, respectively. The proposed method was validated for precision, accuracy, linearity, range, robustness, ruggedness and force degradation study. The calibration curves of OLME, AMLO and HCTZ were linear over the range of 50-150, 12.5-37.5 and 31-93 µg/mL, respectively. The method was found to be sensitive. The limits of detection of OLME, AMLO and HCTZ were determined 0.19, 0.16 and 0.22 µg/mL and limits of quantification of OLME, AMLO and HCTZ were determined 0.57, 0.49 and 0.66, respectively. Forced degradation study was performed according to International Conference on Harmonization guidelines.

Tunneled Mesoporous Carbon Nanofibers with Embedded ZnO Nanoparticles for Ultrafast Lithium Storage.

PubMed

An, Geon-Hyoung; Lee, Do-Young; Ahn, Hyo-Jin

2017-04-12

Carbon and metal oxide composites have received considerable attention as anode materials for Li-ion batteries (LIBs) owing to their excellent cycling stability and high specific capacity based on the chemical and physical stability of carbon and the high theoretical specific capacity of metal oxides. However, efforts to obtain ultrafast cycling stability in carbon and metal oxide composites at high current density for practical applications still face important challenges because of the longer Li-ion diffusion pathway, which leads to poor ultrafast performance during cycling. Here, tunneled mesoporous carbon nanofibers with embedded ZnO nanoparticles (TMCNF/ZnO) are synthesized by electrospinning, carbonization, and postcalcination. The optimized TMCNF/ZnO shows improved electrochemical performance, delivering outstanding ultrafast cycling stability, indicating a higher specific capacity than previously reported ZnO-based anode materials in LIBs. Therefore, the unique architecture of TMCNF/ZnO has potential for use as an anode material in ultrafast LIBs.

Quality by design approach for the separation of naproxcinod and its related substances by fused core particle technology column.

PubMed

Inugala, Ugandar Reddy; Pothuraju, Nageswara Rao; Vangala, Ranga Reddy

2013-01-01

This paper describes the development of a rapid, novel, stability-indicating gradient reversed-phase high-performance liquid chromatographic method and associated system suitability parameters for the analysis of naproxcinod in the presence of its related substances and degradents using a quality-by-design approach. All of the factors that affect the separation of naproxcinod and its impurities and their mutual interactions were investigated and robustness of the method was ensured. The method was developed using an Ascentis Express C8 150 × 4.6 mm, 2.7 µm column with a mobile phase containing a gradient mixture of two solvents. The eluted compounds were monitored at 230 nm, the run time was 20 min within which naproxcinod and its eight impurities were satisfactorily separated. Naproxcinod was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Naproxcinod was found to degrade significantly in acidic and basic conditions and to be stable in thermal, photolytic, oxidative and aqueous degradation conditions. The degradation products were satisfactorily resolved from the primary peak and its impurities, proving the stability-indicating power of the method. The developed method was validated as per International Conference on Harmonization guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness.

Stability of Two Antifungal Agents, Fluconazole and Miconazole, Compounded in HUMCO RECURA Topical Cream to Determine Beyond-Use Date.

PubMed

Gautam, Pradeep; Light, Bob; Purvis, Troy

2017-01-01

A novel compounding vehicle (RECURA) has previously been proven to penetrate the nail bed when compounded with the antifungal agent miconazole or fluconazole, providing for an effective treatment for onychomycosis. In this study, miconazole and fluconazole were compounded separately in RECURA compounding cream, and they were tested at different time points (0, 7, 14, 28, 45, 60, 90, and 180 days) to determine the beyond-use date of those formulations. The beyond-use date testing of both formulations (10% miconazole in RECURA and 10% fluconazole in RECURA) proved them to be physically, chemically, and microbiologically stable under International Conference of Harmonisation controlled room temperature (25°C ± 2°C/60% RH ±5%) for at least 180 days from the date of compounding. Stability-indicating analytical method validation was completed for the simultaneous determination of miconazole and fluconazole in RECURA base using high-performance liquid chromatography coupled with photodiode array detector prior to the study. Copyright© by International Journal of Pharmaceutical Compounding, Inc.

Physical and chemical stability of proflavine contrast agent solutions for early detection of oral cancer.

PubMed

Kawedia, Jitesh D; Zhang, Yan-Ping; Myers, Alan L; Richards-Kortum, Rebecca R; Kramer, Mark A; Gillenwater, Ann M; Culotta, Kirk S

2016-02-01

Proflavine hemisulfate solution is a fluorescence contrast agent to visualize cell nuclei using high-resolution optical imaging devices such as the high-resolution microendoscope. These devices provide real-time imaging to distinguish between normal versus neoplastic tissue. These images could be helpful for early screening of oral cancer and its precursors and to determine accurate margins of malignant tissue for ablative surgery. Extemporaneous preparation of proflavine solution for these diagnostic procedures requires preparation in batches and long-term storage to improve compounding efficiency in the pharmacy. However, there is a paucity of long-term stability data for proflavine contrast solutions. The physical and chemical stability of 0.01% (10 mg/100 ml) proflavine hemisulfate solutions prepared in sterile water was determined following storage at refrigeration (4-8℃) and room temperature (23℃). Concentrations of proflavine were measured at predetermined time points up to 12 months using a validated stability-indicating high-performance liquid chromatography method. Proflavine solutions stored under refrigeration were physically and chemically stable for at least 12 months with concentrations ranging from 95% to 105% compared to initial concentration. However, in solutions stored at room temperature increased turbidity and particulates were observed in some of the tested vials at 9 months and 12 months with peak particle count reaching 17-fold increase compared to baseline. Solutions stored at room temperature were chemically stable up to six months (94-105%). Proflavine solutions at concentration of 0.01% were chemically and physically stable for at least 12 months under refrigeration. The solution was chemically stable for six months when stored at room temperature. We recommend long-term storage of proflavine solutions under refrigeration prior to diagnostic procedure. © The Author(s) 2014.

Cognitive vulnerability to depression during middle childhood: Stability and associations with maternal affective styles and parental depression

PubMed Central

Hayden, Elizabeth P.; Olino, Thomas M.; Mackrell, Sarah V.M.; Jordan, Patricia L.; Desjardins, Jasmine; Katsiroumbas, Patrice

2014-01-01

Theories of cognitive vulnerability to depression (CVD) imply that CVD is early-emerging and trait-like; however, little longitudinal work has tested this premise in middle childhood, or examined theoretically relevant predictors of child CVD. We examined test–retest correlations of self-referent encoding task performance and self-reported attributional styles and their associations with parental characteristics in 205 seven-year-olds. At baseline, child CVD was assessed, structured clinical interviews were conducted with parents, and ratings of observed maternal affective styles were made. Children’s CVD was re-assessed approximately one and two years later. Both measures of children’s CVD were prospectively and concurrently associated with children’s depressive symptoms and showed modest stability. Multilevel modeling indicated that maternal criticism and paternal depression were related to children’s CVD. Findings indicate that even early-emerging CVD is a valid marker of children’s depression risk. PMID:25392596

The predictive validity of quality of evidence grades for the stability of effect estimates was low: a meta-epidemiological study.

PubMed

Gartlehner, Gerald; Dobrescu, Andreea; Evans, Tammeka Swinson; Bann, Carla; Robinson, Karen A; Reston, James; Thaler, Kylie; Skelly, Andrea; Glechner, Anna; Peterson, Kimberly; Kien, Christina; Lohr, Kathleen N

2016-02-01

To determine the predictive validity of the U.S. Evidence-based Practice Center (EPC) approach to GRADE (Grading of Recommendations Assessment, Development and Evaluation). Based on Cochrane reports with outcomes graded as high quality of evidence (QOE), we prepared 160 documents which represented different levels of QOE. Professional systematic reviewers dually graded the QOE. For each document, we determined whether estimates were concordant with high QOE estimates of the Cochrane reports. We compared the observed proportion of concordant estimates with the expected proportion from an international survey. To determine the predictive validity, we used the Hosmer-Lemeshow test to assess calibration and the C (concordance) index to assess discrimination. The predictive validity of the EPC approach to GRADE was limited. Estimates graded as high QOE were less likely, estimates graded as low or insufficient QOE more likely to remain stable than expected. The EPC approach to GRADE could not reliably predict the likelihood that individual bodies of evidence remain stable as new evidence becomes available. C-indices ranged between 0.56 (95% CI, 0.47 to 0.66) and 0.58 (95% CI, 0.50 to 0.67) indicating a low discriminatory ability. The limited predictive validity of the EPC approach to GRADE seems to reflect a mismatch between expected and observed changes in treatment effects as bodies of evidence advance from insufficient to high QOE. Copyright © 2016 Elsevier Inc. All rights reserved.

SEALDH-II-An Autonomous, Holistically Controlled, First Principles TDLAS Hygrometer for Field and Airborne Applications: Design-Setup-Accuracy/Stability Stress Test.

PubMed

Buchholz, Bernhard; Kallweit, Sören; Ebert, Volker

2016-12-30

Instrument operation in harsh environments often significantly impacts the trust level of measurement data. While commercial instrument manufacturers clearly define the deployment conditions to achieve trustworthy data in typical standard applications, it is frequently unavoidable in scientific field applications to operate instruments outside these commercial standard application specifications. Scientific instrumentation, however, is employing cutting-edge technology and often highly optimized but also lacks long-term field tests to assess the field vs. laboratory performance. Recently, we developed the Selective Extractive Laser Diode Hygrometer (SEALDH-II), which addresses field and especially airborne applications as well as metrological laboratory validations. SEALDH-II targets reducing deviations between airborne hygrometers (currently up to 20% between the most advanced hygrometers) with a new holistic, internal control and validation concept, which guarantees the transfer of the laboratory performance into a field scenario by capturing more than 80 instrument internal "housekeeping" data to nearly perfectly control SEALDH-II's health status. SEALDH-II uses a calibration-free, first principles based, direct Tuneable Diode Laser Absorption Spectroscopy (dTDLAS) approach, to cover the entire atmospheric humidity measurement range from about 3 to 40,000 ppmv with a calculated maximum uncertainty of 4.3% ± 3 ppmv. This is achieved not only by innovations in internal instrument monitoring and design, but also by active control algorithms such as a high resolution spectral stabilization. This paper describes the setup, working principles, and instrument stabilization, as well as its precision validation and long-term stress tests in an environmental chamber over an environmental temperature and humidity range of ΔT = 50 K and ΔRH = 80% RH, respectively.

SEALDH-II—An Autonomous, Holistically Controlled, First Principles TDLAS Hygrometer for Field and Airborne Applications: Design–Setup–Accuracy/Stability Stress Test

PubMed Central

Buchholz, Bernhard; Kallweit, Sören; Ebert, Volker

2016-01-01

Instrument operation in harsh environments often significantly impacts the trust level of measurement data. While commercial instrument manufacturers clearly define the deployment conditions to achieve trustworthy data in typical standard applications, it is frequently unavoidable in scientific field applications to operate instruments outside these commercial standard application specifications. Scientific instrumentation, however, is employing cutting-edge technology and often highly optimized but also lacks long-term field tests to assess the field vs. laboratory performance. Recently, we developed the Selective Extractive Laser Diode Hygrometer (SEALDH-II), which addresses field and especially airborne applications as well as metrological laboratory validations. SEALDH-II targets reducing deviations between airborne hygrometers (currently up to 20% between the most advanced hygrometers) with a new holistic, internal control and validation concept, which guarantees the transfer of the laboratory performance into a field scenario by capturing more than 80 instrument internal “housekeeping” data to nearly perfectly control SEALDH-II’s health status. SEALDH-II uses a calibration-free, first principles based, direct Tuneable Diode Laser Absorption Spectroscopy (dTDLAS) approach, to cover the entire atmospheric humidity measurement range from about 3 to 40,000 ppmv with a calculated maximum uncertainty of 4.3% ± 3 ppmv. This is achieved not only by innovations in internal instrument monitoring and design, but also by active control algorithms such as a high resolution spectral stabilization. This paper describes the setup, working principles, and instrument stabilization, as well as its precision validation and long-term stress tests in an environmental chamber over an environmental temperature and humidity range of ΔT = 50 K and ΔRH = 80% RH, respectively. PMID:28042844

A novel integrated framework and improved methodology of computer-aided drug design.

PubMed

Chen, Calvin Yu-Chian

2013-01-01

Computer-aided drug design (CADD) is a critical initiating step of drug development, but a single model capable of covering all designing aspects remains to be elucidated. Hence, we developed a drug design modeling framework that integrates multiple approaches, including machine learning based quantitative structure-activity relationship (QSAR) analysis, 3D-QSAR, Bayesian network, pharmacophore modeling, and structure-based docking algorithm. Restrictions for each model were defined for improved individual and overall accuracy. An integration method was applied to join the results from each model to minimize bias and errors. In addition, the integrated model adopts both static and dynamic analysis to validate the intermolecular stabilities of the receptor-ligand conformation. The proposed protocol was applied to identifying HER2 inhibitors from traditional Chinese medicine (TCM) as an example for validating our new protocol. Eight potent leads were identified from six TCM sources. A joint validation system comprised of comparative molecular field analysis, comparative molecular similarity indices analysis, and molecular dynamics simulation further characterized the candidates into three potential binding conformations and validated the binding stability of each protein-ligand complex. The ligand pathway was also performed to predict the ligand "in" and "exit" from the binding site. In summary, we propose a novel systematic CADD methodology for the identification, analysis, and characterization of drug-like candidates.

Noncredible cognitive performance at clinical evaluation of adult ADHD: An embedded validity indicator in a visuospatial working memory test.

PubMed

Fuermaier, Anselm B M; Tucha, Oliver; Koerts, Janneke; Lange, Klaus W; Weisbrod, Matthias; Aschenbrenner, Steffen; Tucha, Lara

2017-12-01

The assessment of performance validity is an essential part of the neuropsychological evaluation of adults with attention-deficit/hyperactivity disorder (ADHD). Most available tools, however, are inaccurate regarding the identification of noncredible performance. This study describes the development of a visuospatial working memory test, including a validity indicator for noncredible cognitive performance of adults with ADHD. Visuospatial working memory of adults with ADHD (n = 48) was first compared to the test performance of healthy individuals (n = 48). Furthermore, a simulation design was performed including 252 individuals who were randomly assigned to either a control group (n = 48) or to 1 of 3 simulation groups who were requested to feign ADHD (n = 204). Additional samples of 27 adults with ADHD and 69 instructed simulators were included to cross-validate findings from the first samples. Adults with ADHD showed impaired visuospatial working memory performance of medium size as compared to healthy individuals. Simulation groups committed significantly more errors and had shorter response times as compared to patients with ADHD. Moreover, binary logistic regression analysis was carried out to derive a validity index that optimally differentiates between true and feigned ADHD. ROC analysis demonstrated high classification rates of the validity index, as shown in excellent specificity (95.8%) and adequate sensitivity (60.3%). The visuospatial working memory test as presented in this study therefore appears sensitive in indicating cognitive impairment of adults with ADHD. Furthermore, the embedded validity index revealed promising results concerning the detection of noncredible cognitive performance of adults with ADHD. (PsycINFO Database Record (c) 2017 APA, all rights reserved).

Aqueous clay suspensions stabilized by alginate fluid gels for coal spontaneous combustion prevention and control.

PubMed

Qin, Botao; Ma, Dong; Li, Fanglei; Li, Yong

2017-11-01

We have developed aqueous clay suspensions stabilized by alginate fluid gels (AFG) for coal spontaneous combustion prevention and control. Specially, this study aimed to characterize the effect of AFG on the microstructure, static and dynamic stability, and coal fire inhibition performances of the prepared AFG-stabilized clay suspensions. Compared with aqueous clay suspensions, the AFG-stabilized clay suspensions manifest high static and dynamic stability, which can be ascribed to the formation of a robust three-dimensional gel network by AFG. The coal acceleration oxidation experimental results show that the prepared AFG-stabilized clay suspensions can improve the coal thermal stability and effectively inhibit the coal spontaneous oxidation process by increasing crossing point temperature (CPT) and reducing CO emission. The prepared low-cost and nontoxic AFG-stabilized clay suspensions, exhibiting excellent coal fire extinguishing performances, indicate great application potentials in coal spontaneous combustion prevention and control.

Exploratory Research on Bearing Characteristics of Confined Stabilized Soil

NASA Astrophysics Data System (ADS)

Wu, Shuai Shuai; Gao, Zheng Guo; Li, Shi Yang; Cui, Wen Bo; Huang, Xin

2018-06-01

The performance of a new kind of confined stabilized soil (CSS) was investigated which was constructed by filling the stabilized soil, which was made by mixing soil with a binder containing a high content of expansive component, into an engineering plastic pipe. Cube compressive strength of the stabilized soil formed with constraint and axial compression performance of stabilized soil cylinders confined with the constraint pipe were measured. The results indicated that combining the constraint pipe and the binder containing expansion component could achieve such effects: higher production of expansive hydrates could be adopted so as to fill more voids in the stabilized soil and improve its strength; at the same time compressive prestress built on the core stabilized soil, combined of which hoop constraint provided effective radial compressive force on the core stabilized soil. These effects made the CSS acquire plastic failure mode and more than twice bearing capacity of ordinary stabilized soil with the same binder content.

[Toward a deeper understanding of motivation towards exercise: measurement of integrated regulation in the Spanish context].

PubMed

González-Cutre, David; Sicilia, Álvaro; Fernández, Alberto

2010-11-01

The purpose of this study was to validate the Behavioural Regulation in Exercise Questionnaire in the Spanish context, including items to measure integrated regulation. Participants were 524 exercisers, mean age 29.59 years. The results revealed acceptable fit indices in the confirmatory factor analysis and good internal consistency (with a Cronbach alpha of .87 for integrated regulation). The diverse subscales also conformed to a simplex pattern and the factor structure was invariant across gender and age. Integrated regulation reflected high temporal stability over a 4-week period (ICC=.90). The criterion validity analysis of integrated regulation indicated that this variable was positively predicted by satisfaction of the needs for competence and autonomy. The results regarding the importance of measuring integrated regulation in exercise are discussed.

AFM as an analysis tool for high-capacity sulfur cathodes for Li–S batteries

PubMed Central

Sörgel, Seniz; Costa, Rémi; Carlé, Linus; Galm, Ines; Cañas, Natalia; Pascucci, Brigitta; Friedrich, K Andreas

2013-01-01

Summary In this work, material-sensitive atomic force microscopy (AFM) techniques were used to analyse the cathodes of lithium–sulfur batteries. A comparison of their nanoscale electrical, electrochemical, and morphological properties was performed with samples prepared by either suspension-spraying or doctor-blade coating with different binders. Morphological studies of the cathodes before and after the electrochemical tests were performed by using AFM and scanning electron microscopy (SEM). The cathodes that contained polyvinylidene fluoride (PVDF) and were prepared by spray-coating exhibited a superior stability of the morphology and the electric network associated with the capacity and cycling stability of these batteries. A reduction of the conductive area determined by conductive AFM was found to correlate to the battery capacity loss for all cathodes. X-ray diffraction (XRD) measurements of Li2S exposed to ambient air showed that insulating Li2S hydrolyses to insulating LiOH. This validates the significance of electrical ex-situ AFM analysis after cycling. Conductive tapping mode AFM indicated the existence of large carbon-coated sulfur particles. Based on the analytical findings, the first results of an optimized cathode showed a much improved discharge capacity of 800 mA·g(sulfur)−1 after 43 cycles. PMID:24205455

Validity of maximal isometric knee extension strength measurements obtained via belt-stabilized hand-held dynamometry in healthy adults.

PubMed

Ushiyama, Naoko; Kurobe, Yasushi; Momose, Kimito

2017-11-01

[Purpose] To determine the validity of knee extension muscle strength measurements using belt-stabilized hand-held dynamometry with and without body stabilization compared with the gold standard isokinetic dynamometry in healthy adults. [Subjects and Methods] Twenty-nine healthy adults (mean age, 21.3 years) were included. Study parameters involved right side measurements of maximal isometric knee extension strength obtained using belt-stabilized hand-held dynamometry with and without body stabilization and the gold standard. Measurements were performed in all subjects. [Results] A moderate correlation and fixed bias were found between measurements obtained using belt-stabilized hand-held dynamometry with body stabilization and the gold standard. No significant correlation and proportional bias were found between measurements obtained using belt-stabilized hand-held dynamometry without body stabilization and the gold standard. The strength identified using belt-stabilized hand-held dynamometry with body stabilization may not be commensurate with the maximum strength individuals can generate; however, it reflects such strength. In contrast, the strength identified using belt-stabilized hand-held dynamometry without body stabilization does not reflect the maximum strength. Therefore, a chair should be used to stabilize the body when performing measurements of maximal isometric knee extension strength using belt-stabilized hand-held dynamometry in healthy adults. [Conclusion] Belt-stabilized hand-held dynamometry with body stabilization is more convenient than the gold standard in clinical settings.

Comparison of five cluster validity indices performance in brain [18 F]FET-PET image segmentation using k-means.

PubMed

Abualhaj, Bedor; Weng, Guoyang; Ong, Melissa; Attarwala, Ali Asgar; Molina, Flavia; Büsing, Karen; Glatting, Gerhard

2017-01-01

Dynamic [ 18 F]fluoro-ethyl-L-tyrosine positron emission tomography ([ 18 F]FET-PET) is used to identify tumor lesions for radiotherapy treatment planning, to differentiate glioma recurrence from radiation necrosis and to classify gliomas grading. To segment different regions in the brain k-means cluster analysis can be used. The main disadvantage of k-means is that the number of clusters must be pre-defined. In this study, we therefore compared different cluster validity indices for automated and reproducible determination of the optimal number of clusters based on the dynamic PET data. The k-means algorithm was applied to dynamic [ 18 F]FET-PET images of 8 patients. Akaike information criterion (AIC), WB, I, modified Dunn's and Silhouette indices were compared on their ability to determine the optimal number of clusters based on requirements for an adequate cluster validity index. To check the reproducibility of k-means, the coefficients of variation CVs of the objective function values OFVs (sum of squared Euclidean distances within each cluster) were calculated using 100 random centroid initialization replications RCI 100 for 2 to 50 clusters. k-means was performed independently on three neighboring slices containing tumor for each patient to investigate the stability of the optimal number of clusters within them. To check the independence of the validity indices on the number of voxels, cluster analysis was applied after duplication of a slice selected from each patient. CVs of index values were calculated at the optimal number of clusters using RCI 100 to investigate the reproducibility of the validity indices. To check if the indices have a single extremum, visual inspection was performed on the replication with minimum OFV from RCI 100 . The maximum CV of OFVs was 2.7 × 10 -2 from all patients. The optimal number of clusters given by modified Dunn's and Silhouette indices was 2 or 3 leading to a very poor segmentation. WB and I indices suggested in median 5, [range 4-6] and 4, [range 3-6] clusters, respectively. For WB, I, modified Dunn's and Silhouette validity indices the suggested optimal number of clusters was not affected by the number of the voxels. The maximum coefficient of variation of WB, I, modified Dunn's, and Silhouette validity indices were 3 × 10 -2 , 1, 2 × 10 -1 and 3 × 10 -3 , respectively. WB-index showed a single global maximum, whereas the other indices showed also local extrema. From the investigated cluster validity indices, the WB-index is best suited for automated determination of the optimal number of clusters for [ 18 F]FET-PET brain images for the investigated image reconstruction algorithm and the used scanner: it yields meaningful results allowing better differentiation of tissues with higher number of clusters, it is simple, reproducible and has an unique global minimum. © 2016 American Association of Physicists in Medicine.

Radiation Impact on Pharmaceutical Stability: Retrospective Data Review

NASA Technical Reports Server (NTRS)

Daniels, V. R.; Bayuse, T. M.; McGuire, K. M.; Antonsen, E. L.; Putcha, L.

2017-01-01

Historical studies performed by the JSC Pharmacotherapeutics Discipline suggest that exposure to spaceflight conditions may compromise the safety and efficacy of some medications. Follow-on studies have revealed that affected medications demonstrate reductions in active pharmaceutical ingredient (API) concentrations and altered release characteristics. It was hypothesized that the changes in API potency and release were from the medication's exposure to the harsh environmental conditions of spaceflight. Subsequent review of the spaceflight environmental control records from the time of these studies indicated that temperature and humidity levels aboard all spacecraft remained within United States Pharmacopeia (USP) recommended ranges to maintain optimal pharmaceutical stability. Therefore, space radiation was presumed to be the source of observed drug degradation. The Pharmacotherapeutics Discipline conducted a ground analog radiation experiment in 2006 at the NASA Space Radiation Laboratory (NSRL) at Brookhaven to validate this theory and to characterize the effects of high-energy radioactive particles on pharmaceutical stability. These data were never published. Recently, the Exploration Medical Capability (ExMC) Element finalized a research plan (RP) aimed at providing a safe and effective medication formulary for exploration spaceflight. As ExMC begins to design new flight and ground analog radiation studies, further analysis of the 2006 NSRL study data is essential for the characterization of the impact of radiation on medication potency and efficacy in the exploration spaceflight environment.

In-Flight Validation of a Pilot Rating Scale for Evaluating Failure Transients in Electronic Flight Control Systems

NASA Technical Reports Server (NTRS)

Kalinowski, Kevin F.; Tucker, George E.; Moralez, Ernesto, III

2006-01-01

Engineering development and qualification of a Research Flight Control System (RFCS) for the Rotorcraft Aircrew Systems Concepts Airborne Laboratory (RASCAL) JUH-60A has motivated the development of a pilot rating scale for evaluating failure transients in fly-by-wire flight control systems. The RASCAL RFCS includes a highly-reliable, dual-channel Servo Control Unit (SCU) to command and monitor the performance of the fly-by-wire actuators and protect against the effects of erroneous commands from the flexible, but single-thread Flight Control Computer. During the design phase of the RFCS, two piloted simulations were conducted on the Ames Research Center Vertical Motion Simulator (VMS) to help define the required performance characteristics of the safety monitoring algorithms in the SCU. Simulated failures, including hard-over and slow-over commands, were injected into the command path, and the aircraft response and safety monitor performance were evaluated. A subjective Failure/Recovery Rating (F/RR) scale was developed as a means of quantifying the effects of the injected failures on the aircraft state and the degree of pilot effort required to safely recover the aircraft. A brief evaluation of the rating scale was also conducted on the Army/NASA CH-47B variable stability helicopter to confirm that the rating scale was likely to be equally applicable to in-flight evaluations. Following the initial research flight qualification of the RFCS in 2002, a flight test effort was begun to validate the performance of the safety monitors and to validate their design for the safe conduct of research flight testing. Simulated failures were injected into the SCU, and the F/RR scale was applied to assess the results. The results validate the performance of the monitors, and indicate that the Failure/Recovery Rating scale is a very useful tool for evaluating failure transients in fly-by-wire flight control systems.

Magic Numbers in Small Iron Clusters: A First-Principles Study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Eunja; Mohrland, Andrew B.; Weck, Philippe F.

2014-10-03

We perform ab initio spin-polarized density functional calculations of Fen aggregates with n ≤ 17 atoms to reveal the origin of the observed magic numbers, which indicate particularly high stability of clusters with 7, 13 and 15 atoms. Our results clarify the controversy regarding the ground state geometry of clusters such as Fe5and indicate that magnetism plays an important role in determining the stability and magic numbers in small iron clusters.

Concept Designed and Developed for Distortion- Tolerant, High-Stability Engine Control

NASA Technical Reports Server (NTRS)

1995-01-01

Engine Control Future aircraft turbine engines, both commercial and military, must be able to successfully accommodate expected increased levels of steady-state and dynamic engine-face distortion. Advanced tactical aircraft are likely to use thrust vectoring to enhance their maneuverability. As a result, the engines will see more extreme aircraft angles-of-attack and sideslip levels than are currently encountered with present-day aircraft. Also, the mixed-compression inlets needed for the High Speed Civil Transport will likely encounter disturbances similar to those seen by tactical aircraft, in addition to planar pulse, inlet buzz, and high distortion levels at low flight speed and off-design operation. The current approach of incorporating a sufficient component design stall margin to tolerate these increased levels of distortion would significantly reduce performance. The objective of the High Stability Engine Control (HISTEC) program is to design, develop, and flight demonstrate an advanced, high-stability, integrated engine-control system that uses measurement-based, real-time estimates of distortion to enhance engine stability. The resulting distortion-tolerant control reduces the required design stall margin, with a corresponding increase in performance and decrease in fuel burn. The HISTEC concept has been designed and developed, and the software implementing the concept has successfully accommodated time-varying distortion. The NASA Lewis Research Center is currently overseeing the development and validation of the hardware and software necessary to flight test the HISTEC concept. HISTEC is a contracted effort with Pratt & Whitney of West Palm Beach, Florida. The HISTEC approach includes two major systems: A Distortion Estimation System (DES) and Stability Management Control (SMC). DES is an aircraft-mounted, high-speed processor that estimates the amount and type of distortion present and its effect on the engine. It uses high-response pressure measurements at the engine face to calculate indicators of the type and extent of distortion in real time. From these indicators, DES determines the effects of distortion on the propulsion systems and the corresponding engine match point necessary to accommodate it. DES output consists of fan and compressor pressure ratio trim commands that are passed to the SMC. In addition, DES uses maneuver information, consisting of angle-of-attack and sideslip from the flight control, to anticipate high inlet distortion conditions. The SMC, which is contained in the engine-mounted, Improved Digital Electronic Engine Control (IDEEC), includes advanced control laws to directly control the fan and compressor transient operating line (pressure ratio). These advanced control laws, with a multivariable design, have the potential for higher bandwidth and the resulting more precise control of engine match. The ability to measure and assess the distortion effects in real time coupled with a high-response controller improves engine stability at high levels of distortion. The software algorithms implementing DES have been designed, developed, and demonstrated, and integration testing of the DES and SMC software has been completed. The results show that the HISTEC system will be able to sense inlet distortion, determine the effect on engine stability, and accommodate distortion by maintaining an adequate margin for engine surge. The Pratt &Whitney Comprehensive Engine Diagnostic Unit was chosen as the DES processor. An instrumented inlet case for sensing distortion was designed and fabricated. HISTEC is scheduled for flight test on the ACTIVE F-15 aircraft at the NASA Dryden Flight Research Center in Edwards, California, in late 1996.

Reduced Graphene Oxide-Wrapped FeS2 Composite as Anode for High-Performance Sodium-Ion Batteries

NASA Astrophysics Data System (ADS)

Wang, Qinghong; Guo, Can; Zhu, Yuxuan; He, Jiapeng; Wang, Hongqiang

2018-06-01

Iron disulfide is considered to be a potential anode material for sodium-ion batteries due to its high theoretical capacity. However, its applications are seriously limited by the weak conductivity and large volume change, which results in low reversible capacity and poor cycling stability. Herein, reduced graphene oxide-wrapped FeS2 (FeS2/rGO) composite was fabricated to achieve excellent electrochemical performance via a facile two-step method. The introduction of rGO effectively improved the conductivity, BET surface area, and structural stability of the FeS2 active material, thus endowing it with high specific capacity, good rate capability, as well as excellent cycling stability. Electrochemical measurements show that the FeS2/rGO composite had a high initial discharge capacity of 1263.2 mAh g-1 at 100 mA g-1 and a high discharge capacity of 344 mAh g-1 at 10 A g-1, demonstrating superior rate performance. After 100 cycles at 100 mA g-1, the discharge capacity remained at 609.5 mAh g-1, indicating the excellent cycling stability of the FeS2/rGO electrode.

Wavelet Filtering to Reduce Conservatism in Aeroservoelastic Robust Stability Margins

NASA Technical Reports Server (NTRS)

Brenner, Marty; Lind, Rick

1998-01-01

Wavelet analysis for filtering and system identification was used to improve the estimation of aeroservoelastic stability margins. The conservatism of the robust stability margins was reduced with parametric and nonparametric time-frequency analysis of flight data in the model validation process. Nonparametric wavelet processing of data was used to reduce the effects of external desirableness and unmodeled dynamics. Parametric estimates of modal stability were also extracted using the wavelet transform. Computation of robust stability margins for stability boundary prediction depends on uncertainty descriptions derived from the data for model validation. F-18 high Alpha Research Vehicle aeroservoelastic flight test data demonstrated improved robust stability prediction by extension of the stability boundary beyond the flight regime.

A validated analytical method to study the long-term stability of natural and synthetic glucocorticoids in livestock urine using ultra-high performance liquid chromatography coupled to Orbitrap-high resolution mass spectrometry.

PubMed

De Clercq, Nathalie; Julie, Vanden Bussche; Croubels, Siska; Delahaut, Philippe; Vanhaecke, Lynn

2013-08-02

Due to their growth-promoting effects, the use of synthetic glucocorticoids is strictly regulated in the European Union (Council Directive 2003/74/EC). In the frame of the national control plans, which should ensure the absence of residues in food products of animal origin, in recent years, a higher frequency of prednisolone positive bovine urines has been observed. This has raised questions with respect to the stability of natural corticoids in the respective urine samples and their potential to be transformed into synthetic analogs. In this study, a ultra high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) methodology was developed to examine the stability of glucocorticoids in bovine urine under various storage conditions (up to 20 weeks) and to define suitable conditions for sample handling and storage, using an Orbitrap Exactive™. To this end, an extraction procedure was optimized using a Plackett-Burman experimental design to determine the key conditions for optimal extraction of glucocorticoids from urine. Next, the analytical method was successfully validated according to the guidelines of CD 2002/657/EC. Decision limits and detection capabilities for prednisolone, prednisone and methylprednisolone ranged, respectively, from 0.1 to 0.5μgL(-1) and from 0.3 to 0.8μgL(-1). For the natural glucocorticoids limits of detection and limits of quantification for dihydrocortisone, cortisol and cortisone ranged, respectively, from 0.1 to 0.2μgL(-1) and from 0.3 to 0.8μgL(-1). The stability study demonstrated that filter-sterilization of urine, storage at -80°C, and acidic conditions (pH 3) were optimal for preservation of glucocorticoids in urine and able to significantly limit degradation up to 20 weeks. Copyright © 2013 Elsevier B.V. All rights reserved.

Corrosion testing of candidates for the alkaline fuel cell cathode

NASA Technical Reports Server (NTRS)

Singer, Joseph; Fielder, William L.

1989-01-01

Current/voltage data was obtained for specially made corrosion electrodes of some oxides and of gold materials for the purpose of developing a screening test of catalysts and supports for use at the cathode of the alkaline fuel cell. The data consists of measurements of current at fixed potentials and cyclic voltammograms. These data will have to be correlated with longtime performance data in order to fully evaluate this approach to corrosion screening. Corrosion test screening of candidates for the oxygen reduction electrode of the alkaline fuel cell was applied to two substances, the pyrochlore Pb2Ru2O6.5 and the spinel NiCo2O4. The substrate gold screen and a sample of the IFC Orbiter Pt-Au performance electrode were included as blanks. The pyrochlore data indicate relative stability, although nothing yet can be said about long term stability. The spinel was plainly unstable. For this type of testing to be validated, comparisons will have to be made with long term performance tests.

Validity, reliability and Norwegian adaptation of the Stroke-Specific Quality of Life (SS-QOL) scale

PubMed Central

Pedersen, Synne Garder; Heiberg, Guri Anita; Nielsen, Jørgen Feldbæk; Friborg, Oddgeir; Stabel, Henriette Holm; Anke, Audny; Arntzen, Cathrine

2018-01-01

Background: There is a paucity of stroke-specific instruments to assess health-related quality of life in the Norwegian language. The objective was to examine the validity and reliability of a Norwegian version of the 12-domain Stroke-Specific Quality of Life scale. Methods: A total of 125 stroke survivors were prospectively recruited. Questionnaires were administered at 3 months; 36 test–retests were performed at 12 months post stroke. The translation was conducted according to guidelines. The internal consistency was assessed with Cronbach’s alpha; convergent validity, with item-to-subscale correlations; and test–retest, with Spearman’s correlations. Scaling validity was explored by calculating both floor and ceiling effects. A priori hypotheses regarding the associations between the Stroke-Specific Quality of Life domain scores and scores of established measures were tested. Standard error of measurement was assessed. Results: The Norwegian version revealed no major changes in back translations. The internal consistency values of the domains were Cronbach’s alpha = 0.79–0.93. Rates of missing items were small, and the item-to-subscale correlation coefficients supported convergent validity (0.48–0.87). The observed floor effects were generally small, whereas the ceiling effects had moderate or high values (16%–63%). Test–retest reliability indicated stability in most domains, with Spearman’s rho = 0.67–0.94 (all p < 0.001), whereas the rho was 0.35 (p < 0.05) for the ‘Vision’ domain. Hypothesis testing supported the construct validity of the scale. Standard error of measurement values for each domain were generated to indicate the required magnitudes of detectable change. Conclusions: The Norwegian version of the Stroke-Specific Quality of Life scale is a reliable and valid instrument with good psychometric properties. It is suited for use in health research as well as in individual assessments of persons with stroke. PMID:29344360

Validity, reliability and Norwegian adaptation of the Stroke-Specific Quality of Life (SS-QOL) scale.

PubMed

Pedersen, Synne Garder; Heiberg, Guri Anita; Nielsen, Jørgen Feldbæk; Friborg, Oddgeir; Stabel, Henriette Holm; Anke, Audny; Arntzen, Cathrine

2018-01-01

There is a paucity of stroke-specific instruments to assess health-related quality of life in the Norwegian language. The objective was to examine the validity and reliability of a Norwegian version of the 12-domain Stroke-Specific Quality of Life scale. A total of 125 stroke survivors were prospectively recruited. Questionnaires were administered at 3 months; 36 test-retests were performed at 12 months post stroke. The translation was conducted according to guidelines. The internal consistency was assessed with Cronbach's alpha; convergent validity, with item-to-subscale correlations; and test-retest, with Spearman's correlations. Scaling validity was explored by calculating both floor and ceiling effects. A priori hypotheses regarding the associations between the Stroke-Specific Quality of Life domain scores and scores of established measures were tested. Standard error of measurement was assessed. The Norwegian version revealed no major changes in back translations. The internal consistency values of the domains were Cronbach's alpha = 0.79-0.93. Rates of missing items were small, and the item-to-subscale correlation coefficients supported convergent validity (0.48-0.87). The observed floor effects were generally small, whereas the ceiling effects had moderate or high values (16%-63%). Test-retest reliability indicated stability in most domains, with Spearman's rho = 0.67-0.94 (all p < 0.001), whereas the rho was 0.35 (p < 0.05) for the 'Vision' domain. Hypothesis testing supported the construct validity of the scale. Standard error of measurement values for each domain were generated to indicate the required magnitudes of detectable change. The Norwegian version of the Stroke-Specific Quality of Life scale is a reliable and valid instrument with good psychometric properties. It is suited for use in health research as well as in individual assessments of persons with stroke.

Stability characterization and modeling of robust distributed benthic microbial fuel cell (DBMFC) system.

PubMed

Karra, Udayarka; Huang, Guoxian; Umaz, Ridvan; Tenaglier, Christopher; Wang, Lei; Li, Baikun

2013-09-01

A novel and robust distributed benthic microbial fuel cell (DBMFC) was developed to address the energy supply issues for oceanographic sensor network applications, especially under scouring and bioturbation by aquatic life. Multi-anode/cathode configuration was employed in the DBMFC system for enhanced robustness and stability in the harsh ocean environment. The results showed that the DBMFC system achieved peak power and current densities of 190mW/m(2) and 125mA/m(2) respectively. Stability characterization tests indicated the DBMFC with multiple anodes achieved higher power generation over the systems with single anode. A computational model that integrated physical, electrochemical and biological factors of MFCs was developed to validate the overall performance of the DBMFC system. The model simulation well corresponded with the experimental results, and confirmed the hypothesis that using a multi anode/cathode MFC configuration results in reliable and robust power generation. Published by Elsevier Ltd.

Agility performance in high-level junior basketball players: the predictive value of anthropometrics and power qualities.

PubMed

Sisic, Nedim; Jelicic, Mario; Pehar, Miran; Spasic, Miodrag; Sekulic, Damir

2016-01-01

In basketball, anthropometric status is an important factor when identifying and selecting talents, while agility is one of the most vital motor performances. The aim of this investigation was to evaluate the influence of anthropometric variables and power capacities on different preplanned agility performances. The participants were 92 high-level, junior-age basketball players (16-17 years of age; 187.6±8.72 cm in body height, 78.40±12.26 kg in body mass), randomly divided into a validation and cross-validation subsample. The predictors set consisted of 16 anthropometric variables, three tests of power-capacities (Sargent-jump, broad-jump and medicine-ball-throw) as predictors. The criteria were three tests of agility: a T-Shape-Test; a Zig-Zag-Test, and a test of running with a 180-degree turn (T180). Forward stepwise multiple regressions were calculated for validation subsamples and then cross-validated. Cross validation included correlations between observed and predicted scores, dependent samples t-test between predicted and observed scores; and Bland Altman graphics. Analysis of the variance identified centres being advanced in most of the anthropometric indices, and medicine-ball-throw (all at P<0.05); with no significant between-position-differences for other studied motor performances. Multiple regression models originally calculated for the validation subsample were then cross-validated, and confirmed for Zig-zag-Test (R of 0.71 and 0.72 for the validation and cross-validation subsample, respectively). Anthropometrics were not strongly related to agility performance, but leg length is found to be negatively associated with performance in basketball-specific agility. Power capacities are confirmed to be an important factor in agility. The results highlighted the importance of sport-specific tests when studying pre-planned agility performance in basketball. The improvement in power capacities will probably result in an improvement in agility in basketball athletes, while anthropometric indices should be used in order to identify those athletes who can achieve superior agility performance.

[Validity and Reliability of the Attitudes Toward Sexuality in the Elderly Questionnaire in Cartagena, Colombia].

PubMed

Melguizo-Herrera, Estela; Álvarez-Romero, Yuleysi; Cabarcas-Mendoza, Mayerlin Vanessa; Calvo-Rodríguez, Rossy Stefanie; Flórez-Almanza, Jeomaidis; Moadie-Contreras, Olga Patricia; Campo-Arias, Adalberto

2015-01-01

There are many stereotypes and prejudices about the sexual lives of the elderly. However, there are no validated and reliable tools for measuring these in the Latin-American context. To determine the internal consistency, dimensionality, differential item functioning (DIF) by gender and stability of the Attitudes towards Sexuality in the Elderly Questionnaire (ASEQ) in adults over 60 years-old in Cartagena, Colombia. A validation study was designed that included a sample of 130 participants without cognitive impairment attending a Life Center. The ages ranged between 60 and 90 years (mean, 73.7±8.0), and there were 61.5% females. Internal consistency was calculated using Cronbach alpha and McDonald omega, exploratory factor analysis (EFA) (dimensionality), DIF by gender (item response theory) with Kendall correlation, and stability (reproducibility) with Pearson correlation and intraclass correlation coefficient (ICC). The ASEQ showed high internal consistency on the first application (α=.83 and ω=.87) and in the second one (α=.85 and ω=.89). AFE showed two salient factors (prejudices and limitations) that explained 42.6% of the total variance. The IDF presented appropriate coefficients, with the exception of item 14 that showed a high value (τ=.37). ASEQ showed high stability (r=.82 and ICC=.89; 95% confidence interval, 0.83- 0.92; P<.001). ASEQ is a two-dimensional and reliable scale in older adults attending a Life Center in Cartagena, Colombia. New studies are required to evaluate the performance in a representative sample. Copyright © 2014 Asociación Colombiana de Psiquiatría. Publicado por Elsevier España. All rights reserved.

Development and validation of a stability-indicating LC method for the assay of lodenafil carbonate in tablets.

PubMed

Codevilla, Cristiane Franco; Lemos, Alice Machado; Delgado, Leila Schreiner; Rolim, Clarice Madalena Bueno; Adams, Andréa Inês Horn; Bergold, Ana Maria

2011-08-01

A stability-indicating liquid chromatographic method has been developed for the quantitative determination of lodenafil carbonate in tablets. The method employs a Synergi Fusion C18 column (250 × 4.6 mm, i.d., 4 μm particle size), with mobile phase consisting of a mixture of methanol-acetic acid 0.1% pH 4.0 (65:35, v/v) and UV detection at 290 nm, using a photodiode array detector. A linear response (r = 0.9999) was observed in the range of 10-80 μg/mL. The method showed good recoveries (average 100.3%) and also intra and inter-day precision (RSD < 2.0%). Validation parameters as specificity and robustness were also determined. Specificity analysis showed that no impurities or degradation products were co-eluting with the lodenafil carbonate peak. The method was found to be stability-indicating and due to its simplicity and accuracy can be applied for routine quality control analysis of lodenafil carbonate in tablets.

Least-Squares Regression and Spectral Residual Augmented Classical Least-Squares Chemometric Models for Stability-Indicating Analysis of Agomelatine and Its Degradation Products: A Comparative Study.

PubMed

Naguib, Ibrahim A; Abdelrahman, Maha M; El Ghobashy, Mohamed R; Ali, Nesma A

2016-01-01

Two accurate, sensitive, and selective stability-indicating methods are developed and validated for simultaneous quantitative determination of agomelatine (AGM) and its forced degradation products (Deg I and Deg II), whether in pure forms or in pharmaceutical formulations. Partial least-squares regression (PLSR) and spectral residual augmented classical least-squares (SRACLS) are two chemometric models that are being subjected to a comparative study through handling UV spectral data in range (215-350 nm). For proper analysis, a three-factor, four-level experimental design was established, resulting in a training set consisting of 16 mixtures containing different ratios of interfering species. An independent test set consisting of eight mixtures was used to validate the prediction ability of the suggested models. The results presented indicate the ability of mentioned multivariate calibration models to analyze AGM, Deg I, and Deg II with high selectivity and accuracy. The analysis results of the pharmaceutical formulations were statistically compared to the reference HPLC method, with no significant differences observed regarding accuracy and precision. The SRACLS model gives comparable results to the PLSR model; however, it keeps the qualitative spectral information of the classical least-squares algorithm for analyzed components.

Wechsler Adult Intelligence Scale-Fourth Edition (WAIS-IV) processing speed scores as measures of noncredible responding: The third generation of embedded performance validity indicators.

PubMed

Erdodi, Laszlo A; Abeare, Christopher A; Lichtenstein, Jonathan D; Tyson, Bradley T; Kucharski, Brittany; Zuccato, Brandon G; Roth, Robert M

2017-02-01

Research suggests that select processing speed measures can also serve as embedded validity indicators (EVIs). The present study examined the diagnostic utility of Wechsler Adult Intelligence Scale-Fourth Edition (WAIS-IV) subtests as EVIs in a mixed clinical sample of 205 patients medically referred for neuropsychological assessment (53.3% female, mean age = 45.1). Classification accuracy was calculated against 3 composite measures of performance validity as criterion variables. A PSI ≤79 produced a good combination of sensitivity (.23-.56) and specificity (.92-.98). A Coding scaled score ≤5 resulted in good specificity (.94-1.00), but low and variable sensitivity (.04-.28). A Symbol Search scaled score ≤6 achieved a good balance between sensitivity (.38-.64) and specificity (.88-.93). A Coding-Symbol Search scaled score difference ≥5 produced adequate specificity (.89-.91) but consistently low sensitivity (.08-.12). A 2-tailed cutoff on the Coding/Symbol Search raw score ratio (≤1.41 or ≥3.57) produced acceptable specificity (.87-.93), but low sensitivity (.15-.24). Failing ≥2 of these EVIs produced variable specificity (.81-.93) and sensitivity (.31-.59). Failing ≥3 of these EVIs stabilized specificity (.89-.94) at a small cost to sensitivity (.23-.53). Results suggest that processing speed based EVIs have the potential to provide a cost-effective and expedient method for evaluating the validity of cognitive data. Given their generally low and variable sensitivity, however, they should not be used in isolation to determine the credibility of a given response set. They also produced unacceptably high rates of false positive errors in patients with moderate-to-severe head injury. Combining evidence from multiple EVIs has the potential to improve overall classification accuracy. (PsycINFO Database Record (c) 2017 APA, all rights reserved).

Stability of Clindamycin Hydrochloride in PCCA Base SuspendIt.

PubMed

Pramar, Yashoda V; Graves, Richard A; Ledet, Grace A; Phan, Kelly V; Bostanian, Levon A; Mandal, Tarun K

2016-01-01

Clindamycin is an effective antibiotic in the treatment of infections caused by certain gram-positive and gram-negative anaerobic microorganisms. While manufactured forms of the drug for pediatric use are available, there are instances when a compounded liquid dosage form is essential to meet unique patient needs. The purpose of this study was to determine the chemical stability of clindamycin hydrochloride in the PCCA base SuspendIt, a sugar-free, paraben- free, dye-free, and gluten-free thixotropic vehicle containing a natural sweetener obtained from the monk fruit. It thickens upon standing to minimize settling of any insoluble drug particles and becomes fluid upon shaking to allow convenient pouring during administration to the patient. A robust stability-indicating high-performance liquid chromatographic assay for the determination of clindamycin hydrochloride in SuspendIt was developed and validated. This assay was used to determine the chemical stability of the drug in SuspendIt. Samples were prepared and stored under three different temperature conditions (5°C, 25°C, and 40°C), and assayed using the high-performance liquid chromatographic assay at pre-determined intervals over an extended period of time as follows: 7, 14, 30, 45, 60, 91, 120, and 182 days at each designated temperature. Physical data such as pH, viscosity, and appearance were also monitored. The study showed that drug concentration did not go below 90% of the label claim (initial drug concentration) at all three temperatures studied, barring isolated experimental errors. Viscosity and pH values also did not change significantly. Some variations in viscosity were attributed to the thixotropic nature of the vehicle. This study demonstrates that clindamycin hydrochloride is physically and chemically stable in SuspendIt for 182 days in the refrigerator and at room temperature, thus providing a viable, compounded alternative for clindamycin hydrochloride in a liquid dosage form, with an extended beyond-use date to meet patient needs. Copyright© by International Journal of Pharmaceutical Compounding, Inc.

Is Learner Self-Assessment Reliable and Valid in a Web-Based Portfolio Environment for High School Students?

ERIC Educational Resources Information Center

Chang, Chi-Cheng; Liang, Chaoyun; Chen, Yi-Hui

2013-01-01

This study explored the reliability and validity of Web-based portfolio self-assessment. Participants were 72 senior high school students enrolled in a computer application course. The students created learning portfolios, viewed peers' work, and performed self-assessment on the Web-based portfolio assessment system. The results indicated: 1)…

ACCESS - A Science and Engineering Assessment of Space Coronagraph Concepts for the Direct Imaging and Spectroscopy of Exoplanetary Systems

NASA Technical Reports Server (NTRS)

Trauger, John

2008-01-01

Topics include and overview, science objectives, study objectives, coronagraph types, metrics, ACCESS observatory, laboratory validations, and summary. Individual slides examine ACCESS engineering approach, ACCESS gamut of coronagraph types, coronagraph metrics, ACCESS Discovery Space, coronagraph optical layout, wavefront control on the "level playing field", deformable mirror development for HCIT, laboratory testbed demonstrations, high contract imaging with the HCIT, laboratory coronagraph contrast and stability, model validation and performance predictions, HCIT coronagraph optical layout, Lyot coronagraph on the HCIT, pupil mapping (PIAA), shaped pupils, and vortex phase mask experiments on the HCIT.

Differential nephrotoxicity of cisplatin and a novel series of traditional Chinese medicine-platinum anticancer agents correlates with their chemical reactivity towards sulfur-containing nucleophiles.

PubMed

To, Kenneth K W; Au-Yeung, Steve C F; Ho, Yee-Ping

2006-07-01

A series of novel traditional Chinese medicine-platinum compounds has been found to be active against a number of murine and human cancers both in vitro and in vivo. Their high potency and the lack of cisplatin cross-resistance are believed to be due to the inclusion of the protein phosphatase 2A-inhibiting demethylcantharidin in the novel structures. A simple reversed-phase high-performance liquid chromatographic method was developed and validated as a stability-indicating assay for the platinum compounds. Using cisplatin and carboplatin as reference compounds, the stability study agrees well with the literature-reported findings. The novel traditional Chinese medicine-platinum compounds were more stable than cisplatin in water and dextrose, but became unstable in normal saline, a characteristic similar to that of carboplatin. The developed assay was further applied to study the chemical reactivity of the novel platinum compounds towards physiologically important nucleophiles such as glutathione and cysteine. The novel compounds were considerably less reactive to the sulfur-containing nucleophiles than cisplatin. In-vitro cytotoxicity assay was performed in a porcine kidney LLC-PK1 cell line model to investigate the nephrotoxicity potential of the platinum compounds. The lower rate of hydrolysis and the decreased reactivity of the novel traditional Chinese medicine-platinum compounds towards sulfur-containing bionucleophiles appear to have reduced their toxicity when compared with cisplatin, yet the antitumor activities of the novel compounds have not been compromised.

Development and application of a validated stability-indicating high-performance liquid chromatographic method using photodiode array detection for simultaneous determination of granisetron, methylparaben, propylparaben, sodium benzoate, and their main degradation products in oral pharmaceutical preparations.

PubMed

Hewala, Ismail; El-Fatatry, Hamed; Emam, Ehab; Mabrouk, Mokhtar

2011-01-01

A simple, rapid, and sensitive RP-HPLC method using photodiode array detection was developed and validated for the simultaneous determination of granisetron hydrochloride, 1-methyl-1H-indazole-3-carboxylic acid (the main degradation product of granisetron), sodium benzoate, methylparaben, propylparaben, and 4-hydroxybenzoic acid (the main degradation product of parabens) in granisetron oral drops and solutions. The separation of the compounds was achieved within 8 min on a SymmetryShield RP18 column (100 x 4.6 mm id, 3.5 microm particle size) using the mobile phase acetonitrile--0.05 M KH2PO4 buffered to pH 3 using H3PO4 (3+7, v/v). The photodiode array detector was used to test the purity of the peaks, and the chromatograms were extracted at 240 nm. The method was validated, and validation acceptance criteria were met in all cases. The robust method was successfully applied to the determination of granisetron and preservatives, as well as their degradation products in different batches of granisetron oral drops and solutions. The method proved to be sensitive for determination down to 0.04% (w/w) of granisetron degradation product relative to granisetron and 0.03% (w/w) 4-hydroxybenzoic acid relative to total parabens.

Tailoring the surface properties of LiNi 0.4Mn 0.4Co 0.2O₂ by titanium substitution for improved high voltage cycling performance

DOE PAGES

Wolff-Goodrich, Silas; Xin, Huolin L.; Lin, Feng; ...

2015-07-30

The present research aims to provide insights into the behavior of LiNi0.4Mn0.4Co0.2O2 (NMC442) and LiNi 0.4Mn 0.4Co 0.2O₂ (NMC442-Ti02) cathode materials under galvanostatic cycling to high potentials, in the context of previous work which predicted that Ti-substituted variants should deliver higher capacities and exhibit better cycling stability than the unsubstituted compounds. It is found that NMC cathodes containing Ti show equivalent capacity fading but greater specific capacity than those without Ti in the same potential range. When repeatedly charged to the same degree of delithiation, NMC cathodes containing Ti showed better capacity retention. Soft x-ray absorption spectroscopy (XAS) spectra formore » Mn and Co indicated increased reduction in these elements for NMC cathodes without Ti, indicating that the substitution of Ti for Co acts to suppress the formation of a high impedance rock salt phase at the surface of NMC cathode particles. The results of this study validate the adoption of a facile change to existing NMC chemistries to improve cathode capacity retention under high voltage cycling conditions.« less

A Pilot Stability Study of Dehydroepiandrosterone Rapid-dissolving Tablets Prepared by Extemporaneous Compounding.

PubMed

Rush, Steven D; Vernak, Charlene; Zhao, Fang

2017-01-01

Dehydroepiandrosterone supplementation is used to treat a variety of conditions. Rapid-dissolving tablets are a relatively novel choice for compounded dehydroepiandrosterone dosage forms. While rapid-dissolving tablets offer ease of administration, there are uncertainties about the physical and chemical stability of the drug and dosage form during preparation and over long-term storage. This study was designed to evaluate the stability of dehydroepiandrosterone rapid-dissolving tablets just after preparation and over six months of storage. The Professional Compounding Centers of America rapid-dissolving tablet mold and base formula were used to prepare 10-mg strength dehydroepiandrosterone rapid-dissolving tablets. The formulation was heated at 100°C to 110°C for 30 minutes, released from the mold, and cooled at room temperature for 30 minutes. The resulting rapid-dissolving tablets were individually packaged in amber blister packs and stored in a stability chamber maintained at 25°C and 60% relative humidity. The stability samples were pulled at pre-determined time points for evaluation, which included visual inspection, tablet weight check, United States Pharmacopeia disintegration test, and stability-indicating high-performance liquid chromatography. The freshly prepared dehydroepiandrosterone rapiddissolving tablets exhibited satisfactory chemical and physical stability. Time 0 samples disintegrated within 40 seconds in water kept at 37°C. The high-performance liquid chromatographic results confirmed that the initial potency was 101.9% of label claim and that there was no chemical degradation from the heating procedure. Over six months of storage, there were no significant changes in visual appearance, physical integrity, or disintegration time for any of the stability samples. The high-performance liquid chromatographic results also indicated that dehydroepiandrosterone rapid-dissolving tablets retained >95% label claim with no detectable degradation products. The dehydroepiandrosterone rapid-dissolving tablets investigated in this pilot study were physically and chemically stable during preparation and over six months of storage at 25°C and 60% relative humidity. Copyright© by International Journal of Pharmaceutical Compounding, Inc.

JWST Point Spread Function Quality and Stability: Ground Testing, Integrated Modeling, and Space Validation

NASA Technical Reports Server (NTRS)

McElwain, Michael; Van Gorkom, Kyle; Bowers, Charles W.; Carnahan, Timothy M.; Kimble, Randy A.; Knight, J. Scott; Lightsey, Paul; Maghami, Peiman G.; Mustelier, David; Niedner, Malcolm B.;

A Historical Review of Cermet Fuel Development and the Engine Performance Implications

NASA Technical Reports Server (NTRS)

Stewart, Mark E. M.

2015-01-01

This paper reviews test data for cermet fuel samples developed in the 1960's to better quantify Nuclear Thermal Propulsion (NTP) cermet engine performance, and to better understand contemporary fuel testing results. Over 200 cermet (W-UO2) samples were tested by thermally cycling to 2500 deg (2770 K) in hydrogen. The data indicates two issues at high temperatures: the vaporization rate of UO2 and the chemical stability of UO2. The data show that cladding and chemical stabilizers each result in large, order of magnitude improvements in high temperature performance, while other approaches yield smaller, incremental improvements. Data is very limited above 2770 K, and this complicates predictions of engine performance at high Isp. The paper considers how this material performance data translates into engine performance. In particular, the location of maximum temperature within the fuel element and the effect of heat deposition rate are examined.

Aeromechanical stability analysis of COPTER

NASA Technical Reports Server (NTRS)

Yin, Sheng K.; Yen, Jing G.

1988-01-01

A plan was formed for developing a comprehensive, second-generation system with analytical capabilities for predicting performance, loads and vibration, handling qualities, aeromechanical stability, and acoustics. This second-generation system named COPTER (COmprehensive Program for Theoretical Evaluation of Rotorcraft) is designed for operational efficiency, user friendliness, coding readability, maintainability, transportability, modularity, and expandability for future growth. The system is divided into an executive, a data deck validator, and a technology complex. At present a simple executive, the data deck validator, and the aeromechanical stability module of the technology complex were implemented. The system is described briefly, the implementation of the technology module is discussed, and correlation data presented. The correlation includes hingeless-rotor isolated stability, hingeless-rotor ground-resonance stability, and air-resonance stability of an advanced bearingless-rotor in forward flight.

Determination of osthol and its metabolites in a phase I reaction system and the Caco-2 cell model by HPLC-UV and LC-MS/MS

PubMed Central

Yuan, Zhenting; Xu, Haiyan; Wang, Ke; Zhao, Zhonghua; Hu, Ming

2012-01-01

A straightforward and sensitive reversed-phase high-performance liquid chromatography (HPLC) assay was developed and validated for the analysis of osthol and its phase I metabolites (internal standard: umbelliferone). The method was validated for the determination of osthol with respect to selectivity, precision, linearity, limit of detection, recovery, and stability. The linear response range was 0.47 ~ 60 μM, and the average recoveries ranged from 98 to 101%. The inter-day and intra-day relative standard deviations were both less than 5%. Using this method, we showed that more than 80% of osthol was metabolized in 20 min in a phase I metabolic reaction system. Transport experiments in the Caco-2 cell culture model indicated that osthol was easily absorbed with high absorptive permeability (>10×10-6 cm/sec). The permeability did not display concentration-dependence or vectorial-dependence and is mildly temperature sensitive (activation energy less than 10 Kcal/mole), indicating passive mechanism of transport. When analyzed by LC-MS/MS, five metabolites were detected in a phase I reaction system and in the receiver side of a modified Caco-2 cell model, which was supplemented with the phase I reaction system. The major metabolites appeared to be desmethyl-osthol and multiple isomers of dehydro-osthol. In conclusion, a likely cause of poor osthol bioavailability is rapid phase I metabolism via the cytochrome P-450 pathways. PMID:19304430

FT4 Data Analysis Summary (SSI-ARC)

NASA Technical Reports Server (NTRS)

Isaacson, Douglas R.; Gong, Chester; Reardon, Scott Edward; Santiago, Confesor

2016-01-01

Standards for Unmanned Aircraft System (UAS) Detect-and-Avoid (DAA) systems are currently being developed under the auspices of the RTCA Special Committee 228 (SC-228). To support the development of these standards, a series of flight tests has been conducted at NASAs Armstrong Flight Research Center (NASA-AFRC). The fourth in this series of flight test activities (Flight Test 4, or simply FT4) was conducted during the Spring and Summer of 2016. FT4 supported the objectives of numerous organizations working toward UAS DAA Minimum Operational Performance Standards (MOPS) and UAS DAA Radar MOPS. The summary provided herein is limited to the objectives, analysis and conclusions of the NASA Ames Research Center (NASA-ARC) SSI team toward the refinement of UAS DAA MOPS. This document provides a high-level overview of FT4 and the SSI-ARC objectives, a summary of the data analysis methodology and recommendations for UAS DAA MOPS refinements based on the data analysis results. A total of 72 encounters were flown to support SSI-ARC objectives. Test results were generally consistent with acceptable UAS DAA system performance and will be considered in broader SC-228 requirements validation efforts. Observed alert lead times indicated acceptable UAS DAA alerting performance. Effective interoperability between the UAS DAA system and the Traffic Alert and Collision Avoidance System (TCAS) was observed with one notable exception: TCAS Resolutions Advisories (RA) were observed in the absence of any DAA alert on two occasions, indicating the need for alert parameter refinement. Findings further indicated the need for continued work in the areas of DAA Well Clear Recovery logic and alert stability for Mode-C-only intruders. Finally, results demonstrated a high level of compliance with a set of evaluation criteria designed to provide anecdotal evidence of acceptable UAS DAA system performance.

Long-term urine biobanking: storage stability of clinical chemical parameters under moderate freezing conditions without use of preservatives.

PubMed

Remer, Thomas; Montenegro-Bethancourt, Gabriela; Shi, Lijie

2014-12-01

To examine the long-term stability and validity of analyte concentrations of 21 clinical biochemistry parameters in 24-h urine samples stored for 12 or 15 yr at -22°C and preservative free. Healthy children's 24-h urine samples in which the respective analytes had been measured shortly after sample collection (baseline) were reanalyzed. Second measurement was performed after 12 yr (organic acids) and 15 yr (creatinine, urea, osmolality, iodine, nitrogen, anions, cations, acid-base parameters) with the same analytical methodology. Paired comparisons and correlations between the baseline and repeated measurements were done. Recovery rates were calculated. More than half of the analytes (creatinine, urea, iodine, nitrogen, sodium, potassium, magnesium, calcium, ammonium, bicarbonate, citric & uric acid) showed measurement values after >10 yr of storage not significantly different from baseline. 15 of the 21 parameters were highly correlated (r=0.99) between baseline and second measurement. Poorest correlation was r=0.77 for oxalate. Recovery ranged from 73% (oxalate) to 105% (phosphate). Our results suggest high long-term stability and measurement validity for numerous clinical chemistry parameters stored at -22°C without addition of any urine preservative. Prospective storage of urine aliquots at -22°C for periods even exceeding 10 yr, appears to be an acceptable and valid tool in epidemiological settings for later quantification of several urine analytes. Copyright © 2014 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Thirty-Year Stability and Predictive Validity of Vocational Interests

ERIC Educational Resources Information Center

Rottinghaus, Patrick J.; Coon, Kristin L.; Gaffey, Abigail R.; Zytowski, Donald G.

2007-01-01

This study reports a 30-year follow-up of 107 former high school juniors and seniors from a rural Midwestern community who completed the Kuder Occupational Interest Survey (KOIS) in 1975 and 2005. Absolute, intra-individual, and test-retest stability of interests, and predictive validity of occupations were examined. Results showed minor absolute…

Developing and testing the CHORDS: Characteristics of Responsible Drinking Survey.

PubMed

Barry, Adam E; Goodson, Patricia

2011-01-01

Report on the development and psychometric testing of a theoretically and evidence-grounded instrument, the Characteristics of Responsible Drinking Survey (CHORDS). Instrument subjected to four phases of pretesting (cognitive validity, cognitive and motivational qualities, pilot test, and item evaluation) and a final posttest implementation. Large public university in Texas. Randomly selected convenience sample (n  =  729) of currently enrolled students. This 78-item questionnaire measures individuals' responsible drinking beliefs, motivations, intentions, and behaviors. Cronbach α, split-half reliability, principal components analysis and Spearman ρ were conducted to investigate reliability, stability, and validity. Measures in the CHORDS exhibited high internal consistency reliability and strong correlations of split-half reliability. Factor analyses indicated five distinct scales were present, as proposed in the theoretical model. Subscale composite scores also exhibited a correlation to alcohol consumption behaviors, indicating concurrent validity. The CHORDS represents the first instrument specifically designed to assess responsible drinking beliefs and behaviors. It was found to elicit valid and reliable data among a college student sample. This instrument holds much promise for practitioners who desire to empirically investigate dimensions of responsible drinking.

Psychometrics and life history strategy: the structure and validity of the High K Strategy Scale.

PubMed

Copping, Lee T; Campbell, Anne; Muncer, Steven

2014-03-22

In this paper, we critically review the conceptualization and implementation of psychological measures of life history strategy associated with Differential K theory. The High K Strategy Scale (HKSS: Giosan, 2006) was distributed to a large British sample (n = 809) with the aim of assessing its factor structure and construct validity in relation to theoretically relevant life history variables: age of puberty, age of first sexual encounter, and number of sexual partners. Exploratory and confirmatory factor analyses indicated that the HKSS in its current form did not show an adequate statistical fit to the data. Modifications to improve fit indicated four correlated factors (personal capital, environmental stability, environmental security, and social capital). Later puberty in women was positively associated with measures of the environment and personal capital. Among men, contrary to Differential K predictions but in line with female mate preferences, earlier sexual debut and more sexual partners were positively associated with more favorable environments and higher personal and social capital. We raise concerns about the use of psychometric indicators of lifestyle and personality as proxies for life history strategy when they have not been validated against objective measures derived from contemporary life history theory and when their status as causes, mediators, or correlates has not been investigated.

Developing an Index to Measure Health System Performance: Measurement for Districts of Nepal.

PubMed

Kandel, N; Fric, A; Lamichhane, J

2014-01-01

Various frameworks for measuring health system performance have been proposed and discussed. The scope of using performance indicators are broad, ranging from examining national health system to individual patients at various levels of health system. Development of innovative and easy index is essential to measure multidimensionality of health systems. We used indicators, which also serve as proxy to the set of activities, whose primary goal is to maintain and improve health. We used eleven indicators of MDGs, which represent all dimensions of health to develop index. These indicators are computed with similar methodology that of human development index. We used published data of Nepal for computation of the index for districts of Nepal as an illustration. To validate our finding, we compared the indices of these districts with other development indices of Nepal. An index for each district has been computed from eleven indicators. Then indices are compared with that of human development index, socio-economic and infrastructure development indices and findings has shown the similarity on distribution of districts. Categories of low and high performing districts on health system performance are also having low and high human development, socio-economic, and infrastructure indices respectively. This methodology of computing index from various indicators could assist policy makers and program managers to prioritize activities based on their performance. Validation of the findings with that of other development indicators show that this can be one of the tools, which can assist on assessing health system performance for policy makers, program managers and others.

Determination of rifampicin in human plasma by high-performance liquid chromatography coupled with ultraviolet detection after automatized solid-liquid extraction.

PubMed

Louveau, B; Fernandez, C; Zahr, N; Sauvageon-Martre, H; Maslanka, P; Faure, P; Mourah, S; Goldwirt, L

2016-12-01

A precise and accurate high-performance liquid chromatography (HPLC) quantification method of rifampicin in human plasma was developed and validated using ultraviolet detection after an automatized solid-phase extraction. The method was validated with respect to selectivity, extraction recovery, linearity, intra- and inter-day precision, accuracy, lower limit of quantification and stability. Chromatographic separation was performed on a Chromolith RP 8 column using a mixture of 0.05 m acetate buffer pH 5.7-acetonitrile (35:65, v/v) as mobile phase. The compounds were detected at a wavelength of 335 nm with a lower limit of quantification of 0.05 mg/L in human plasma. Retention times for rifampicin and 6,7-dimethyl-2,3-di(2-pyridyl) quinoxaline used as internal standard were respectively 3.77 and 4.81 min. This robust and exact method was successfully applied in routine for therapeutic drug monitoring in patients treated with rifampicin. Copyright © 2016 John Wiley & Sons, Ltd.

Development and validation of stability indicating HPLC methods for related substances and assay analyses of amoxicillin and potassium clavulanate mixtures.

PubMed

Bellur Atici, Esen; Yazar, Yücel; Ağtaş, Çağan; Ridvanoğlu, Nurten; Karlığa, Bekir

2017-03-20

Antibacterial combinations consisting of the semisynthetic antibiotic amoxicillin (amox) and the β-lactamase inhibitor potassium clavulanate (clav) are commonly used and several chromatographic methods were reported for their quantification in mixtures. In the present work, single HPLC method for related substances analyses of amoxicillin and potassium clavulanate mixtures was developed and validated according to international conference on harmonization (ICH) guidelines. Eighteen amoxicillin and six potassium clavulanate impurities were successfully separated from each other by using triple gradient elution using a Thermo Hypersil Zorbax BDS C18 (250 mm×4.6mm, 3μm) column with 50μL injection volumes at a wavelength of 215nm. Commercially unavailable impurities were formed by degradation of amoxicillin and potassium clavulanate, identified by LC-MS studies and used during analytical method development and validation studies. Also, process related amoxicillin impurity-P was synthesized and characterized by using nuclear magnetic resonance (NMR) and mass spectroscopy (MS) for the first time. As complementary of this work, an assay method for amoxicillin and potassium clavulanate mixtures was developed and validated; stress-testing and stability studies of amox/clav mixtures was carried out under specified conditions according to ICH and analyzed by using validated stability-indicating assay and related substances methods. Copyright © 2016 Elsevier B.V. All rights reserved.

Healing of voids in the aluminum metallization of integrated circuit chips

NASA Technical Reports Server (NTRS)

Cuddihy, Edward F.; Lawton, Russell A.; Gavin, Thomas R.

1990-01-01

The thermal stability of GaAs modulation-doped field effect transistors (MODFETs) is evaluated in order to identify failure mechanisms and validate the reliability of these devices. The transistors were exposed to thermal step-stress and characterized at ambient temperatures to indicate device reliability, especially that of the transistor ohmic contacts with and without molybdenum diffusion barriers. The devices without molybdenum exhibited important transconductance deterioration. MODFETs with molybdenum diffusion barriers were tolerant to temperatures above 300 C. This tolerance indicates that thermally activated failure mechanisms are slow at operational temperatures. Therefore, high-reliability MODFET-based circuits are possible.

Nonlinear stability and control study of highly maneuverable high performance aircraft, phase 2

NASA Technical Reports Server (NTRS)

Mohler, R. R.

1992-01-01

This research should lead to the development of new nonlinear methodologies for the adaptive control and stability analysis of high angle-of-attack aircraft such as the F18 (HARV). The emphasis has been on nonlinear adaptive control, but associated model development, system identification, stability analysis and simulation is performed in some detail as well. Various models under investigation for different purposes are summarized in tabular form. Models and simulation for the longitudinal dynamics have been developed for all types except the nonlinear ordinary differential equation model. Briefly, studies completed indicate that nonlinear adaptive control can outperform linear adaptive control for rapid maneuvers with large changes in alpha. The transient responses are compared where the desired alpha varies from 5 degrees to 60 degrees to 30 degrees and back to 5 degrees in all about 16 sec. Here, the horizontal stabilator is the only control used with an assumed first-order linear actuator with a 1/30 sec time constant.

Identification and Structure Elucidation of Forced Degradation Products of the Novel Propionic acid Derivative Loxoprofen: Development of Stability-Indicating Chromatographic Methods Validated as per ICH Guidelines.

PubMed

Eissa, Maya S; Abd El-Sattar, Osama I

2017-04-01

Loxoprofen sodium (LOX) is a recently developed novel propionic acid derivative. Owing to its instability under both hydrolytic and oxidative conditions, the development of simple, rapid and sensitive methods for its determination in the presence of its possible forced degradation products becomes essential. Two simple chromatographic methods, high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC), were developed associated with ultraviolet (UV) detection. In HPTLC-densitometric method, the separation of LOX from its degradation products was achieved using silica gel F254 plates and toluene:acetone:acetic acid (1.8:1.0:0.1, v/v/v) as the developing system followed by densitometric scanning at 220 nm. In the HPLC-UV method, the separation was performed using isocratic elution system with acetonitrile: 0.15% triethylamine (pH 2.2) (50:50, v/v) on C18 analytical column. The flow rate was optimized at 1.0 mL·min-1 and UV detection was achieved at 220 nm. Validation was performed in accordance with the International Conference on Harmonization guidelines and the method was perfectly applied for determination of LOX in its pharmaceutical preparation. The results obtained were statistically compared to those obtained after application of the official HPLC method, where no significant difference was found incompliance with precision and accuracy. Identification and characterization of the possible hydrolytic degradation product under alkaline conditions and that produced during oxidative degradation using hydrogen peroxide were structurally elucidated using infrared and mass spectrometry analyses. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A systematic review of the asymmetric inheritance of cellular organelles in eukaryotes: A critique of basic science validity and imprecision

PubMed Central

Collins, Anne; Ross, Janine

2017-01-01

We performed a systematic review to identify all original publications describing the asymmetric inheritance of cellular organelles in normal animal eukaryotic cells and to critique the validity and imprecision of the evidence. Searches were performed in Embase, MEDLINE and Pubmed up to November 2015. Screening of titles, abstracts and full papers was performed by two independent reviewers. Data extraction and validity were performed by one reviewer and checked by a second reviewer. Study quality was assessed using the SYRCLE risk of bias tool, for animal studies and by developing validity tools for the experimental model, organelle markers and imprecision. A narrative data synthesis was performed. We identified 31 studies (34 publications) of the asymmetric inheritance of organelles after mitotic or meiotic division. Studies for the asymmetric inheritance of centrosomes (n = 9); endosomes (n = 6), P granules (n = 4), the midbody (n = 3), mitochondria (n = 3), proteosomes (n = 2), spectrosomes (n = 2), cilia (n = 2) and endoplasmic reticulum (n = 2) were identified. Asymmetry was defined and quantified by variable methods. Assessment of the statistical reliability of the results indicated only two studies (7%) were judged to have low concern, the majority of studies (77%) were 'unclear' and five (16%) were judged to have 'high concerns'; the main reasons were low technical repeats (<10). Assessment of model validity indicated that the majority of studies (61%) were judged to be valid, ten studies (32%) were unclear and two studies (7%) were judged to have 'high concerns'; both described 'stem cells' without providing experimental evidence to confirm this (pluripotency and self-renewal). Assessment of marker validity indicated that no studies had low concern, most studies were unclear (96.5%), indicating there were insufficient details to judge if the markers were appropriate. One study had high concern for marker validity due to the contradictory results of two markers for the same organelle. For most studies the validity and imprecision of results could not be confirmed. In particular, data were limited due to a lack of reporting of interassay variability, sample size calculations, controls and functional validation of organelle markers. An evaluation of 16 systematic reviews containing cell assays found that only 50% reported adherence to PRISMA or ARRIVE reporting guidelines and 38% reported a formal risk of bias assessment. 44% of the reviews did not consider how relevant or valid the models were to the research question. 75% reviews did not consider how valid the markers were. 69% of reviews did not consider the impact of the statistical reliability of the results. Future systematic reviews in basic or preclinical research should ensure the rigorous reporting of the statistical reliability of the results in addition to the validity of the methods. Increased awareness of the importance of reporting guidelines and validation tools is needed for the scientific community. PMID:28562636

Advanced aeroservoelastic stabilization techniques for hypersonic flight vehicles

NASA Technical Reports Server (NTRS)

Chan, Samuel Y.; Cheng, Peter Y.; Myers, Thomas T.; Klyde, David H.; Magdaleno, Raymond E.; Mcruer, Duane T.

1992-01-01

Advanced high performance vehicles, including Single-Stage-To-Orbit (SSTO) hypersonic flight vehicles, that are statically unstable, require higher bandwidth flight control systems to compensate for the instability resulting in interactions between the flight control system, the engine/propulsion dynamics, and the low frequency structural modes. Military specifications, such as MIL-F-9490D and MIL-F-87242, tend to limit treatment of structural modes to conventional gain stabilization techniques. The conventional gain stabilization techniques, however, introduce low frequency effective time delays which can be troublesome from a flying qualities standpoint. These time delays can be alleviated by appropriate blending of gain and phase stabilization techniques (referred to as Hybrid Phase Stabilization or HPS) for the low frequency structural modes. The potential of using HPS for compensating structural mode interaction was previously explored. It was shown that effective time delay was significantly reduced with the use of HPS; however, the HPS design was seen to have greater residual response than a conventional gain stablized design. Additional work performed to advance and refine the HPS design procedure, to further develop residual response metrics as a basis for alternative structural stability specifications, and to develop strategies for validating HPS design and specification concepts in manned simulation is presented. Stabilization design sensitivity to structural uncertainties and aircraft-centered requirements are also assessed.

Medicinal cannabis: Principal cannabinoids concentration and their stability evaluated by a high performance liquid chromatography coupled to diode array and quadrupole time of flight mass spectrometry method.

PubMed

Citti, Cinzia; Ciccarella, Giuseppe; Braghiroli, Daniela; Parenti, Carlo; Vandelli, Maria Angela; Cannazza, Giuseppe

2016-09-05

In the last few years, there has been a boost in the use of cannabis-based extracts for medicinal purposes, although their preparation procedure has not been standardized but rather decided by the individual pharmacists. The present work describes the development of a simple and rapid high performance liquid chromatography method with UV detection (HPLC-UV) for the qualitative and quantitative determination of the principal cannabinoids (CBD-A, CBD, CBN, THC and THC-A) that could be applied to all cannabis-based medicinal extracts (CMEs) and easily performed by a pharmacist. In order to evaluate the identity and purity of the analytes, a high-resolution mass spectrometry (HPLC-ESI-QTOF) analysis was also carried out. Full method validation has been performed in terms of specificity, selectivity, linearity, recovery, dilution integrity and thermal stability. Moreover, the influence of the solvent (ethyl alcohol and olive oil) was evaluated on cannabinoids degradation rate. An alternative extraction method has then been proposed in order to preserve cannabis monoterpene component in final CMEs. Copyright © 2016 Elsevier B.V. All rights reserved.

Sexual compulsivity scale: adaptation and validation in the spanish population.

PubMed

Ballester-Arnal, Rafael; Gómez-Martínez, Sandra; Llario, M Dolores-Gil; Salmerón-Sánchez, Pedro

2013-01-01

Sexual compulsivity has been studied in relation to high-risk behavior for sexually transmitted infections. The aim of this study was the adaptation and validation of the Sexual Compulsivity Scale to a sample of Spanish young people. This scale was applied to 1,196 (891 female, 305 male) Spanish college students. The results of principal components factor analysis using a varimax rotation indicated a two-factor solution. The reliability of the Sexual Compulsivity Scale was found to be high. Moreover, the scale showed good temporal stability. External correlates were examined through Pearson correlations between the Sexual Compulsivity Scale and other constructs related with HIV prevention. The authors' results suggest that the Sexual Compulsivity Scale is an appropriate measure for assessing sexual compulsivity, showing adequate psychometric properties in the Spanish population.

Longitudinal Stability of Person Characteristics: Intelligence and Creativity.

ERIC Educational Resources Information Center

Magnusson, D.; Backteman, G.

1979-01-01

A longitudinal study of approximately 1,000 students aged 10-16 showed high stability of intelligence and creativity. Stability coefficients for intelligence were higher than those for creativity. Results supported the construct validity of creativity. (MH)

Advanced Lithium-ion Batteries with High Specific Energy and Improved Safety for Nasa's Missions

NASA Technical Reports Server (NTRS)

West, William; Smart, Marshall; Soler, Jess; Krause, Charlie; Hwang, Constanza; Bugga, Ratnakumar

2012-01-01

High Energy Materials ( Cathodes, anodes and high voltage and safe electrolyte are required to meet the needs of the future space missions. A. Cathodes: The layered layered composites of of Li2MnO3 and LiMO2 are promising Power capability of the materials, however requires further improvement. Suitable morphology is critical for good performance and high tap (packing) density. Surface coatings help in the interfacial kinetics and stability. B. Electrolytes: Small additions of Flame Retardant Additives improves flammability without affecting performance (Rate and cycle life). 1.0 M in EC+EMC+TPP was shown to have good performance against the high voltage cathode; Performance demonstrated in large capacity prototype MCMB- LiNiCoO2 Cells. Formulations with higher proportions are looking promising. Still requires further validation through abuse tests (e.g., on 18650 cells).

Single Laboratory Validation of a Method for Determination of Glucosamine in Raw Materials and Dietary Supplements Containing Glucosamine Sulfate and/or Glucosamine Hydrochloride by High-Performance Liquid Chromatography with FMOC-Su Derivatization

PubMed Central

Zhou, Joseph ZiQi; Waszkuc, Ted; Mohammed, Felicia

2008-01-01

Single laboratory validation of a method for determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by with high-performance liquid Chromatography FMOC-Su derivatization. Tests with 2 blank matrixes containing SAMe, vitamin C, citric acid, chondroitin sulfates, methylsulfonylmethane, lemon juice concentrate, and other potential interferents showed the method to be selective and specific. Eight calibration curves prepared over 7 working days indicated excellent reproducibility with the linear range at least over 2.0–150 μg/mL, and determination coefficients >0.9999. Average spike recovery from the blank matrix (n = 8 over 2 days) was 93.5, 99.4, and 100.4% at respective spike levels of 15,100, and 150%, and from the sample matrix containing glucosamine (n = 3) was 99.9 and 102.8% at respective levels of 10 and 40%, with relative standard deviations <0.9%. The method was also applied to 12 various glucosamine finished products and raw materials. The stability tests confirmed that glucosamine–FMOC-Su derivative once formed is stable at room temperature for at least 5 days. Limit of quantitation was 1 μg/mL and limit of detection was 0.3 μg/mL. The method is ready to proceed for the collaborative study. PMID:15493664

Analyses of soft tissue from Tyrannosaurus rex suggest the presence of protein.

PubMed

Schweitzer, Mary Higby; Suo, Zhiyong; Avci, Recep; Asara, John M; Allen, Mark A; Arce, Fernando Teran; Horner, John R

2007-04-13

We performed multiple analyses of Tyrannosaurus rex (specimen MOR 1125) fibrous cortical and medullary tissues remaining after demineralization. The results indicate that collagen I, the main organic component of bone, has been preserved in low concentrations in these tissues. The findings were independently confirmed by mass spectrometry. We propose a possible chemical pathway that may contribute to this preservation. The presence of endogenous protein in dinosaur bone may validate hypotheses about evolutionary relationships, rates, and patterns of molecular change and degradation, as well as the chemical stability of molecules over time.

Development of validated stability indicating assay method for simultaneous estimation of metformin hydrochloride and vildagliptin by RP-HPLC.

PubMed

Satheeshkumar, N; Pradeepkumar, M; Shanthikumar, S; Rao, V J

2014-03-01

A simple, precise and stability-indicating HPLC method was developed and validated for the simultaneous determination of metformin hydrochloride (MET) and vildagliptin (VLG) in pharmaceutical dosage forms. The method involves use of easily available inexpensive laboratory reagents. The separation was achieved on Grace Cyano column (250 mm×4.6 mm) 5 µm with isocratic flow. The mobile phase was pumped at a flow rate of 1.0 mL/min, consisted of 25 mM ammonium bicarbonate buffer and acetonitrile (65:35, v/v). The UV detection was carried out at 207 nm. A linear response was observed over the concentration range of 25-125 µg/mL for MET and 50-250 µg/mL for VLG respectively. Limit of detection and limit of quantification for MET were 0.36 µg/mL and 1.22 µg/mL, and for VLG were 0.75 µg/mL and 2.51 µg/mL respectively. The method was successfully validated in accordance to ICH guidelines acceptance criteria for specificity, linearity, accuracy, precision, robustness, and system suitability. Individual drugs (MET and VLG) were exposed to thermal, photolytic, hydrolytic and oxidative stress conditions. The resultant stressed samples were analyzed by the proposed method. The method gave high resolution among the degradation products and the analytes. The peak purity of analyte peak in the stressed samples was confirmed by photo diode array detector. The proposed method was successfully applied for the quantitative analysis of MET and VLG in tablet dosage form, which will help to improve quality control and contribute to stability studies of pharmaceutical tablets containing these drugs. © Georg Thieme Verlag KG Stuttgart · New York.

Development and Application of a High-Performance Liquid Chromatography Stability-Indicating Assay for Beyond-Use Date Determination of Compounded Topical Gels Containing Multiple Active Drugs.

PubMed

Gorman, Gregory; Sokom, Simara; Coward, Lori; Arnold, John J

2017-01-01

Topical gels compounded by pharmacists are important clinical tools for the management of pain. Nevertheless, there is often a dearth of information about the chemical stability of drugs included in these topical formulations, complicating the assignment of beyond-use dating. The purpose of this study was to develop a high-performance liquid chromatography photodiode array-based stability-indicating assay that could simultaneously resolve six drugs (amitriptyline, baclofen, clonidine, gabapentin, ketoprofen, lidocaine) commonly included in topical gels for pain management and their potential degradation products. Furthermore, this method was applied to the determination of beyond-use dating of combinations of these drugs prepared in commonly utilized bases (Lipobase, Lipoderm, Pluronic organogel). Gabapentin was determined to be the least stable component in all formulations tested. Measured stability ranged between 7 to 49 days depending on the base and other active drugs present in the formulation. In the absence of gabapentin, baclofen was the next least stable component, lasting for 120 days, regardless of the type of formulating base used. Copyright© by International Journal of Pharmaceutical Compounding, Inc.

Evaluation of the Stability of Mercaptopurine Suspension Compounded in a Commercial Vehicle and the Determination of an Appropriate Beyond-use Date.

PubMed

Peacock, Gina F; Sauvageot, Jurgita; Hill, Ashley; Killian, Alyssa

2016-01-01

Mercaptopurine is commonly used to treat acute lymphoblastic leukemia and has historically been commercially available only in tablet form. Since tablets may be difficult for children and elderly patients to swallow, many pharmacists have compounded mercaptopurine suspensions. The U.S. Food and Drug Administration recently approved a commercial suspension, but it is not widely available at this time. Therefore, pharmacists may still need to compound mercaptopurine suspension for use in areas where it is not available or if the commercial suspension is in short supply. Stability studies must be conducted in order to assign appropriate beyond-use dates for compounded preparations. The objective of this study was to evaluate the stability of extemporaneously compounded suspensions using commercially available mercaptopurine tablets, as well as active pharmaceutical ingredient in a vehicle of Ora-Sweet and Ora-Plus (1:1) stored in plastic and glass containers at room temperature. Each mercaptopurine preparation was analyzed using a validated stability-indicating high-performance liquid chromatography method at the following time points: 0, 7, 14, 21, 30, 60, and 90 days. Suspensions were also observed for changes in appearance or odor, and pH was tested at each time point. The suspension compounded from Roxane generic tablets was extremely viscous and was therefore eliminated from the study. All other suspensions showed no observed physical changes and maintained greater than 93% of initial concentration of mercaptopurine for the entire study period.

Development of a stability-indicating UPLC method for determining olanzapine and its associated degradation products present in active pharmaceutical ingredients and pharmaceutical dosage forms.

PubMed

Krishnaiah, Ch; Vishnu Murthy, M; Kumar, Ramesh; Mukkanti, K

2011-03-25

A simple, sensitive and reproducible ultra performance liquid chromatography (UPLC) coupled with a photodiode array detector method was developed for the quantitative determination of olanzapine (OLN) in API and pharmaceutical dosage forms. The method is applicable to the quantification of related substances and assays of drug substances. Chromatographic separation was achieved on Acquity UPLC BEH 100-mm, 2.1-mm, and 1.7-μm C-18 columns, and the gradient eluted within a short runtime, i.e., within 10.0 min. The eluted compounds were monitored at 250 nm, the flow rate was 0.3 mL/min, and the column oven temperature was maintained at 27°C. The resolution of OLN and eight (potential, bi-products and degradation) impurities was greater than 2.0 for all pairs of components. The high correlation coefficient (r(2)>0.9991) values indicated clear correlations between the investigated compound concentrations and their peak areas within the test ranges. The repeatability and intermediate precision, expressed by the RSD, were less than 2.4%. The accuracy and validity of the method were further ascertained by performing recovery studies via a spike method. The accuracy of the method expressed as relative error was satisfactory. No interference was observed from concomitant substances normally added to the tablets. The drug was subjected to the International Conference on Harmonization (ICH)-prescribed hydrolytic, oxidative, photolytic and thermal stress conditions. The performance of the method was validated according to the present ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, ruggedness and robustness. Copyright © 2010 Elsevier B.V. All rights reserved.

Relative and absolute reliability of the clinical version of the Narrow Path Walking Test (NPWT) under single and dual task conditions.

PubMed

Gimmon, Yoav; Jacob, Grinshpon; Lenoble-Hoskovec, Constanze; Büla, Christophe; Melzer, Itshak

2013-01-01

Decline in gait stability has been associated with increased fall risk in older adults. Reliable and clinically feasible methods of gait instability assessment are needed. This study evaluated the relative and absolute reliability and concurrent validity of the testing procedure of the clinical version of the Narrow Path Walking Test (NPWT) under single task (ST) and dual task (DT) conditions. Thirty independent community-dwelling older adults (65-87 years) were tested twice. Participants were instructed to walk within the 6-m narrow path without stepping out. Trial time, number of steps, trial velocity, number of step errors, and number of cognitive task errors were determined. Intraclass correlation coefficients (ICCs) were calculated as indices of agreement, and a graphic approach called "mountain plot" was applied to help interpret the direction and magnitude of disagreements between testing procedures. Smallest detectable change and smallest real difference (SRD) were computed to determine clinically relevant improvement at group and individual levels, respectively. Concurrent validity was assessed using Performance Oriented Mobility Assessment Tool (POMA) and the Short Physical Performance Battery (SPPB). Test-retest agreement (ICC1,2) varied from 0.77 to 0.92 in ST and from 0.78 to 0.92 in DT conditions, with no apparent systematic differences between testing procedures demonstrated by the mountain plot graphs. Smallest detectable change and smallest real change were small for motor task performance and larger for cognitive errors. Significant correlations were observed for trial velocity and trial time with POMA and SPPB. The present results indicate that the NPWT testing procedure is highly reliable and reproducible. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Validation and Uncertainty Estimation of an Ecofriendly and Stability-Indicating HPLC Method for Determination of Diltiazem in Pharmaceutical Preparations

PubMed Central

Sadeghi, Fahimeh; Navidpour, Latifeh; Bayat, Sima; Afshar, Minoo

2013-01-01

A green, simple, and stability-indicating RP-HPLC method was developed for the determination of diltiazem in topical preparations. The separation was based on a C18 analytical column using a mobile phase consisted of ethanol: phosphoric acid solution (pH = 2.5) (35 : 65, v/v). Column temperature was set at 50°C and quantitation was achieved with UV detection at 240 nm. In forced degradation studies, the drug was subjected to oxidation, hydrolysis, photolysis, and heat. The method was validated for specificity, selectivity, linearity, precision, accuracy, and robustness. The applied procedure was found to be linear in diltiazem concentration range of 0.5–50 μg/mL (r 2 = 0.9996). Precision was evaluated by replicate analysis in which % relative standard deviation (RSD) values for areas were found below 2.0. The recoveries obtained (99.25%–101.66%) ensured the accuracy of the developed method. The degradation products as well as the pharmaceutical excipients were well resolved from the pure drug. The expanded uncertainty (5.63%) of the method was also estimated from method validation data. Accordingly, the proposed validated and sustainable procedure was proved to be suitable for routine analyzing and stability studies of diltiazem in pharmaceutical preparations. PMID:24163778

Investigating the potential of Bacillus subtilis alpha-amylase as a pressure-temperature-time indicator for high hydrostatic pressure pasteurization processes.

PubMed

Grauwet, Tara; Van der Plancken, Iesel; Vervoort, Liesbeth; Hendrickx, Marc E; Van Loey, Ann

2009-01-01

The potential of Bacillus subtilis alpha-amylase (BSA) as a pressure-temperature-time indicator (pTTI) for high pressure pasteurization processing (400-600 MPa; T(i) 10-40 degrees C; 1-15 min) was investigated. A stepwise approach was followed for the development of an enzyme-based, extrinsic, isolated pTTI. First, based on literature data on the pressure stability, BSA was selected as a candidate indicator. Next to the accuracy and ease of the measurement of the indicator's response (residual activity) to the pressure treatment, the storage and handling stability of BSA at atmospheric pressure was verified. Second, the stability of BSA at a constant temperature (T) and time in function of pressure (p) was investigated. Solvent engineering was used to shift the inactivation window of BSA in the processing range of interest. Third, the enzyme (1 g/L BSA-MES 0.05 M pH 5.0) was kinetically calibrated under isobaric-isothermal conditions. Time dependent changes in activity could be modeled best by a first-order model. Except for low pressures and high temperatures, a synergistic effect between pressure and temperature could be observed. Based on the model selected to describe the combined p,T-dependency of the inactivation rate constant, an elliptically shaped isorate contour plot could be constructed, illustrating the processing range where BSA can be used to demonstrate temperature gradients. Fourth, the validity of the kinetic model was tested successfully under dynamic conditions similar to those used in food industry. Finally, the indicator was found suitable to demonstrate nonuniformity in two-sectional planes of a vertical, single vessel system. (c) 2009 American Institute of Chemical Engineers. Biotechnol. Prog., 2009.

Stability-Indicating HPTLC Method for Studying Stress Degradation Behavior of Sulbutiamine HCl

PubMed Central

Farid, Nehal F.; Abdelwahab, Nada S.

2016-01-01

Sulbutiamine (SUL) is an ester of thiazides with neurotropic action. A new stability indicating HPTLC method has been developed and validated for the determination of SUL in the presence of different degradation products. The drug was subjected to different stress conditions following ICH strategy such as hydrolytic degradation (neutral, alkaline and acidic hydrolysis), oxidation, photodegradation and dry heat degradation. The drug demonstrated degradation under all decomposition conditions except neutral hydrolysis and dry heat, where the drug was completely degraded with 0.1 N NaOH, 1 N HCl and 30% H2O2 while it was partially degradaed by 0.1 N HCl, 3% H2O2 and UV light. Structure elucidation of the resulting degradation products was performed using ESI-Q-MS–MS. A well-defined peak for SUL was obtained at Rf = 0.46 and was completely separated from all obtained degradation products. Chromatographic separation was carried out on HPTLC aluminum plates precoated with silica gel 60 F254 using acetone–methylene chloride–ammonia buffer (pH 8.5 ± 0.2) (7:3:0.5, v/v) as a developing system. Densitometric scanning of the separated peaks was performed at 254 nm. System suitability testing parameters were calculated to ascertain the quality performance of the developed method. The method was validated with respect to USP guidelines regarding accuracy, precision, specificity, robustness and ruggedness. Good correlation coefficients were achieved in the range of 0.4–5.0 µg/band, and the limit of detection and limit of quantitation were found to be 0.11 and 0.33 µg/band, respectively. The utility of the suggested method was verified by application to Arcalion forte® tablets where no interference from additives was found. PMID:26759487

[Multicenter validation of an evaluation tool for clinical training activities (SVAT) of the nursing students].

PubMed

Finotto, Sergio; Gradellini, Cinzia; Bandini, Stefania; Burrai, Francesco; Lucchi Casadei, Sandra; Villani, Carolina; Vincenzi, Simone; Mecugni, Daniela

2017-01-01

To evaluate the psychometric characteristics of the Scheda di Valutazione delle Attività di Tirocinio (SVAT). The degree courses in Nursing of the University of Modena and Reggio Emilia, site of Reggio Emilia, the University of Bologna Formative Section BO1, Imola and training center of Cesena, the University of Ferrara training centers of Ferrara and Codigoro were all enrolled in the research. For the content validation the reactive Delphi method was chosen. The panel of experts expressed a qualitative-intuitive judgment on the adequacy of language and on the stimulus material (SVAT). For internal consistency Cronbach's alpha was calculated the. The test-retest method was used for the reliability of stability. all indicators of the SVAT have achieved a degree of consensus not less than 80% demonstrating its content validity. The face validity is demonstrated by an average score equal to or greater than 7 obtained by all indicators. The reliability of internal consistency of the SVAT was appraised by Cronbach's alpha that was 0.987 for the entire instrument. The reliability of the stability has been calculated through the correlation's coefficient expressed by Pearson's r that was 0.983 (p = 1.3E-198). in Italy there is no a "gold standard" tool to evaluate the clinical performance of nursing students during and at the end of their clinical training. The SVAT proves to be a valuable and reliable tool it furthermore could stimulate the discussion and the debate among educators and nurses, so that also in our country, it may be possible develop and refine tools that support the evaluation of clinical skills of nursing students.

Validity and test-retest reliability of an at-work production loss instrument.

PubMed

Aboagye, E; Jensen, I; Bergström, G; Hagberg, J; Axén, I; Lohela-Karlsson, M

2016-07-01

Besides causing ill health, a poor work environment may contribute to production loss. Production loss assessment instruments emphasize health-related consequences but there is no instrument to measure reduced work performance related to the work environment. To examine convergent validity and test-retest reliability of health-related production loss (HRPL) and work environment-related production loss (WRPL) against a valid comparable instrument, the Health and Work Performance Questionnaire (HPQ). Cross-sectional study of employees, not on sick leave, who were asked to self-rate their work performance and production losses. Using the Pearson correlation and Bland and Altman's Test of Agreement, convergent validity was examined. Subgroup analyses were performed for employees recording problem-specific reduced work performance. Consistency of pairs of HRPL and WRPL for samples responding to both assessments was expressed using Intraclass Correlation Coefficient (ICC) and tests of repeatability. A total of 88 employees participated and 44 responded to both assessments. Test of agreement between measurements estimates a mean difference of 0.34 for HRPL and -0.03 for WRPL compared with work performance. This indicates that the production loss questions are valid and moderately associated with work performance for the total sample and subgroups. ICC for paired HRPL assessments was 0.90 and 0.91 for WRPL, i.e. the test-retest reliability was good and suggests stability in the instrument. HRPL and WRPL can be used to measure production loss due to health-related and work environment-related problems. These results may have implications for advancing methods of assessing production loss, which represents an important cost to employers. © The Author 2016. Published by Oxford University Press on behalf of the Society of Occupational Medicine. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Stability-indicating UPLC method for determination of Valsartan and their degradation products in active pharmaceutical ingredient and pharmaceutical dosage forms.

PubMed

Krishnaiah, Ch; Reddy, A Raghupathi; Kumar, Ramesh; Mukkanti, K

2010-11-02

A simple, precise, accurate stability-indicating gradient reverse phase ultra-performance liquid chromatographic (RP-UPLC) method was developed for the quantitative determination of purity of Valsartan drug substance and drug products in bulk samples and pharmaceutical dosage forms in the presence of its impurities and degradation products. The method was developed using Waters Aquity BEH C18 (100 mm x 2.1 mm, 1.7 microm) column with mobile phase containing a gradient mixture of solvents A and B. The eluted compounds were monitored at 225 nm, the run time was within 9.5 min, which Valsartan and its seven impurities were well separated. Valsartan was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Valsartan was found to degrade significantly in acid and oxidative stress conditions and stable in base, hydrolytic and photolytic degradation conditions. The degradation products were well resolved from main peak and its impurities, proving the stability-indicating power of the method. The developed method was validated as per international conference on harmonization (ICH) guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness. This method was also suitable for the assay determination of Valsartan in pharmaceutical dosage forms.

Using Lunar Observations to Validate In-Flight Calibrations of Clouds and Earth Radiant Energy System Instruments

NASA Technical Reports Server (NTRS)

Daniels, Janet L.; Smith, G. Louis; Priestley, Kory J.; Thomas, Susan

2014-01-01

The validation of in-orbit instrument performance requires stability in both instrument and calibration source. This paper describes a method of validation using lunar observations scanning near full moon by the Clouds and Earth Radiant Energy System (CERES) instruments. Unlike internal calibrations, the Moon offers an external source whose signal variance is predictable and non-degrading. From 2006 to present, in-orbit observations have become standardized and compiled for the Flight Models-1 and -2 aboard the Terra satellite, for Flight Models-3 and -4 aboard the Aqua satellite, and beginning 2012, for Flight Model-5 aboard Suomi-NPP. Instrument performance parameters which can be gleaned are detector gain, pointing accuracy and static detector point response function validation. Lunar observations are used to examine the stability of all three detectors on each of these instruments from 2006 to present. This validation method has yielded results showing trends per CERES data channel of 1.2% per decade or less.

Validity of the Nintendo Wii® balance board for the assessment of standing balance in Parkinson's disease.

PubMed

Holmes, Jeffrey D; Jenkins, Mary E; Johnson, Andrew M; Hunt, Michael A; Clark, Ross A

2013-04-01

Impaired postural stability places individuals with Parkinson's at an increased risk for falls. Given the high incidence of fall-related injuries within this population, ongoing assessment of postural stability is important. To evaluate the validity of the Nintendo Wii(®) balance board as a measurement tool for the assessment of postural stability in individuals with Parkinson's. Twenty individuals with Parkinson's participated. Subjects completed testing on two balance tasks with eyes open and closed on a Wii(®) balance board and biomechanical force platform. Bland-Altman plots and a two-way, random-effects, single measure intraclass correlation coefficient model were used to assess concurrent validity of centre-of-pressure data. Concurrent validity was demonstrated to be excellent across balance tasks (intraclass correlation coefficients = 0.96, 0.98, 0.92, 0.94). This study suggests that the Wii(®) balance board is a valid tool for the quantification of postural stability among individuals with Parkinson's.

Stability-Indicating Reversed-Phase UHPLC Method Development and Characterization of Degradation Products of Almotriptan Maleate by LC-QTOF-MS/MS.

PubMed

Saibaba, B; Vishnuvardhan, Ch; Johnsi Rani, P; Satheesh Kumar, N

2018-01-01

Almotriptan maleate (ALMT), a highly selective 5-hydroxy tryptamine 1B/1D (5-HT1B/1D) receptor agonist used in the treatment of migraine headache was subjected to various ICH (Q1A (R2)) specified guidelines. The drug underwent significant degradation under hydrolytic (acid, base and neutral), oxidative and photolytic stress conditions, while it was stable under thermal stress condition. A total of seven significant degradation products (DPs) were obtained. A simple, selective and reliable UPLC method has been developed for the separation of ALMT and its DPs using Acquity UPLC HSS Cyano (100 × 2.1 mm, 1.8 μm) column with mobile phase consisting of ammonium acetate (10 mM, pH 4.4) buffer and acetonitrile in gradient elution mode. Chromatographic analysis was performed at a flow rate of 0.3 mL/min using a PDA detector at a wavelength of 230 nm. All the DPs (DP-1 to DP-7) were characterized using UHPLC-ESI-QTOF based on mass fragmentation pattern and accurate m/z values. The developed UPLC method was validated in terms of specificity, linearity, precision and accuracy. The developed stability-indicating method helps in quantification of drug in the presence of DPs. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A Rapid Novel HPLC Method for Estimation of Eight Related Compounds in Azilsartan Kamedoxomil and Identification of Degradation Compounds by Using LC-MS.

PubMed

Sreenivasulu, J; Venkata Ramana, P; Sampath Kumar Reddy, G; Nagaraju, Ch V S; Thirumalai Rajan, S; Eswaraiah, S

2015-10-01

A novel, rapid, specific and stability-indicating reverse-phase high-performance liquid chromatography method was developed for the quantitative determination of related compounds, obtained from two different synthetic routes and degradation products of Azilsartan kamedoxomil (AZL). The method was developed by using a YMC-Pack pro C18 (150 × 4.6 mm, 3 µm) column with a mobile phase containing a gradient mobile phase combination. The eluted compounds were measured at wavelength 220 nm. The developed method run time was 25 min, within which AZL and its eight impurities were well separated with minimum 3.0 resolution. The drug substance was subjected to stress conditions of hydrolysis (acid, base and water), oxidation, photolysis, sunlight, 75% relative humidity and thermal degradation as per International Conference on Harmonization (ICH) prescribed stress conditions to ascertain the stability-indicating power of the method. Significant degradation was observed during acid, base, peroxide, water hydrolysis and 75% relative humidity studies. The mass balance of AZL was close to 100% in all the stress condition. The developed method was validated as per the ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Longitudinal data analysis in support of functional stability concepts for leachate management at closed municipal landfills.

PubMed

Gibbons, Robert D; Morris, Jeremy W F; Prucha, Christopher P; Caldwell, Michael D; Staley, Bryan F

2014-09-01

Landfill functional stability provides a target that supports no environmental threat at the relevant point of exposure in the absence of active control systems. With respect to leachate management, this study investigates "gateway" indicators for functional stability in terms of the predictability of leachate characteristics, and thus potential threat to water quality posed by leachate emissions. Historical studies conducted on changes in municipal solid waste (MSW) leachate concentrations over time (longitudinal analysis) have concentrated on indicator compounds, primarily chemical oxygen demand (COD) and biochemical oxygen demand (BOD). However, validation of these studies using an expanded database and larger constituent sets has not been performed. This study evaluated leachate data using a mixed-effects regression model to determine the extent to which leachate constituent degradation can be predicted based on waste age or operational practices. The final dataset analyzed consisted of a total of 1402 samples from 101 MSW landfills. Results from the study indicated that all leachate constituents exhibit a decreasing trend with time in the post-closure period, with 16 of the 25 target analytes and aggregate classes exhibiting a statistically significant trend consistent with well-studied indicators such as BOD. Decreasing trends in BOD concentration after landfill closure can thus be considered representative of trends for many leachate constituents of concern. Copyright © 2014 Elsevier Ltd. All rights reserved.

Investigation of folic acid stability in fortified instant noodles by use of capillary electrophoresis and reversed-phase high performance liquid chromatography.

PubMed

Hau Fung Cheung, Rodney; Morrison, Paul D; Small, Darryl M; Marriott, Philip J

2008-12-05

A single enzyme treatment with alpha-amylase, prior to the quantification of added folic acid (FA) in fortified instant fried Asian noodles with analysis performed by capillary zone electrophoresis (CZE) and reversed-phase high performance liquid chromatography (RP-HPLC) with UV detection, is described. The method was validated and optimized for capillary electrophoresis (CE) with separation achieved using a 8 mM phosphate-12 mM borate run buffer with 5% MeOH at pH 9.5. FA was well separated from matrix components with nicotinic acid (NA) employed as an internal standard. In a comparative study, separation of FA was performed using HPLC with a mobile phase consisting of 27% MeOH (v/v) in aqueous potassium phosphate buffer (3.5 mM KH(2)PO(4) and 3.2 mM K(2)HPO(4)), pH 8.5, and containing 5 mM tetrabutylammonium dihydrogen phosphate as an ion-pairing agent. For both methods, excellent results were obtained for various analytical parameters including linearity, accuracy and precision. The limit of detection was calculated to be 2.2 mg/L for CE without sample stacking and 0.10 mg/L with high performance liquid chromatography (HPLC). Sample extraction involved homogenization and enzymatic extraction with alpha-amylase. Results indicated that FA was stable during four main stages of instant fried noodle manufacturing (dough crumbs, cut sheets, steaming and frying).

Stability of the guinea pigs personality - cognition - linkage over time.

PubMed

Brust, Vera; Guenther, Anja

2017-01-01

In human psychological research, personality traits as well as cognitive traits are usually validated for both, their stability over time and contexts. While stability over time gives an estimate on how genetically fixated a trait can be, correlations across traits have the power to reveal linkages or trade - offs. In animals, these validations have widely been done for personality but not for cognitive traits. We tested guinea pigs in four consecutive discrimination tasks using four unique pairs of objects with two objects of the same form but different size in each pair. The same animals were tested twice each for three personality traits, i.e. boldness, aggression and sociopositive behaviour. The animals did not learn to "always choose the larger item" in the cognitive task but learned to discriminate the two objects of each stimulus pair anew, so that we did test for learning speed in four slightly different task setups. Performance over the four tasks was significantly repeatable as well as all tested personality traits. A stable linkage over time was found between sociopositive behaviour and learning performance, probably indicating an ecological relevance for a correlation between these two traits. Still, not all traits seem to be connected amongst each other, as in our case boldness and aggression are both not linked to individual learning performance. Future studies will hopefully further investigate the repeatability of various cognitive traits in several species and thus lead to a better understanding of the interdependence of personality and cognition. This will help to unravel which suites of traits facilitate individual life histories and hence improve our understanding of the emergence and maintenance of individual differences. Copyright © 2016 Elsevier B.V. All rights reserved.

Clinical validation of the nursing diagnosis of dysfunctional family processes related to alcoholism.

PubMed

Mangueira, Suzana de Oliveira; Lopes, Marcos Venícios de Oliveira

2016-10-01

To evaluate the clinical validity indicators for the nursing diagnosis of dysfunctional family processes related to alcohol abuse. Alcoholism is a chronic disease that negatively affects family relationships. Studies on the nursing diagnosis of dysfunctional family processes are scarce in the literature. This diagnosis is currently composed of 115 defining characteristics, hindering their use in practice and highlighting the need for clinical validation. This was a diagnostic accuracy study. A sample of 110 alcoholics admitted to a reference centre for alcohol treatment was assessed during the second half of 2013 for the presence or absence of the defining characteristics of the diagnosis. Operational definitions were created for each defining characteristic based on concept analysis and experts evaluated the content of these definitions. Diagnostic accuracy measures were calculated from latent class models with random effects. All 89 clinical indicators were found in the sample and a set of 24 clinical indicators was identified as clinically valid for a diagnostic screening for family dysfunction from the report of alcoholics. Main clinical indicators with high specificity included sexual abuse, disturbance in academic performance in children and manipulation. The main indicators that showed high sensitivity values were distress, loss, anxiety, low self-esteem, confusion, embarrassment, insecurity, anger, loneliness, deterioration in family relationships and disturbance in family dynamics. Eighteen clinical indicators showed a high capacity for diagnostic screening for alcoholics (high sensitivity) and six indicators can be used for confirmatory diagnosis (high specificity). © 2016 John Wiley & Sons Ltd.

Improved image reconstruction of low-resolution multichannel phase contrast angiography

PubMed Central

P. Krishnan, Akshara; Joy, Ajin; Paul, Joseph Suresh

2016-01-01

Abstract. In low-resolution phase contrast magnetic resonance angiography, the maximum intensity projected channel images will be blurred with consequent loss of vascular details. The channel images are enhanced using a stabilized deblurring filter, applied to each channel prior to combining the individual channel images. The stabilized deblurring is obtained by the addition of a nonlocal regularization term to the reverse heat equation, referred to as nonlocally stabilized reverse diffusion filter. Unlike reverse diffusion filter, which is highly unstable and blows up noise, nonlocal stabilization enhances intensity projected parallel images uniformly. Application to multichannel vessel enhancement is illustrated using both volunteer data and simulated multichannel angiograms. Robustness of the filter applied to volunteer datasets is shown using statistically validated improvement in flow quantification. Improved performance in terms of preserving vascular structures and phased array reconstruction in both simulated and real data is demonstrated using structureness measure and contrast ratio. PMID:26835501

The Rosenberg Self-Esteem Scale: translation and validation in university students.

PubMed

Martín-Albo, José; Núñiez, Juan L; Navarro, José G; Grijalvo, Fernando

2007-11-01

The aim of this study was to translate into Spanish and to validate the Rosenberg Self-Esteem Scale (RSES), completed by 420 university students. Confirmatory factor analysis revealed that the model that best fit the data, both in the total sample and in the male and female subsamples, was the one-factor structure with method effects associated with positively worded items. The results indicated high, positive correlations between self-esteem and the five dimensions of self-concept. The scale showed satisfactory levels of internal consistency and temporal stability over a four-week period. Lastly, gender differences were obtained. These findings support the use of the RSES for the assessment of self-esteem in higher education.

miR-16-5p Is a Stably-Expressed Housekeeping MicroRNA in Breast Cancer Tissues from Primary Tumors and from Metastatic Sites

PubMed Central

Rinnerthaler, Gabriel; Hackl, Hubert; Gampenrieder, Simon Peter; Hamacher, Frank; Hufnagl, Clemens; Hauser-Kronberger, Cornelia; Zehentmayr, Franz; Fastner, Gerd; Sedlmayer, Felix; Mlineritsch, Brigitte; Greil, Richard

2016-01-01

For quantitative microRNA analyses in formalin-fixed paraffin-embedded (FFPE) tissue, expression levels have to be normalized to endogenous controls. To investigate the most stably-expressed microRNAs in breast cancer and its surrounding tissue, we used tumor samples from primary tumors and from metastatic sites. MiRNA profiling using TaqMan® Array Human MicroRNA Cards, enabling quantification of 754 unique human miRNAs, was performed in FFPE specimens from 58 patients with metastatic breast cancer. Forty-two (72%) samples were collected from primary tumors and 16 (28%) from metastases. In a cross-platform analysis of a validation cohort of 32 FFPE samples from patients with early breast cancer genome-wide microRNA expression analysis using SurePrintG3 miRNA (8 × 60 K)® microarrays from Agilent® was performed. Eleven microRNAs could be detected in all samples analyzed. Based on NormFinder and geNorm stability values and the high correlation (rho ≥ 0.8) with the median of all measured microRNAs, miR-16-5p, miR-29a-3p, miR-126-3p, and miR-222-3p are suitable single gene housekeeper candidates. In the cross-platform validation, 29 human microRNAs were strongly expressed (mean log2-intensity > 10) and 21 of these microRNAs including miR-16-5p and miR-29a-3p were also stably expressed (CV < 5%). Thus, miR-16-5p and miR-29a-3p are both strong housekeeper candidates. Their Normfinder stability values calculated across the primary tumor and metastases subgroup indicate that miR-29a-3p can be considered as the strongest housekeeper in a cohort with mainly samples from primary tumors, whereas miR-16-5p might perform better in a metastatic sample enriched cohort. PMID:26821018

miR-16-5p Is a Stably-Expressed Housekeeping MicroRNA in Breast Cancer Tissues from Primary Tumors and from Metastatic Sites.

PubMed

Rinnerthaler, Gabriel; Hackl, Hubert; Gampenrieder, Simon Peter; Hamacher, Frank; Hufnagl, Clemens; Hauser-Kronberger, Cornelia; Zehentmayr, Franz; Fastner, Gerd; Sedlmayer, Felix; Mlineritsch, Brigitte; Greil, Richard

2016-01-26

For quantitative microRNA analyses in formalin-fixed paraffin-embedded (FFPE) tissue, expression levels have to be normalized to endogenous controls. To investigate the most stably-expressed microRNAs in breast cancer and its surrounding tissue, we used tumor samples from primary tumors and from metastatic sites. MiRNA profiling using TaqMan(®) Array Human MicroRNA Cards, enabling quantification of 754 unique human miRNAs, was performed in FFPE specimens from 58 patients with metastatic breast cancer. Forty-two (72%) samples were collected from primary tumors and 16 (28%) from metastases. In a cross-platform analysis of a validation cohort of 32 FFPE samples from patients with early breast cancer genome-wide microRNA expression analysis using SurePrintG3 miRNA (8 × 60 K)(®) microarrays from Agilent(®) was performed. Eleven microRNAs could be detected in all samples analyzed. Based on NormFinder and geNorm stability values and the high correlation (rho ≥ 0.8) with the median of all measured microRNAs, miR-16-5p, miR-29a-3p, miR-126-3p, and miR-222-3p are suitable single gene housekeeper candidates. In the cross-platform validation, 29 human microRNAs were strongly expressed (mean log2-intensity > 10) and 21 of these microRNAs including miR-16-5p and miR-29a-3p were also stably expressed (CV < 5%). Thus, miR-16-5p and miR-29a-3p are both strong housekeeper candidates. Their Normfinder stability values calculated across the primary tumor and metastases subgroup indicate that miR-29a-3p can be considered as the strongest housekeeper in a cohort with mainly samples from primary tumors, whereas miR-16-5p might perform better in a metastatic sample enriched cohort.

Electrochemically fabricated polypyrrole-cobalt-oxygen coordination complex as high-performance lithium-storage materials.

PubMed

Guo, Bingkun; Kong, Qingyu; Zhu, Ying; Mao, Ya; Wang, Zhaoxiang; Wan, Meixiang; Chen, Liquan

2011-12-23

Current lithium-ion battery (LIB) technologies are all based on inorganic electrode materials, though organic materials have been used as electrodes for years. Disadvantages such as limited thermal stability and low specific capacity hinder their applications. On the other hand, the transition metal oxides that provide high lithium-storage capacity by way of electrochemical conversion reaction suffer from poor cycling stability. Here we report a novel high-performance, organic, lithium-storage material, a polypyrrole-cobalt-oxygen (PPy-Co-O) coordination complex, with high lithium-storage capacity and excellent cycling stability. Extended X-ray absorption fine structure and Raman spectroscopy and other physical and electrochemical characterizations demonstrate that this coordination complex can be electrochemically fabricated by cycling PPy-coated Co(3)O(4) between 0.0 V and 3.0 V versus Li(+)/Li. Density functional theory (DFT) calculations indicate that each cobalt atom coordinates with two nitrogen atoms within the PPy-Co coordination layer and the layers are connected with oxygen atoms between them. Coordination weakens the C-H bonds on PPy and makes the complex a novel lithium-storage material with high capacity and high cycling stability. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Systematic Review of Clinical Functional Outcomes After Medial Stabilized Versus Non-Medial Stabilized Total Knee Joint Replacement

PubMed Central

Young, Tony; Dowsey, Michelle M.; Pandy, Marcus; Choong, Peter F.

2018-01-01

Background Medial stabilized total knee joint replacement (TKJR) construct is designed to closely replicate the kinematics of the knee. Little is known regarding comparison of clinical functional outcomes of patients utilising validated patient reported outcome measures (PROM) after medial stabilized TKJR and other construct designs. Purpose To perform a systematic review of the available literature related to the assessment of clinical functional outcomes following a TKJR employing a medial stabilized construct design. Methods The review was performed with a Preferred Reporting Items for Systematic Review and Meta-Analyses (PRISMA) algorithm. The literature search was performed using variouscombinations of keywords. The statistical analysis was completed using Review Manager (RevMan), Version 5.3. Results In the nineteen unique studies identified, there were 2,448 medial stabilized TKJRs implanted in 2,195 participants, there were 1,777 TKJRs with non-medial stabilized design constructs implanted in 1,734 subjects. The final mean Knee Society Score (KSS) value in the medial stabilized group was 89.92 compared to 90.76 in the non-medial stabilized group, with the final KSS mean value difference between the two groups was statistically significant and favored the non-medial stabilized group (SMD 0.21; 95% CI: 0.01 to 0.41; p = 004). The mean difference in the final WOMAC values between the two groups was also statistically significant and favored the medial stabilized group (SMD: −0.27; 95% CI: −0.47 to −0.07; p = 0.009). Moderate to high values (I2) of heterogeneity were observed during the statistical comparison of these functional outcomes. Conclusion Based on the small number of studies with appropriate statistical analysis, we are unable to reach a clear conclusion in the clinical performance of medial stabilized knee replacement construct. Level of Evidence Level II PMID:29696144

A Systematic Review of Clinical Functional Outcomes After Medial Stabilized Versus Non-Medial Stabilized Total Knee Joint Replacement.

PubMed

Young, Tony; Dowsey, Michelle M; Pandy, Marcus; Choong, Peter F

2018-01-01

Medial stabilized total knee joint replacement (TKJR) construct is designed to closely replicate the kinematics of the knee. Little is known regarding comparison of clinical functional outcomes of patients utilising validated patient reported outcome measures (PROM) after medial stabilized TKJR and other construct designs. To perform a systematic review of the available literature related to the assessment of clinical functional outcomes following a TKJR employing a medial stabilized construct design. The review was performed with a Preferred Reporting Items for Systematic Review and Meta-Analyses (PRISMA) algorithm. The literature search was performed using variouscombinations of keywords. The statistical analysis was completed using Review Manager (RevMan), Version 5.3. In the nineteen unique studies identified, there were 2,448 medial stabilized TKJRs implanted in 2,195 participants, there were 1,777 TKJRs with non-medial stabilized design constructs implanted in 1,734 subjects. The final mean Knee Society Score (KSS) value in the medial stabilized group was 89.92 compared to 90.76 in the non-medial stabilized group, with the final KSS mean value difference between the two groups was statistically significant and favored the non-medial stabilized group (SMD 0.21; 95% CI: 0.01 to 0.41; p = 004). The mean difference in the final WOMAC values between the two groups was also statistically significant and favored the medial stabilized group (SMD: -0.27; 95% CI: -0.47 to -0.07; p = 0.009). Moderate to high values ( I 2 ) of heterogeneity were observed during the statistical comparison of these functional outcomes. Based on the small number of studies with appropriate statistical analysis, we are unable to reach a clear conclusion in the clinical performance of medial stabilized knee replacement construct. Level II.

Analyses of a heterogeneous lattice hydrodynamic model with low and high-sensitivity vehicles

NASA Astrophysics Data System (ADS)

Kaur, Ramanpreet; Sharma, Sapna

2018-06-01

Basic lattice model is extended to study the heterogeneous traffic by considering the optimal current difference effect on a unidirectional single lane highway. Heterogeneous traffic consisting of low- and high-sensitivity vehicles is modeled and their impact on stability of mixed traffic flow has been examined through linear stability analysis. The stability of flow is investigated in five distinct regions of the neutral stability diagram corresponding to the amount of higher sensitivity vehicles present on road. In order to investigate the propagating behavior of density waves non linear analysis is performed and near the critical point, the kink antikink soliton is obtained by driving mKdV equation. The effect of fraction parameter corresponding to high sensitivity vehicles is investigated and the results indicates that the stability rise up due to the fraction parameter. The theoretical findings are verified via direct numerical simulation.

Stability-indicating HPLC-DAD methods for determination of two binary mixtures: Rabeprazole sodium-mosapride citrate and rabeprazole sodium-itopride hydrochloride.

PubMed

El-Fatatry, Hamed M; Mabrouk, Mokhtar M; Hewala, Ismail I; Emam, Ehab H

2014-08-01

Two selective stability-indicating HPLC methods are described for determination of rabeprazole sodium (RZ)-mosapride citrate (MR) and RZ-itopride hydrochloride (IO) mixtures in the presence of their ICH-stress formed degradation products. Separations were achieved on X-Bridge C18 column using two mobile phases: the first for RZ-MR mixture consisted of acetonitrile: 0.025 M KH 2 PO 4 solution: TEA (30:69:1 v/v; pH 7.0); the second for RZ-IO mixture was at ratio of 25:74:1 (v/v; pH 9.25). The detection wavelength was 283 nm. The two methods were validated and validation acceptance criteria were met in all cases. Peak purity testing using contrast angle theory, relative absorbance and log  A versus the wavelengths plots were presented. The % recoveries of the intact drugs were between 99.1% and 102.2% with RSD% values less than 1.6%. Application of the proposed HPLC methods indicated that the methods could be adopted to follow the stability of their formulations.

Development and validation of a mass casualty conceptual model.

PubMed

Culley, Joan M; Effken, Judith A

2010-03-01

To develop and validate a conceptual model that provides a framework for the development and evaluation of information systems for mass casualty events. The model was designed based on extant literature and existing theoretical models. A purposeful sample of 18 experts validated the model. Open-ended questions, as well as a 7-point Likert scale, were used to measure expert consensus on the importance of each construct and its relationship in the model and the usefulness of the model to future research. Computer-mediated applications were used to facilitate a modified Delphi technique through which a panel of experts provided validation for the conceptual model. Rounds of questions continued until consensus was reached, as measured by an interquartile range (no more than 1 scale point for each item); stability (change in the distribution of responses less than 15% between rounds); and percent agreement (70% or greater) for indicator questions. Two rounds of the Delphi process were needed to satisfy the criteria for consensus or stability related to the constructs, relationships, and indicators in the model. The panel reached consensus or sufficient stability to retain all 10 constructs, 9 relationships, and 39 of 44 indicators. Experts viewed the model as useful (mean of 5.3 on a 7-point scale). Validation of the model provides the first step in understanding the context in which mass casualty events take place and identifying variables that impact outcomes of care. This study provides a foundation for understanding the complexity of mass casualty care, the roles that nurses play in mass casualty events, and factors that must be considered in designing and evaluating information-communication systems to support effective triage under these conditions.

Simultaneous selection for cowpea (Vigna unguiculata L.) genotypes with adaptability and yield stability using mixed models.

PubMed

Torres, F E; Teodoro, P E; Rodrigues, E V; Santos, A; Corrêa, A M; Ceccon, G

2016-04-29

The aim of this study was to select erect cowpea (Vigna unguiculata L.) genotypes simultaneously for high adaptability, stability, and yield grain in Mato Grosso do Sul, Brazil using mixed models. We conducted six trials of different cowpea genotypes in 2005 and 2006 in Aquidauana, Chapadão do Sul, Dourados, and Primavera do Leste. The experimental design was randomized complete blocks with four replications and 20 genotypes. Genetic parameters were estimated by restricted maximum likelihood/best linear unbiased prediction, and selection was based on the harmonic mean of the relative performance of genetic values method using three strategies: selection based on the predicted breeding value, having considered the performance mean of the genotypes in all environments (no interaction effect); the performance in each environment (with an interaction effect); and the simultaneous selection for grain yield, stability, and adaptability. The MNC99542F-5 and MNC99-537F-4 genotypes could be grown in various environments, as they exhibited high grain yield, adaptability, and stability. The average heritability of the genotypes was moderate to high and the selective accuracy was 82%, indicating an excellent potential for selection.

Validity and reliability assessment of the Brazilian version of the game addiction scale (GAS).

PubMed

Lemos, Igor Lins; Cardoso, Adriana; Sougey, Everton Botelho

2016-05-01

The uncontrolled use of video games can be addictive. The Game Addiction Scale (GAS) is an instrument that was developed to assess this type of addiction. The GAS consists of 21 items that are divided into the following seven factors: salience, tolerance, mood modification, relapse, withdrawal, conflict and problems. This study assessed the convergent validity and reliability of the GAS according to measures of internal consistency and test-retest stability. Three hundred and eighty four students completed the GAS, the Internet Addiction Test (IAT), the Liebowitz Social Anxiety Scale (LSAS), the Beck Depression Inventory (BDI) and the Video Game Addiction Test (VAT). A subgroup of the participants (n=76) completed the GAS again after 30days to determine test-retest stability. The GAS demonstrated excellent internal consistency (Cronbach's alpha=0.92), was highly correlated with the VAT (r=0.883) and was moderately correlated with the BDI (r=0.358), the LSAS (r=0.326) and the IAT (r=0.454). In the Brazilian Portuguese population, the GAS shows good internal consistency. These data indicate that the GAS can be used to assess video game addiction due to its demonstrated psychometric validity. Copyright © 2016 Elsevier Inc. All rights reserved.

Stability of minoxidil in Espumil foam base.

PubMed

Geiger, Christine M; Sorenson, Bridget; Whaley, Paul A

2013-01-01

Minoxidil is a drug used to stimulate hair growth and to slow balding. It is marketed under a number of trade names, including Rogaine, and is available in varying strength dose forms from a number of generic manufacturers. Minoxidil is available in oral and topical forms. In topical form, it can be applied by a metered-spray or rub-on applicator. A hydroalcoholic compounding vehicle can minimize greasiness, itching, burning, and contact dermatitis where low concentrations of ethanol and propylene glycol are present. Espumil Foam Base contains low concentrations of these ingredients and also can form a foam on topical application. Espumil's unique delivery by foam-activating packaging assures simple application to difficult-to-treat areas, and it vanishes quickly after application, keeping it in place and avoiding health skin areas. The objective of this study was to determine the stability of minoxidil in Espumil Foam Base. The studied sample was compounded into a 50-mg/mL solution and stored in a plastic foam-activating bottle at room temperature conditions. Three samples were assayed at each time point out to 90 days by a stability-indicating high-performance liquid chromatography method. The method was validated for its specificity through forced-degradation studies. The beyond-use-date is at least 90 days, based on data collected when this formulation was stored at room temperature, protected from light.

Development and validation of a stability-indicating HPLC-UV method for the determination of triamcinolone acetonide and its degradation products in an ointment formulation.

PubMed

van Heugten, A J P; de Boer, W; de Vries, W S; Markesteijn, C M A; Vromans, H

2018-02-05

A stability indicating high performance liquid chromatography method has been developed for the determination of triamcinolone acetonide (TCA) and its main degradation products in ointment formulations. The method, based on extensive stress testing using metal salts, azobisisobutyronitrile, acid, base and peroxide, showed that TCA undergoes oxidative degradation. All degradation products were identified using HPLC mass spectrometry. Separation and quantification was achieved using an Altima C18 RP18 HP column (250×4.6mm 2 , with 5μm particles) using a mobile phase consisting of acetonitrile and water buffered at pH 7 using 10mM phosphate buffer. A gradient mode was operated at a flow rate of 1.5ml/min and detection was at 241nm. The method showed linearity for TCA and Impurity C in 0.02-125% of the workload, both square roots of the correlation coefficients were larger than 0.9999. Repeatability and intermediate precision were performed by six consecutive injections of both 1.25% and 125% of the work load for both TCA and Impurity C divided equally over two days. RSD were 0.6% and 0.7% for TCA and 0.5% and 0.1% for Impurity C respectively. Accuracy was determined as well, the average recoveries were 99.5% (±0.1%, n=3) for TCA and 96.9% (±1.3%, n=3) for impurity C respectively from spiked ointment samples. The robustness was also evaluated by variations of column (old vs new), mobile phase pH and filter retention. The applicability of the method was evaluated by analysis of a commercial ointment formulation. Interestingly, the extensive stress tests were able to predict all degradation products of TCA in a long term stability ointment sample. Copyright © 2017 Elsevier B.V. All rights reserved.

Molecular docking and simulation studies of gustatory receptor of Aedes aegypti: A potent drug target to distract host-seeking behaviour in mosquitoes.

PubMed

Gupta, Krishna Kant; Sethi, Guneswar; Jayaraman, Manikandan

2016-01-01

It is well reported that exhaled CO 2 and skin odour from human being assist female mosquitoes to locate human host. Basically, the receptors for this activity are expressed in cpA neurons. In both Aedes aegypti and Anopheles gambiae, this CO 2-sensitive olfactory neuron detects myriad number of chemicals present in human skin. Therefore, manipulation of gustatory receptors housing these neurons may serve as important targets for behavioural intervention. The study was aimed towards virtual screening of small molecules in the analyzed conserved active site residues of gustatory receptor and molecular dynamics simulation study of optimum protein-ligand complex to identify a suitable lead molecule for distracting host-seeking behaviour of mosquitoes. The conserved residue analysis of gustatory receptor (GR) of Ae. aegypti and An. gambiae was performed. The structure of GR protein from Ae. aegypti was modeled and validated, and then molecular docking was performed to screen 2903 small molecules against the predicted active residues of GR. Further, simulation studies were also carried out to prove protein-ligand stability. The glutamine 154 residue of GR was found to be highly conserved in Ae. aegypti and An. gambiae. Docking results indicated that the dodecanoic acid, 1,2,3-propanetriyl ester (dynasan 112) was interacting with this residue, as it showed better LibDock score than previously reported ethyl acetate used as mosquito repellant. Simulation studies indicated the structural instability of GR protein in docked form with dynasan 112 suggesting its involvement in structural changes. Based on the interaction energies and stability, this compound has been proposed to be used in mosquitoes' repellant. A novel effective odorant acting as inhibitor of GR is proposed based on its stability, docking score, interactions and RMSD, considering ethyl pyruvate as a standard inhibitor. Host preference and host-seeking ability of mosquito vectors play key roles in disease transmission, a clear understanding of these aspects is essential for preventing the spread of the disease.

The Psychometric Parameters of the Farsi Form of the Arabic Scale of Death Anxiety

PubMed Central

Abdel-Khalek, Ahmed M.; Lester, David

2017-01-01

The aim of this study was to describe the psychometric properties of the Farsi Form of the Arabic Scale of Death Anxiety (ASDA). The original scale was first translated into Farsi by language experts using the back translation procedure and then administered to a total of 252 Iranian college students and 52 psychiatric outpatients from psychiatric and psychological clinics. The one-week test-retest reliability of the Farsi version in a sample of college students was 0.78, indicating good temporal stability and corroborating the trait-like nature of scores. Cronbach's α was 0.90 for the college students and 0.92 for the psychiatric outpatients, indicating high internal consistency. Scale scores correlated 0.46 with Death Obsession Scale scores, 0.56 with Death Depression Scale scores, 0.41 with Death Anxiety Scale scores, and 0.40 with Wish to be Dead Scale scores, indicating good construct and criterion-related validity. A principal component analysis with a Varimax rotation yielded four factors in the sample of Iranian college students, indicating a lack of homogeneity in the content of the scale. Male students obtained a significant higher mean score than did females. It was concluded that the Farsi ASDA had good internal consistency, temporal stability, criterion-related validity, and a factor structure reflecting important features of death anxiety. In general, the Farsi ASDA could be recommended for use in research on death anxiety among Iranian college students and psychiatric outpatients. PMID:28698887

The Psychometric Parameters of the Farsi Form of the Arabic Scale of Death Anxiety.

PubMed

Dadfar, Mahboubeh; Abdel-Khalek, Ahmed M; Lester, David; Atef Vahid, Mohammad Kazem

2017-01-01

The aim of this study was to describe the psychometric properties of the Farsi Form of the Arabic Scale of Death Anxiety (ASDA). The original scale was first translated into Farsi by language experts using the back translation procedure and then administered to a total of 252 Iranian college students and 52 psychiatric outpatients from psychiatric and psychological clinics. The one-week test-retest reliability of the Farsi version in a sample of college students was 0.78, indicating good temporal stability and corroborating the trait-like nature of scores. Cronbach's α was 0.90 for the college students and 0.92 for the psychiatric outpatients, indicating high internal consistency. Scale scores correlated 0.46 with Death Obsession Scale scores, 0.56 with Death Depression Scale scores, 0.41 with Death Anxiety Scale scores, and 0.40 with Wish to be Dead Scale scores, indicating good construct and criterion-related validity. A principal component analysis with a Varimax rotation yielded four factors in the sample of Iranian college students, indicating a lack of homogeneity in the content of the scale. Male students obtained a significant higher mean score than did females. It was concluded that the Farsi ASDA had good internal consistency, temporal stability, criterion-related validity, and a factor structure reflecting important features of death anxiety. In general, the Farsi ASDA could be recommended for use in research on death anxiety among Iranian college students and psychiatric outpatients.

Computational design and experimental validation of new thermal barrier systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guo, Shengmin

2015-03-31

The focus of this project is on the development of a reliable and efficient ab initio based computational high temperature material design method which can be used to assist the Thermal Barrier Coating (TBC) bond-coat and top-coat design. Experimental evaluations on the new TBCs are conducted to confirm the new TBCs’ properties. Southern University is the subcontractor on this project with a focus on the computational simulation method development. We have performed ab initio density functional theory (DFT) method and molecular dynamics simulation on screening the top coats and bond coats for gas turbine thermal barrier coating design and validationmore » applications. For experimental validations, our focus is on the hot corrosion performance of different TBC systems. For example, for one of the top coatings studied, we examined the thermal stability of TaZr 2.75O 8 and confirmed it’s hot corrosion performance.« less

Availability of High Quality TRMM Ground Validation Data from Kwajalein, RMI: A Practical Application of the Relative Calibration Adjustment Technique

NASA Technical Reports Server (NTRS)

Marks, David A.; Wolff, David B.; Silberstein, David S.; Tokay, Ali; Pippitt, Jason L.; Wang, Jianxin

2008-01-01

Since the Tropical Rainfall Measuring Mission (TRMM) satellite launch in November 1997, the TRMM Satellite Validation Office (TSVO) at NASA Goddard Space Flight Center (GSFC) has been performing quality control and estimating rainfall from the KPOL S-band radar at Kwajalein, Republic of the Marshall Islands. Over this period, KPOL has incurred many episodes of calibration and antenna pointing angle uncertainty. To address these issues, the TSVO has applied the Relative Calibration Adjustment (RCA) technique to eight years of KPOL radar data to produce Ground Validation (GV) Version 7 products. This application has significantly improved stability in KPOL reflectivity distributions needed for Probability Matching Method (PMM) rain rate estimation and for comparisons to the TRMM Precipitation Radar (PR). In years with significant calibration and angle corrections, the statistical improvement in PMM distributions is dramatic. The intent of this paper is to show improved stability in corrected KPOL reflectivity distributions by using the PR as a stable reference. Inter-month fluctuations in mean reflectivity differences between the PR and corrected KPOL are on the order of 1-2 dB, and inter-year mean reflectivity differences fluctuate by approximately 1 dB. This represents a marked improvement in stability with confidence comparable to the established calibration and uncertainty boundaries of the PR. The practical application of the RCA method has salvaged eight years of radar data that would have otherwise been unusable, and has made possible a high-quality database of tropical ocean-based reflectivity measurements and precipitation estimates for the research community.

Prevalence of Invalid Performance on Baseline Testing for Sport-Related Concussion by Age and Validity Indicator.

PubMed

Abeare, Christopher A; Messa, Isabelle; Zuccato, Brandon G; Merker, Bradley; Erdodi, Laszlo

2018-03-12

Estimated base rates of invalid performance on baseline testing (base rates of failure) for the management of sport-related concussion range from 6.1% to 40.0%, depending on the validity indicator used. The instability of this key measure represents a challenge in the clinical interpretation of test results that could undermine the utility of baseline testing. To determine the prevalence of invalid performance on baseline testing and to assess whether the prevalence varies as a function of age and validity indicator. This retrospective, cross-sectional study included data collected between January 1, 2012, and December 31, 2016, from a clinical referral center in the Midwestern United States. Participants included 7897 consecutively tested, equivalently proportioned male and female athletes aged 10 to 21 years, who completed baseline neurocognitive testing for the purpose of concussion management. Baseline assessment was conducted with the Immediate Postconcussion Assessment and Cognitive Testing (ImPACT), a computerized neurocognitive test designed for assessment of concussion. Base rates of failure on published ImPACT validity indicators were compared within and across age groups. Hypotheses were developed after data collection but prior to analyses. Of the 7897 study participants, 4086 (51.7%) were male, mean (SD) age was 14.71 (1.78) years, 7820 (99.0%) were primarily English speaking, and the mean (SD) educational level was 8.79 (1.68) years. The base rate of failure ranged from 6.4% to 47.6% across individual indicators. Most of the sample (55.7%) failed at least 1 of 4 validity indicators. The base rate of failure varied considerably across age groups (117 of 140 [83.6%] for those aged 10 years to 14 of 48 [29.2%] for those aged 21 years), representing a risk ratio of 2.86 (95% CI, 2.60-3.16; P < .001). The results for base rate of failure were surprisingly high overall and varied widely depending on the specific validity indicator and the age of the examinee. The strong age association, with 3 of 4 participants aged 10 to 12 years failing validity indicators, suggests that the clinical interpretation and utility of baseline testing in this age group is questionable. These findings underscore the need for close scrutiny of performance validity indicators on baseline testing across age groups.

Development and Validation of Stability Indicating Spectroscopic Method for Content Analysis of Ceftriaxone Sodium in Pharmaceuticals

PubMed Central

Ethiraj, Revathi; Thiruvengadam, Ethiraj; Sampath, Venkattapuram Saravanan; Vahid, Abdul; Raj, Jithin

2014-01-01

A simple, selective, and stability indicating spectroscopic method has been selected and validated for the assay of ceftriaxone sodium in the powder for injection dosage forms. Proposed method is based on the measurement of absorbance of ceftriaxone sodium in aqueous medium at 241 nm. The method obeys Beer's law in the range of 5–50 μg/mL with correlation coefficient of 0.9983. Apparent molar absorptivity and Sandell's sensitivity were found to be 2.046 × 103 L mol−1 cm−1 and 0.02732 μg/cm2/0.001 absorbance units. This study indicated that ceftriaxone sodium was degraded in acid medium and also underwent oxidative degradation. Percent relative standard deviation associated with all the validation parameters was less than 2, showing compliance with acceptance criteria of Q2 (R1), International Conference on Harmonization (2005) guidelines. Then the proposed method was successfully applied to the determination of ceftriaxone sodium in sterile preparation and results were comparable with reported methods. PMID:27355020

Are NCLB's Measures, Incentives, and Improvement Strategies the Right Ones for the Nation's Low-Performing High Schools?

ERIC Educational Resources Information Center

Balfanz, Robert; Legters, Nettie; West, Thomas C.; Weber, Lisa M.

2007-01-01

This article examines the extent to which adequate yearly progress (AYP) is a valid and reliable indicator of improvement in low-performing high schools. For a random subsample of 202 high schools, the authors investigate the school characteristics and the federal and state policy contexts that influence their AYP status. Logistic regression…

Designing lanthanide-doped nanocrystals with both up- and down-conversion luminescence for anti-counterfeiting

NASA Astrophysics Data System (ADS)

Liu, Yanlan; Ai, Kelong; Lu, Lehui

2011-11-01

The widespread forgery in all kinds of paper documents and certificates has become a real threat to society. Traditional fluorescent anti-counterfeiting materials generally exhibit unicolor display and suffer greatly from substitution, thus leading to a poor anti-counterfeiting effect. In this work, unseen but significant enhanced blue down-conversion emission from oleic acid-stabilized lanthanide-doped fluoride nanocrystals is first present and the mechanism is proposed and validated. This not only endows these nanocrystals with dual-mode fluorescence, but also offers a simplified synthesis approach for dual-mode fluorescent nanocrystals involving no further complicated assembly or coating procedures, unlike the traditional methods. Furthermore, by changing the host/dopant combination or the content of dopant, these nanocrystals can exhibit simultaneously multicolor up-conversion emission under excitation at near-infrared light and unalterable blue down-conversion emission under ultraviolet light. A preliminary investigation of their anti-counterfeiting performance has been made, and the results indicate that this color tuning capability and high concealment makes these nanocrystals behave in a similar way to chameleons and can provide a strengthened and more reliable anti-counterfeiting effect.The widespread forgery in all kinds of paper documents and certificates has become a real threat to society. Traditional fluorescent anti-counterfeiting materials generally exhibit unicolor display and suffer greatly from substitution, thus leading to a poor anti-counterfeiting effect. In this work, unseen but significant enhanced blue down-conversion emission from oleic acid-stabilized lanthanide-doped fluoride nanocrystals is first present and the mechanism is proposed and validated. This not only endows these nanocrystals with dual-mode fluorescence, but also offers a simplified synthesis approach for dual-mode fluorescent nanocrystals involving no further complicated assembly or coating procedures, unlike the traditional methods. Furthermore, by changing the host/dopant combination or the content of dopant, these nanocrystals can exhibit simultaneously multicolor up-conversion emission under excitation at near-infrared light and unalterable blue down-conversion emission under ultraviolet light. A preliminary investigation of their anti-counterfeiting performance has been made, and the results indicate that this color tuning capability and high concealment makes these nanocrystals behave in a similar way to chameleons and can provide a strengthened and more reliable anti-counterfeiting effect. Electronic supplementary information (ESI) available: Fig. S1-S6, Table S. See DOI: 10.1039/c1nr10752f

Primary Stability Recognition of the Newly Designed Cementless Femoral Stem Using Digital Signal Processing

PubMed Central

Salleh, Sh-Hussain; Hamedi, Mahyar; Zulkifly, Ahmad Hafiz; Lee, Muhammad Hisyam; Mohd Noor, Alias; Harris, Arief Ruhullah A.; Abdul Majid, Norazman

2014-01-01

Stress shielding and micromotion are two major issues which determine the success of newly designed cementless femoral stems. The correlation of experimental validation with finite element analysis (FEA) is commonly used to evaluate the stress distribution and fixation stability of the stem within the femoral canal. This paper focused on the applications of feature extraction and pattern recognition using support vector machine (SVM) to determine the primary stability of the implant. We measured strain with triaxial rosette at the metaphyseal region and micromotion with linear variable direct transducer proximally and distally using composite femora. The root mean squares technique is used to feed the classifier which provides maximum likelihood estimation of amplitude, and radial basis function is used as the kernel parameter which mapped the datasets into separable hyperplanes. The results showed 100% pattern recognition accuracy using SVM for both strain and micromotion. This indicates that DSP could be applied in determining the femoral stem primary stability with high pattern recognition accuracy in biomechanical testing. PMID:24800230

Primary stability recognition of the newly designed cementless femoral stem using digital signal processing.

PubMed

Baharuddin, Mohd Yusof; Salleh, Sh-Hussain; Hamedi, Mahyar; Zulkifly, Ahmad Hafiz; Lee, Muhammad Hisyam; Mohd Noor, Alias; Harris, Arief Ruhullah A; Abdul Majid, Norazman

2014-01-01

Stress shielding and micromotion are two major issues which determine the success of newly designed cementless femoral stems. The correlation of experimental validation with finite element analysis (FEA) is commonly used to evaluate the stress distribution and fixation stability of the stem within the femoral canal. This paper focused on the applications of feature extraction and pattern recognition using support vector machine (SVM) to determine the primary stability of the implant. We measured strain with triaxial rosette at the metaphyseal region and micromotion with linear variable direct transducer proximally and distally using composite femora. The root mean squares technique is used to feed the classifier which provides maximum likelihood estimation of amplitude, and radial basis function is used as the kernel parameter which mapped the datasets into separable hyperplanes. The results showed 100% pattern recognition accuracy using SVM for both strain and micromotion. This indicates that DSP could be applied in determining the femoral stem primary stability with high pattern recognition accuracy in biomechanical testing.

Test-retest stability of the Task and Ego Orientation Questionnaire.

PubMed

Lane, Andrew M; Nevill, Alan M; Bowes, Neal; Fox, Kenneth R

2005-09-01

Establishing stability, defined as observing minimal measurement error in a test-retest assessment, is vital to validating psychometric tools. Correlational methods, such as Pearson product-moment, intraclass, and kappa are tests of association or consistency, whereas stability or reproducibility (regarded here as synonymous) assesses the agreement between test-retest scores. Indexes of reproducibility using the Task and Ego Orientation in Sport Questionnaire (TEOSQ; Duda & Nicholls, 1992) were investigated using correlational (Pearson product-moment, intraclass, and kappa) methods, repeated measures multivariate analysis of variance, and calculating the proportion of agreement within a referent value of +/-1 as suggested by Nevill, Lane, Kilgour, Bowes, and Whyte (2001). Two hundred thirteen soccer players completed the TEOSQ on two occasions, 1 week apart. Correlation analyses indicated a stronger test-retest correlation for the Ego subscale than the Task subscale. Multivariate analysis of variance indicated stability for ego items but with significant increases in four task items. The proportion of test-retest agreement scores indicated that all ego items reported relatively poor stability statistics with test-retest scores within a range of +/-1, ranging from 82.7-86.9%. By contrast, all task items showed test-retest difference scores ranging from 92.5-99%, although further analysis indicated that four task subscale items increased significantly. Findings illustrated that correlational methods (Pearson product-moment, intraclass, and kappa) are influenced by the range in scores, and calculating the proportion of agreement of test-retest differences with a referent value of +/-1 could provide additional insight into the stability of the questionnaire. It is suggested that the item-by-item proportion of agreement method proposed by Nevill et al. (2001) should be used to supplement existing methods and could be especially helpful in identifying rogue items in the initial stages of psychometric questionnaire validation.

Stabilized finite element methods to simulate the conductances of ion channels

NASA Astrophysics Data System (ADS)

Tu, Bin; Xie, Yan; Zhang, Linbo; Lu, Benzhuo

2015-03-01

We have previously developed a finite element simulator, ichannel, to simulate ion transport through three-dimensional ion channel systems via solving the Poisson-Nernst-Planck equations (PNP) and Size-modified Poisson-Nernst-Planck equations (SMPNP), and succeeded in simulating some ion channel systems. However, the iterative solution between the coupled Poisson equation and the Nernst-Planck equations has difficulty converging for some large systems. One reason we found is that the NP equations are advection-dominated diffusion equations, which causes troubles in the usual FE solution. The stabilized schemes have been applied to compute fluids flow in various research fields. However, they have not been studied in the simulation of ion transport through three-dimensional models based on experimentally determined ion channel structures. In this paper, two stabilized techniques, the SUPG and the Pseudo Residual-Free Bubble function (PRFB) are introduced to enhance the numerical robustness and convergence performance of the finite element algorithm in ichannel. The conductances of the voltage dependent anion channel (VDAC) and the anthrax toxin protective antigen pore (PA) are simulated to validate the stabilization techniques. Those two stabilized schemes give reasonable results for the two proteins, with decent agreement with both experimental data and Brownian dynamics (BD) simulations. For a variety of numerical tests, it is found that the simulator effectively avoids previous numerical instability after introducing the stabilization methods. Comparison based on our test data set between the two stabilized schemes indicates both SUPG and PRFB have similar performance (the latter is slightly more accurate and stable), while SUPG is relatively more convenient to implement.

A survey of pulse shape options for a revised plastic ablator ignition design

NASA Astrophysics Data System (ADS)

Clark, Daniel; Eder, David; Haan, Steven; Hinkel, Denise; Jones, Ogden; Marinak, Michael; Milovich, Jose; Peterson, Jayson; Robey, Harold; Salmonson, Jay; Smalyuk, Vladimir; Weber, Christopher

2014-10-01

Recent experimental results using the ``high foot'' pulse shape on the National Ignition Facility (NIF) have shown encouraging progress compared to earlier ``low foot'' experiments. These results strongly suggest that controlling ablation front instability growth can dramatically improve implosion performance, even in the presence of persistent, large, low-mode distortions. In parallel, Hydro. Growth Radiography experiments have so far validated the techniques used for modeling ablation front growth in NIF experiments. It is timely then to combine these two results and ask how current ignition pulse shapes could be modified so as to improve implosion performance, namely fuel compressibility, while maintaining the stability properties demonstrated with the high foot. This talk presents a survey of pulse shapes intermediate between the low and high foot extremes in search of a more optimal design. From the database of pulse shapes surveyed, a higher picket version of the original low foot pulse shape shows the most promise for improved compression without loss of stability. This work performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

LOLA: a 40.000 km optical link between an aircraft and a geostationary satellite

NASA Astrophysics Data System (ADS)

Cazaubiel, Vincent; Planche, Gilles; Chorvalli, Vincent; Le Hors, Lénaïc.; Roy, Bernard; Giraud, Emmanuel; Vaillon, Ludovic; Carre, Francois; Decourbey, Eric

2017-11-01

The LOLA program aims at characterising a 40.000 km optical link through the atmosphere between a high altitude aircraft and a geostationary platform. It opens a new area in the field of optical communications with moving platforms. A complete new optical terminal has been designed and manufactured for this program. The optical terminal architecture includes a specific pointing subsystem to acquire and stabilize the line of sight despite the induced vibrations from the aircraft and the moving pattern from the received laser signal. The optical configuration features a silicon carbide telescope and optical bench to ensure a high thermoelastic angular stability between receive and transmit beams. The communications subsystem includes fibered laser diodes developed in Europe and high performance avalanche photo detectors. Specific encoding patterns are used to maintain the performance of the link despite potential strong fading of the signal. A specific optical link model through the atmosphere has been developed and has been validated thanks to the optical link measurements performed between ARTEMIS and the Optical Ground Station located in the Canarian islands. This model will be used during the flight tests campaign that is to start this summer.

Fundamental Investigations and Rational Design of Durable High-Performance SOFC Cathodes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Yu; Ding, Dong; Wei, Tao

The main objective of this project is to unravel the degradation mechanism of LSCF cathodes under realistic operating conditions with different types of contaminants, aiming towards the rational design of cathodes with high-performance and enhanced durability by combining a porous backbone (such as LSCF) with a thin catalyst coating. The mechanistic understanding will help us to optimize the composition and morphology of the catalyst layer and microstructure of the LSCF backbone for better performance and durability. More specifically, the technical objectives include: (1) to unravel the degradation mechanism of LSCF cathodes under realistic operating conditions with different types of contaminantsmore » using in situ and ex situ measurements performed on specially-designed cathodes; (2) to examine the microstructural and compositional evolution of LSCF cathodes as well as the cathode/electrolyte interfaces under realistic operating conditions; (3) to correlate the fuel cell performance instability and degradation with the microstructural and morphological evolution and surface chemistry change of the cathode under realistic operating conditions; (4) to explore new catalyst materials and electrode structures to enhance the stability of the LSCF cathode under realistic operating conditions; and (5) to validate the long term stability of the modified LSCF cathode in commercially available cells under realistic operating conditions. We have systematically evaluated LSCF cathodes in symmetrical cells and anode supported cells under realistic conditions with different types of contaminants such as humidity, CO 2, and Cr. Electrochemical models for the design of test cells and understanding of mechanisms have been developed for the exploration of fundamental properties of electrode materials. It is demonstrated that the activity and stability of LSCF cathodes can be degraded by the introduction of contaminants. The microstructural and compositional evolution of LSCF cathodes as well as the cathode/electrolyte interfaces under realistic operating conditions has been studied. It is found that SrO readily segregated/enriched on the LSCF surface. More severe contamination conditions cause more SrO on surface. Novel catalyst coatings through particle depositions (PrOx) or continuous thin films (PNM) were successfully developed to improve the activity and stability of LSCF cathodes. Finally, we have demonstrated enhanced activity and stability of LSCF cathodes over longer periods of time in homemade and commercially available cells by an optimized PNM (dense film and particles) infiltration process, under clean air and realistic operating conditions (3% H 2O, 5% CO 2 and direct Crofer contact). Both performance and durability of single cells with PNM coating has been enhanced compared with those without coating. Raman analysis of cathodes surface indicated that the intensity of SrCrO 4 was significantly decreased.« less

Effects of Inlet Distortion on Aeromechanical Stability of a Forward-Swept High-Speed Fan

NASA Technical Reports Server (NTRS)

Herrick, Gregory P.

2011-01-01

Concerns regarding noise, propulsive efficiency, and fuel burn are inspiring aircraft designs wherein the propulsive turbomachines are partially (or fully) embedded within the airframe; such designs present serious concerns with regard to aerodynamic and aeromechanic performance of the compression system in response to inlet distortion. Separately, a forward-swept high-speed fan was developed to address noise concerns of modern podded turbofans; however this fan encounters aeroelastic instability (flutter) as it approaches stall. A three-dimensional, unsteady, Navier-Stokes computational fluid dynamics code is applied to analyze and corroborate fan performance with clean inlet flow. This code, already validated in its application to assess aerodynamic damping of vibrating blades at various flow conditions, is modified and then applied in a computational study to preliminarily assess the effects of inlet distortion on aeroelastic stability of the fan. Computational engineering application and implementation issues are discussed, followed by an investigation into the aeroelastic behavior of the fan with clean and distorted inlets.

Towards a full integration of optimization and validation phases: An analytical-quality-by-design approach.

PubMed

Hubert, C; Houari, S; Rozet, E; Lebrun, P; Hubert, Ph

2015-05-22

When using an analytical method, defining an analytical target profile (ATP) focused on quantitative performance represents a key input, and this will drive the method development process. In this context, two case studies were selected in order to demonstrate the potential of a quality-by-design (QbD) strategy when applied to two specific phases of the method lifecycle: the pre-validation study and the validation step. The first case study focused on the improvement of a liquid chromatography (LC) coupled to mass spectrometry (MS) stability-indicating method by the means of the QbD concept. The design of experiments (DoE) conducted during the optimization step (i.e. determination of the qualitative design space (DS)) was performed a posteriori. Additional experiments were performed in order to simultaneously conduct the pre-validation study to assist in defining the DoE to be conducted during the formal validation step. This predicted protocol was compared to the one used during the formal validation. A second case study based on the LC/MS-MS determination of glucosamine and galactosamine in human plasma was considered in order to illustrate an innovative strategy allowing the QbD methodology to be incorporated during the validation phase. An operational space, defined by the qualitative DS, was considered during the validation process rather than a specific set of working conditions as conventionally performed. Results of all the validation parameters conventionally studied were compared to those obtained with this innovative approach for glucosamine and galactosamine. Using this strategy, qualitative and quantitative information were obtained. Consequently, an analyst using this approach would be able to select with great confidence several working conditions within the operational space rather than a given condition for the routine use of the method. This innovative strategy combines both a learning process and a thorough assessment of the risk involved. Copyright © 2015 Elsevier B.V. All rights reserved.

Development and validation of sensitive LC/MS/MS method for quantitative bioanalysis of levonorgestrel in rat plasma and application to pharmacokinetics study.

PubMed

Ananthula, Suryatheja; Janagam, Dileep R; Jamalapuram, Seshulatha; Johnson, James R; Mandrell, Timothy D; Lowe, Tao L

2015-10-15

Rapid, sensitive, selective and accurate LC/MS/MS method was developed for quantitative determination of levonorgestrel (LNG) in rat plasma and further validated for specificity, linearity, accuracy, precision, sensitivity, matrix effect, recovery efficiency and stability. Liquid-liquid extraction procedure using hexane:ethyl acetate mixture at 80:20 v:v ratio was employed to efficiently extract LNG from rat plasma. Reversed phase Luna column C18(2) (50×2.0mm i.d., 3μM) installed on a AB SCIEX Triple Quad™ 4500 LC/MS/MS system was used to perform chromatographic separation. LNG was identified within 2min with high specificity. Linear calibration curve was drawn within 0.5-50ng·mL(-1) concentration range. The developed method was validated for intra-day and inter-day accuracy and precision whose values fell in the acceptable limits. Matrix effect was found to be minimal. Recovery efficiency at three quality control (QC) concentrations 0.5 (low), 5 (medium) and 50 (high) ng·mL(-1) was found to be >90%. Stability of LNG at various stages of experiment including storage, extraction and analysis was evaluated using QC samples, and the results showed that LNG was stable at all the conditions. This validated method was successfully used to study the pharmacokinetics of LNG in rats after SubQ injection, providing its applicability in relevant preclinical studies. Copyright © 2015 Elsevier B.V. All rights reserved.

Integrated vision-based GNC for autonomous rendezvous and capture around Mars

NASA Astrophysics Data System (ADS)

Strippoli, L.; Novelli, G.; Gil Fernandez, J.; Colmenarejo, P.; Le Peuvedic, C.; Lanza, P.; Ankersen, F.

2015-06-01

Integrated GNC (iGNC) is an activity aimed at designing, developing and validating the GNC for autonomously performing the rendezvous and capture phase of the Mars sample return mission as defined during the Mars sample return Orbiter (MSRO) ESA study. The validation cycle includes testing in an end-to-end simulator, in a real-time avionics-representative test bench and, finally, in a dynamic HW in the loop test bench for assessing the feasibility, performances and figure of merits of the baseline approach defined during the MSRO study, for both nominal and contingency scenarios. The on-board software (OBSW) is tailored to work with the sensors, actuators and orbits baseline proposed in MSRO. The whole rendezvous is based on optical navigation, aided by RF-Doppler during the search and first orbit determination of the orbiting sample. The simulated rendezvous phase includes also the non-linear orbit synchronization, based on a dedicated non-linear guidance algorithm robust to Mars ascent vehicle (MAV) injection accuracy or MAV failures resulting in elliptic target orbits. The search phase is very demanding for the image processing (IP) due to the very high visual magnitude of the target wrt. the stellar background, and the attitude GNC requires very high pointing stability accuracies to fulfil IP constraints. A trade-off of innovative, autonomous navigation filters indicates the unscented Kalman filter (UKF) as the approach that provides the best results in terms of robustness, response to non-linearities and performances compatibly with computational load. At short range, an optimized IP based on a convex hull algorithm has been developed in order to guarantee LoS and range measurements from hundreds of metres to capture.

Validity Evidence for Games as Assessment Environments. CRESST Report 773

ERIC Educational Resources Information Center

Delacruz, Girlie C.; Chung, Gregory K. W. K.; Baker, Eva L.

2010-01-01

This study provides empirical evidence of a highly specific use of games in education--the assessment of the learner. Linear regressions were used to examine the predictive and convergent validity of a math game as assessment of mathematical understanding. Results indicate that prior knowledge significantly predicts game performance. Results also…

Measured performance of the GTA rf systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Denney, P.M.; Jachim, S.P.

1993-06-01

This paper describes the performance of the RF systems on the Ground Test Accelerator (GTA). The RF system architecture is briefly described. Among the RF performance results presented are RF field flatness and stability, amplitude and phase control resolution, and control system bandwidth and stability. The rejection by the RF systems of beam-induced disturbances, such as transients and noise, are analyzed. The observed responses are also compared to computer-based simulations of the RF systems for validation.

Measured performance of the GTA rf systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Denney, P.M.; Jachim, S.P.

1993-01-01

This paper describes the performance of the RF systems on the Ground Test Accelerator (GTA). The RF system architecture is briefly described. Among the RF performance results presented are RF field flatness and stability, amplitude and phase control resolution, and control system bandwidth and stability. The rejection by the RF systems of beam-induced disturbances, such as transients and noise, are analyzed. The observed responses are also compared to computer-based simulations of the RF systems for validation.

The Development of HfO2-Rare Earth Based Oxide Materials and Barrier Coatings for Thermal Protection Systems

NASA Technical Reports Server (NTRS)

Zhu, Dongming; Harder, Bryan James

2014-01-01

Advanced hafnia-rare earth oxides, rare earth aluminates and silicates have been developed for thermal environmental barrier systems for aerospace propulsion engine and thermal protection applications. The high temperature stability, low thermal conductivity, excellent oxidation resistance and mechanical properties of these oxide material systems make them attractive and potentially viable for thermal protection systems. This paper will focus on the development of the high performance and high temperature capable ZrO2HfO2-rare earth based alloy and compound oxide materials, processed as protective coating systems using state-or-the-art processing techniques. The emphasis has been in particular placed on assessing their temperature capability, stability and suitability for advanced space vehicle entry thermal protection systems. Fundamental thermophysical and thermomechanical properties of the material systems have been investigated at high temperatures. Laser high-heat-flux testing has also been developed to validate the material systems, and demonstrating durability under space entry high heat flux conditions.

Determination of a novel nonfluorinated quinolone, nemonoxacin, in human feces and its glucuronide conjugate in human urine and feces by high-performance liquid chromatography-triple quadrupole mass spectrometry.

PubMed

He, Gaoli; Guo, Beining; Yu, Jicheng; Zhang, Jing; Wu, Xiaojie; Cao, Guoying; Shi, Yaoguo; Tsai, Cheng-Yuan

2015-05-01

Three methods were developed and validated for determination of nemonoxacin in human feces and its major metabolite, nemonoxacin acyl-β- d-glucuronide, in human urine and feces. Nemonoxacin was extracted by liquid-liquid extraction in feces homogenate samples and nemonoxacin acyl-β- d-glucuronide by a solid-phase extraction procedure for pretreatment of both urine and feces homogenate sample. Separation was performed on a C18 reversed-phase column under isocratic elution with the mobile phase consisting of acetonitrile and 0.1% formic acid. Both analytes were determined by liquid chromatography-tandem mass spectrometry with positive electrospray ionization in selected reaction monitoring mode and gatifloxacin as the internal standard. The lower limit of quantitation (LLOQ) of nemonoxacin in feces was 0.12 µg/g and the calibration curve was linear in the concentration range of 0.12-48.00 µg/g. The LLOQ of the metabolite was 0.0010 µg/mL and 0.03 µg/g in urine and feces matrices, while the linear range was 0.0010-0.2000 µg/mL and 0.03-3.00 µg/g, respectively. Validation included selectivity, accuracy, precision, linearity, recovery, matrix effect, carryover, dilution integrity and stability, indicating that the methods can quantify the corresponding analytes with excellent reliability. The validated methods were successfully applied to an absolute bioavailability clinical study of nemonoxacin malate capsule. Copyright © 2014 John Wiley & Sons, Ltd.

RP-1 Thermal Stability and Copper Based Materials Compatibility Study

NASA Technical Reports Server (NTRS)

Stiegemeier, B. R.; Meyer, M. L.; Driscoll, E.

2005-01-01

A series of electrically heated tube tests was performed at the NASA Glenn Research Center s Heated Tube Facility to investigate the effect that sulfur content, test duration, and tube material play in the overall thermal stability and materials compatibility characteristics of RP-1. Scanning-electron microscopic (SEM) analysis in conjunction with energy dispersive spectroscopy (EDS) were used to characterize the condition of the tube inner wall surface and any carbon deposition or corrosion formed during these runs. Results of the parametric study indicate that tests with standard RP-1 (total sulfur -23 ppm) and pure copper tubing are characterized by a depostion/deposit shedding process producing local wall temperature swings as high as 500 F. The effect of this shedding is to keep total carbon deposition levels relatively constant for run times from 20 minutes up to 5 hours, though increasing tube pressure drops were observed in all runs. Reduction in the total sulfur content of the fuel from 23 ppm to less than 0.1 ppm resulted in the elimination of deposit shedding, local wall temperature variation, and the tube pressure drop increases that were observed in standard sulfur level RP-1 tests. The copper alloy GRCop-84, a copper alloy developed specifically for high heat flux applications, was found to exhibit higher carbon deposition levels compared to identical tests performed in pure copper tubes. Results of the study are consistent with previously published heated tube data which indicates that small changes in fuel total sulfur content can lead to significant differences in the thermal stability of kerosene type fuels and their compatibility with copper based materials. In conjunction with the existing thermal stability database, these findings give insight into the feasibility of cooling a long life, high performance, high-pressure liquid rocket combustor and nozzle with RP-1.

The Estimated Impact of Performing Arts on Adolescent Mood within a Community Sample of Mental Health Professionals

ERIC Educational Resources Information Center

King, Alan; Grieves, Julie; Opp, Dean

2007-01-01

In a brief survey, the authors solicited professional opinions regarding the probable impact of performing arts on adolescent mood stability using a hypothetical scenario where 20 moderately depressed 15-year-olds agreed to participate in a high school play, musical, or other singing performance. The results of the survey indicated that clinicians…

Validation of HPLC and UV spectrophotometric methods for the determination of meropenem in pharmaceutical dosage form.

PubMed

Mendez, Andreas S L; Steppe, Martin; Schapoval, Elfrides E S

2003-12-04

A high-performance liquid chromatographic method and a UV spectrophotometric method for the quantitative determination of meropenem, a highly active carbapenem antibiotic, in powder for injection were developed in present work. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by reversed-phase technique on an RP-18 column with a mobile phase composed of 30 mM monobasic phosphate buffer and acetonitrile (90:10; v/v), adjusted to pH 3.0 with orthophosphoric acid. The UV spectrophotometric method was performed at 298 nm. The samples were prepared in water and the stability of meropenem in aqueous solution at 4 and 25 degrees C was studied. The results were satisfactory with good stability after 24 h at 4 degrees C. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the two methods. The proposed methods are highly sensitive, precise and accurate and can be used for the reliable quantitation of meropenem in pharmaceutical dosage form.

Content and face validity of a comprehensive robotic skills training program for general surgery, urology, and gynecology.

PubMed

Dulan, Genevieve; Rege, Robert V; Hogg, Deborah C; Gilberg-Fisher, Kristine K; Tesfay, Seifu T; Scott, Daniel J

2012-04-01

The authors previously developed a comprehensive, proficiency-based robotic training curriculum that aimed to address 23 unique skills identified via task deconstruction of robotic operations. The purpose of this study was to determine the content and face validity of this curriculum. Expert robotic surgeons (n = 12) rated each deconstructed skill regarding relevance to robotic operations, were oriented to the curricular components, performed 3 to 5 repetitions on the 9 exercises, and rated each exercise. In terms of content validity, experts rated all 23 deconstructed skills as highly relevant (4.5 on a 5-point scale). Ratings for the 9 inanimate exercises indicated moderate to thorough measurement of designated skills. For face validity, experts indicated that each exercise effectively measured relevant skills (100% agreement) and was highly effective for training and assessment (4.5 on a 5-point scale). These data indicate that the 23 deconstructed skills accurately represent the appropriate content for robotic skills training and strongly support content and face validity for this curriculum. Copyright © 2012. Published by Elsevier Inc.

A Simple and Specific Stability- Indicating RP-HPLC Method for Routine Assay of Adefovir Dipivoxil in Bulk and Tablet Dosage Form.

PubMed

Darsazan, Bahar; Shafaati, Alireza; Mortazavi, Seyed Alireza; Zarghi, Afshin

2017-01-01

A simple and reliable stability-indicating RP-HPLC method was developed and validated for analysis of adefovir dipivoxil (ADV).The chromatographic separation was performed on a C 18 column using a mixture of acetonitrile-citrate buffer (10 mM at pH 5.2) 36:64 (%v/v) as mobile phase, at a flow rate of 1.5 mL/min. Detection was carried out at 260 nm and a sharp peak was obtained for ADV at a retention time of 5.8 ± 0.01 min. No interferences were observed from its stress degradation products. The method was validated according to the international guidelines. Linear regression analysis of data for the calibration plot showed a linear relationship between peak area and concentration over the range of 0.5-16 μg/mL; the regression coefficient was 0.9999and the linear regression equation was y = 24844x-2941.3. The detection (LOD) and quantification (LOQ) limits were 0.12 and 0.35 μg/mL, respectively. The results proved the method was fast (analysis time less than 7 min), precise, reproducible, and accurate for analysis of ADV over a wide range of concentration. The proposed specific method was used for routine quantification of ADV in pharmaceutical bulk and a tablet dosage form.

Stability of tacrolimus injection diluted in 0.9% sodium chloride injection and stored in Excel bags.

PubMed

Myers, Alan L; Zhang, Yanping; Kawedia, Jitesh D; Shank, Brandon R; Deaver, Melissa A; Kramer, Mark A

2016-12-15

The chemical stability and physical compatibility of tacrolimus i.v. infusion solutions prepared in Excel bags and stored at 23 or 4 °C for up to nine days were studied. Tacrolimus admixtures (2, 4, and 8 μg/mL) were prepared in Excel bags using 0.9% sodium chloride injection and stored at 23 °C without protection from light or at 4 °C in the dark. Test samples were withdrawn from triplicate bag solutions immediately after preparation and at predetermined time intervals (1, 3, 5, 7, and 9 days). Chemical stability was assessed by measuring tacrolimus concentrations using a validated stability-indicating high-performance liquid chromatography assay. The physical stability of the admixtures was assessed by visual examination and by measuring turbidity, particle size, and drug content. All test solutions stored at 23 or 4 °C had a no greater than 6% loss of the initial tacrolimus concentration throughout the nine-day study period. All test samples of tacrolimus admixtures, under both storage conditions, were without precipitation and remained clear initially and throughout the nine-day observation period. Changes in turbidities were minor; measured particulates remained few in number in all samples throughout the study. Extemporaneously prepared infusion solutions of tacrolimus 2, 4, and 8 μg/mL in 0.9% sodium chloride injection in Excel bags were chemically and physically stable for at least nine days when stored at room temperature (23 °C) without protection from light and when stored in a refrigerator (4 °C) in the dark. Copyright © 2016 by the American Society of Health-System Pharmacists, Inc. All rights reserved.

Chitosan based atorvastatin nanocrystals: effect of cationic charge on particle size, formulation stability, and in-vivo efficacy

PubMed Central

Kurakula, Mallesh; El-Helw, AM; Sobahi, Tariq R; Abdelaal, Magdy Y

2015-01-01

Cationic charged chitosan as stabilizer was evaluated in preparation of nanocrystals using probe sonication method. The influence of cationic charge densities of chitosan (low CSL, medium CSM, high CSH molecular weights) and Labrasol® in solubility enhancement and modifying the release was investigated, using atorvastatin (ATR) as poorly soluble model drug. Compared to CSM and CSH; low cationic charge of CSL acted as both electrostatic and steric stabilizer by significant size reduction to 394 nm with charge of 21.5 meV. Solubility of ATR-CSL increased to 60-fold relative to pure ATR and ATR-L. Nanocrystals were characterized for physiochemical properties. Scanning electron microscopy revealed scaffold-like structures with high surface area. X-ray powder diffractometry and differential scanning calorimetry revealed crystalline to slight amorphous state changes after cationic charge size reduction. Fourier transform-infrared spectra indicated no potent drug-excipient interactions. The enhanced dissolution profile of ATR-CSL indicates that sustained release was achieved compared with ATR-L and Lipitor®. Anti-hyperlipidemic performance was pH dependent where ATR-CSL exhibited 2.5-fold higher efficacy at pH 5 compared to pH 6 and Lipitor®. Stability studies indicated marked changes in size and charge for ATR-L compared to ATR-CSL exemplifying importance of the stabilizer. Therefore, nanocrystals developed with CSL as a stabilizer is a promising choice to enhance dissolution, stability, and in-vivo efficacy of major Biopharmaceutical Classification System II/IV drugs. PMID:25609947

Determination of the Stability and Control Characteristics of a Tailless All-Wing Airplane Model with Sweepback in the Langley Free-Flight Tunnel

NASA Technical Reports Server (NTRS)

Seacord, Charles L.; Campbell, John P.

1945-01-01

Force and flight tests were performance on an all-wing model with windmilling propellers. Tests were conducted with deflected and retracted flaps, with and without auxiliary vertical tail surfaces, and with different centers of gravity and trim coefficients. Results indicate serious reduction of stick-fixed longitudinal stability because of wing-tip stalling at high lift coefficient. Directional stability without vertical tail is undesirably low. Low effective dihedral should be maintained. Elevator and rudder control system is satisfactory.

A validated RP-HPLC method for simultaneous determination of propranolol and valsartan in bulk drug and gel formulation

PubMed Central

Imam, Syed Sarim; Ahad, Abdul; Aqil, Mohammed; Sultana, Yasmin; Ali, Asgar

2013-01-01

Objective: A simple, precise, and stability indicating high performance liquid chromatography (HPLC) method was developed and validated for the simultaneous determination of propranolol hydrochloride and valsartan in pharmaceutical dosage form. Materials and Methods: The method involves the use of easily available inexpensive laboratory reagents. The separation was achieved on Hypersil ODS C-18 column (250*4.6 mm, i.d., 5 μm particle size) with isocratic flow with UV detector. The mobile phase at a flow rate of 1.0 mL/min consisted of acetonitrile, methanol, and 0.01 M disodium hydrogen phosphate (pH 3.5) in the ratio of 50:35:15 v/v. Results: A linear response was observed over the concentration range 5-50 μg/mL of propranolol and the concentration range 4-32 μg/mL of valsartan. Limit of detection and limit of quantitation for propranolol were 0.27 μg/mL and 0.85 μg/mL, and for valsartan were 0.45 μg/mL and 1.39 μg/mL, respectively. The method was successfully validated in accordance to ICH guidelines acceptance criteria for linearity, accuracy, precision, specificity, robustness. Conclusion: The analysis concluded that the method was selective for simultaneous estimation of propranolol and valsartan can be potentially used for the estimation of these drugs in combined dosage form. PMID:23559826

On-Line Robust Modal Stability Prediction using Wavelet Processing

NASA Technical Reports Server (NTRS)

Brenner, Martin J.; Lind, Rick

1998-01-01

Wavelet analysis for filtering and system identification has been used to improve the estimation of aeroservoelastic stability margins. The conservatism of the robust stability margins is reduced with parametric and nonparametric time- frequency analysis of flight data in the model validation process. Nonparametric wavelet processing of data is used to reduce the effects of external disturbances and unmodeled dynamics. Parametric estimates of modal stability are also extracted using the wavelet transform. Computation of robust stability margins for stability boundary prediction depends on uncertainty descriptions derived from the data for model validation. The F-18 High Alpha Research Vehicle aeroservoelastic flight test data demonstrates improved robust stability prediction by extension of the stability boundary beyond the flight regime. Guidelines and computation times are presented to show the efficiency and practical aspects of these procedures for on-line implementation. Feasibility of the method is shown for processing flight data from time- varying nonstationary test points.

Studies on the stability of preservatives under subcritical water conditions.

PubMed

Kapalavavi, B; Marple, R; Gamsky, C; Yang, Y

2015-06-01

The goal of this work was to further validate the subcritical water chromatography (SBWC) methods for separation and analysis of preservatives through the evaluation of analyte stability in subcritical water. In this study, the degradation of preservatives was investigated at temperatures of 100-200°C using two different approaches. First, the peak areas obtained by SBWC at high temperatures were compared with those achieved using the traditional high-performance liquid chromatography (HPLC) at 25°C. In the second approach, several preservatives and water were loaded into a vessel and heated at high temperatures for 30 or 60 min. The heated mixtures were then analysed by GC/MS to determine the stability of preservatives. The t- and F-test on the results of the first approach reveal that the peak areas achieved by HPLC and SBWC are not significantly different at the 95% confidence level, meaning that the preservatives studied are stable during the high-temperature SBWC runs. Although the results of the second approach show approximately 10% degradation of preservatives into mainly p-hydroxybenzoic acid and phenol at 200°C, the preservatives studied are stable at 100 and 150°C. This is in good agreement with the validation results obtained by the first approach. The findings of this work confirm that SBWC methods at temperatures up to 150°C are reliable for separation and analysis of preservatives in cosmetic and other samples. © 2014 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Development and Validation of a Stability-Indicating Assay of Etofenamate by RP-HPLC and Characterization of Degradation Products

PubMed Central

Peraman, Ramalingam; Nayakanti, Devanna; Dugga, Hari Hara Theja; Kodikonda, Sudhakara

2013-01-01

A validated stability-indicating RP-HPLC method for etofenamate (ETF) was developed by separating its degradation products on a C18 (250 mm × 4.6 mm 5 μm) Qualisil BDS column using a phosphate buffer (pH-adjusted to 6.0 with orthophosphoric acid) and methanol in the ratio of 20:80 % v/v as the mobile phase at a flow rate of 1.0 mL/min. The column effluents were monitored by a photodiode array detector set at 286 nm. The method was validated in terms of specificity, linearity, accuracy, precision, detection limit, quantification limit, and robustness. Forced degradation of etofenamate was carried out under acidic, basic, thermal, photo, and peroxide conditions and the major degradation products of acidic and basic degradation were isolated and characterized by 1H-NMR, 13C-NMR, and mass spectral studies. The mass balance of the method varied between 92–99%. PMID:24482770

Quantitative assessment of the risk of microbial spoilage in foods. Prediction of non-stability at 55 °C caused by Geobacillus stearothermophilus in canned green beans.

PubMed

Rigaux, Clémence; André, Stéphane; Albert, Isabelle; Carlin, Frédéric

2014-02-03

Microbial spoilage of canned foods by thermophilic and highly heat-resistant spore-forming bacteria, such as Geobacillus stearothermophilus, is a persistent problem in the food industry. An incubation test at 55 °C for 7 days, then validation of biological stability, is used as an indicator of compliance with good manufacturing practices. We propose a microbial risk assessment model predicting the percentage of non-stability due to G. stearothermophilus in canned green beans manufactured by a French company. The model accounts for initial microbial contaminations of fresh unprocessed green beans with G. stearothermophilus, cross-contaminations in the processing chain, inactivation processes and probability of survival and growth. The sterilization process is modeled by an equivalent heating time depending on sterilization value F₀ and on G. stearothermophilus resistance parameter z(T). Following the recommendations of international organizations, second order Monte-Carlo simulations are used, separately propagating uncertainty and variability on parameters. As a result of the model, the mean predicted non-stability rate is of 0.5%, with a 95% uncertainty interval of [0.1%; 1.2%], which is highly similar to data communicated by the French industry. A sensitivity analysis based on Sobol indices and some scenario tests underline the importance of cross-contamination at the blanching step, in addition to inactivation due to the sterilization process. Copyright © 2013 Elsevier B.V. All rights reserved.

Flight control optimization from design to assessment application on the Cessna Citation X business aircraft =

NASA Astrophysics Data System (ADS)

Boughari, Yamina

New methodologies have been developed to optimize the integration, testing and certification of flight control systems, an expensive process in the aerospace industry. This thesis investigates the stability of the Cessna Citation X aircraft without control, and then optimizes two different flight controllers from design to validation. The aircraft's model was obtained from the data provided by the Research Aircraft Flight Simulator (RAFS) of the Cessna Citation business aircraft. To increase the stability and control of aircraft systems, optimizations of two different flight control designs were performed: 1) the Linear Quadratic Regulation and the Proportional Integral controllers were optimized using the Differential Evolution algorithm and the level 1 handling qualities as the objective function. The results were validated for the linear and nonlinear aircraft models, and some of the clearance criteria were investigated; and 2) the Hinfinity control method was applied on the stability and control augmentation systems. To minimize the time required for flight control design and its validation, an optimization of the controllers design was performed using the Differential Evolution (DE), and the Genetic algorithms (GA). The DE algorithm proved to be more efficient than the GA. New tools for visualization of the linear validation process were also developed to reduce the time required for the flight controller assessment. Matlab software was used to validate the different optimization algorithms' results. Research platforms of the aircraft's linear and nonlinear models were developed, and compared with the results of flight tests performed on the Research Aircraft Flight Simulator. Some of the clearance criteria of the optimized H-infinity flight controller were evaluated, including its linear stability, eigenvalues, and handling qualities criteria. Nonlinear simulations of the maneuvers criteria were also investigated during this research to assess the Cessna Citation X's flight controller clearance, and therefore, for its anticipated certification.

Ready to rumble: how team personality composition and task conflict interact to improve performance.

PubMed

Bradley, Bret H; Klotz, Anthony C; Postlethwaite, Bennett E; Brown, Kenneth G

2013-03-01

Although prior work has proposed a number of conditions under which task conflict in teams may improve performance, composition variables have been left unexplored. Given the effects of personality traits on team processes and outcomes demonstrated in prior work, investigating whether specific personality compositions influence the effect of task conflict on team performance is critical to researchers' understanding of conflict in teams. Our results indicate that team-level averages of both openness to experience and emotional stability function as moderators of the relationship between task conflict and team performance. Specifically, task conflict had a positive impact on performance in teams with high levels of openness or emotional stability; in contrast, task conflict had a negative impact on performance in teams with low levels of openness or emotional stability. Thus, when task conflict emerges, teams composed of members who are open minded or emotionally stable are best able to leverage conflict to improve performance. Implications for theory and practice are discussed.

Flexible, High-Wettability and Fire-Resistant Separators Based on Hydroxyapatite Nanowires for Advanced Lithium-Ion Batteries.

PubMed

Li, Heng; Wu, Dabei; Wu, Jin; Dong, Li-Ying; Zhu, Ying-Jie; Hu, Xianluo

2017-11-01

Separators play a pivotal role in the electrochemical performance and safety of lithium-ion batteries (LIBs). The commercial microporous polyolefin-based separators often suffer from inferior electrolyte wettability, low thermal stability, and severe safety concerns. Herein, a novel kind of highly flexible and porous separator based on hydroxyapatite nanowires (HAP NWs) with excellent thermal stability, fire resistance, and superior electrolyte wettability is reported. A hierarchical cross-linked network structure forms between HAP NWs and cellulose fibers (CFs) via hybridization, which endows the separator with high flexibility and robust mechanical strength. The high thermal stability of HAP NW networks enables the separator to preserve its structural integrity at temperatures as high as 700 °C, and the fire-resistant property of HAP NWs ensures high safety of the battery. In particular, benefiting from its unique composition and highly porous structure, the as-prepared HAP/CF separator exhibits near zero contact angle with the liquid electrolyte and high electrolyte uptake of 253%, indicating superior electrolyte wettability compared with the commercial polyolefin separator. The as-prepared HAP/CF separator has unique advantages of superior electrolyte wettability, mechanical robustness, high thermal stability, and fire resistance, thus, is promising as a new kind of separator for advanced LIBs with enhanced performance and high safety. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Parameter Stability of the Functional–Structural Plant Model GREENLAB as Affected by Variation within Populations, among Seasons and among Growth Stages

PubMed Central

Ma, Yuntao; Li, Baoguo; Zhan, Zhigang; Guo, Yan; Luquet, Delphine; de Reffye, Philippe; Dingkuhn, Michael

2007-01-01

Background and Aims It is increasingly accepted that crop models, if they are to simulate genotype-specific behaviour accurately, should simulate the morphogenetic process generating plant architecture. A functional–structural plant model, GREENLAB, was previously presented and validated for maize. The model is based on a recursive mathematical process, with parameters whose values cannot be measured directly and need to be optimized statistically. This study aims at evaluating the stability of GREENLAB parameters in response to three types of phenotype variability: (1) among individuals from a common population; (2) among populations subjected to different environments (seasons); and (3) among different development stages of the same plants. Methods Five field experiments were conducted in the course of 4 years on irrigated fields near Beijing, China. Detailed observations were conducted throughout the seasons on the dimensions and fresh biomass of all above-ground plant organs for each metamer. Growth stage-specific target files were assembled from the data for GREENLAB parameter optimization. Optimization was conducted for specific developmental stages or the entire growth cycle, for individual plants (replicates), and for different seasons. Parameter stability was evaluated by comparing their CV with that of phenotype observation for the different sources of variability. A reduced data set was developed for easier model parameterization using one season, and validated for the four other seasons. Key Results and Conclusions The analysis of parameter stability among plants sharing the same environment and among populations grown in different environments indicated that the model explains some of the inter-seasonal variability of phenotype (parameters varied less than the phenotype itself), but not inter-plant variability (parameter and phenotype variability were similar). Parameter variability among developmental stages was small, indicating that parameter values were largely development-stage independent. The authors suggest that the high level of parameter stability observed in GREENLAB can be used to conduct comparisons among genotypes and, ultimately, genetic analyses. PMID:17158141

Simultaneous determination of ten Aconitum alkaloids in rat tissues by UHPLC-MS/MS and its application to a tissue distribution study on the compatibility of Heishunpian and Fritillariae thunbergii Bulbus.

PubMed

Yang, Bin; Xu, Yanyan; Wu, Yuanyuan; Wu, Huanyu; Wang, Yuan; Yuan, Lei; Xie, Jiabin; Li, Yubo; Zhang, Yanjun

2016-10-15

A rapid, sensitive and selective ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for simultaneous determination of ten Aconitum alkaloids in rat tissues. The tissue samples were prepared by a simple procedure protein precipitation with acetonitrile containing 0.1% acetic acid and separated on an Agilent XDB C18 column (4.6 mm×50mm, 1.8μm) using gradient elution with a mobile phase consisting of water and acetonitrile (both containing 0.1% formic acid) at a flow rate of 0.3mL/min. The quantitive determination was performed on an electrospray ionization (ESI) triple quadrupole tandem mass spectrometer using selective reaction monitoring (SRM) under positive ionization mode. The established method was fully validated according to the USA Food and Drug Administration (FDA) bioanalytical method validation guidance and the results demonstrated that the method was sensitive and selective with the lowest limits of quantification (LLOQ) at 0.025ng/mL in rat tissue homogenates. Meanwhile, the linearity, precision, accuracy, extraction recovery, matrix effect and stability were all within the required limits of biological sample analysis. After method validation, the validated method was successfully applied to the tissue distribution study on the compatibility of Heishunpian (HSP, the processed product of Aconitum carmichaelii Debx) and Fritillariae thunbergii Bulbus (Zhebeimu, ZBM). The results indicated that the distribution feature of monoester diterpenoid aconitines (MDAs), diester diterpenoid aconitines (DDAs) and non-ester alkaloids (NEAs) were inconsistency, and the compatibility of HSP and ZBM resulted in the distribution amount of DDAs increased in tissues. What's more, the results could provide the reliable basis for systematic research on the substance foundation of the compatibility of the herbal pair. Copyright © 2016 Elsevier B.V. All rights reserved.

High-temperature Y267 EPDM elastomer: field and laboratory experiences, August 1981

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hirasuna, A.R.; Friese, G.J.; Stephens, C.A.

1982-03-01

Experiences which indicate the superiority of Y267 EPDM elastomer for high-temperature brines and other environments uses are summarized. Its good processing qualities, extremely good thermochemical stability, extremely good mechanical properties, its low-cost constituents, and its good performance in hydrocarbons are described in some case histories. (MCW)

Measuring premorbid IQ in traumatic brain injury: an examination of the validity of the Wechsler Test of Adult Reading (WTAR).

PubMed

Green, Robin E A; Melo, Brenda; Christensen, Bruce; Ngo, Le-Anh; Monette, Georges; Bradbury, Cheryl

2008-02-01

Estimation of premorbid IQ in traumatic brain injury (TBI) is clinically and scientifically valuable because it permits the quantification of the cognitive impact of injury. This is achieved by comparing performances on tests of current ability to estimates of premorbid IQ, thereby enabling current capacity to be interpreted in light of preinjury ability. However, the validity of premorbid IQ tests that are commonly used for TBI has been questioned. In the present study, we examined the psychometric properties of a recently developed test, the Wechsler Test of Adult Reading (WTAR), which has yet to be examined for TBI. The cognitive performance of a group of 24 patients recovering from TBI (with a mean Glasgow Coma Scale score in the severely impaired range) was measured at 2 and 5 months postinjury. On both occasions, patients were administered three tests that have been used to measure premorbid IQ (the WTAR and the Vocabulary and Matrix Reasoning subtests of the Wechsler Adult Intelligence Scale 3rd Edition, WAIS-III) and three tests of current ability (Symbol Digit Modalities Test-Oral and Similarities and Block Design subtests of the WAIS-III). We found that performance significantly improved on tests of current cognitive ability, confirming recovery. In contrast, stable performance was observed on the WTAR from Assessment 1 (M = 34.25/50) to Assessment 2 (M = 34.21/50; r = .970, p < .001). Mean improvement across assessments was negligible (t = -0.086, p = .47; Cohen's d = -.005), and minimal individual participant change was observed (modal scaled score change = 0). WTAR scores were also highly similar to scores on a demographic estimate of premorbid IQ. Thus, converging evidence--high stability during recovery from TBI and similar IQ estimates to those of a demographic equation suggests that the WTAR is a valid measure of premorbid IQ for TBI. Where word pronunciation tests are indicated (i.e., in patients for whom English is spoken and read fluently), these results endorse the use of the WTAR for patients with TBI.

Traceability validation of a high speed short-pulse testing method used in LED production

NASA Astrophysics Data System (ADS)

Revtova, Elena; Vuelban, Edgar Moreno; Zhao, Dongsheng; Brenkman, Jacques; Ulden, Henk

2017-12-01

Industrial processes of LED (light-emitting diode) production include LED light output performance testing. Most of them are monitored and controlled by optically, electrically and thermally measuring LEDs by high speed short-pulse measurement methods. However, these are not standardized and a lot of information is proprietary that it is impossible for third parties, such as NMIs, to trace and validate. It is known, that these techniques have traceability issue and metrological inadequacies. Often due to these, the claimed performance specifications of LEDs are overstated, which consequently results to manufacturers experiencing customers' dissatisfaction and a large percentage of failures in daily use of LEDs. In this research a traceable setup is developed to validate one of the high speed testing techniques, investigate inadequacies and work out the traceability issues. A well-characterised short square pulse of 25 ms is applied to chip-on-board (CoB) LED modules to investigate the light output and colour content. We conclude that the short-pulse method is very efficient in case a well-defined electrical current pulse is applied and the stabilization time of the device is "a priori" accurately determined. No colour shift is observed. The largest contributors to the measurement uncertainty include badly-defined current pulse and inaccurate calibration factor.

Carbohydrate-Assisted Combustion Synthesis To Realize High-Performance Oxide Transistors.

PubMed

Wang, Binghao; Zeng, Li; Huang, Wei; Melkonyan, Ferdinand S; Sheets, William C; Chi, Lifeng; Bedzyk, Michael J; Marks, Tobin J; Facchetti, Antonio

2016-06-08

Owing to high carrier mobilities, good environmental/thermal stability, excellent optical transparency, and compatibility with solution processing, thin-film transistors (TFTs) based on amorphous metal oxide semiconductors (AOSs) are promising alternatives to those based on amorphous silicon (a-Si:H) and low-temperature (<600 °C) poly-silicon (LTPS). However, solution-processed display-relevant indium-gallium-tin-oxide (IGZO) TFTs suffer from low carrier mobilities and/or inferior bias-stress stability versus their sputtered counterparts. Here we report that three types of environmentally benign carbohydrates (sorbitol, sucrose, and glucose) serve as especially efficient fuels for IGZO film combustion synthesis to yield high-performance TFTs. The results indicate that these carbohydrates assist the combustion process by lowering the ignition threshold temperature and, for optimal stoichiometries, enhancing the reaction enthalpy. IGZO TFT mobilities are increased to >8 cm(2) V(-1) s(-1) on SiO2/Si gate dielectrics with significantly improved bias-stress stability. The first correlations between precursor combustion enthalpy and a-MO densification/charge transport are established.

Examination of the Psychometric Properties of the Adult Manifest Anxiety Scale-Elderly Version Scores

ERIC Educational Resources Information Center

Lowe, Patricia A.; Reynolds, Cecil R.

2006-01-01

The psychometric properties of the Adult Manifest Anxiety Scale-Elderly Version (AMAS-E) scores were evaluated in two studies. In Study 1, the temporal stability and construct validity of the AMAS-E test scores were examined in a group of 226 older adults, aged 60 years and older. Results indicated adequate to excellent temporal stability (2-week…

EO-1 Hyperion reflectance time series at calibration and validation sites: stability and sensitivity to seasonal dynamics

Treesearch

Petya K. Entcheva Campbell; Elizabeth M. Middleton; Kurt J. Thome; Raymond F. Kokaly; Karl Fred Huemmrich; David Lagomasino; Kimberly A. Novick; Nathaniel A. Brunsell

2013-01-01

This study evaluated Earth Observing 1 (EO-1) Hyperion reflectance time series at established calibration sites to assess the instrument stability and suitability for monitoring vegetation functional parameters. Our analysis using three pseudo-invariant calibration sites in North America indicated that the reflectance time series are devoid of apparent spectral trends...

The relationship between organizational trust and nurse administrators’ productivity in hospitals

PubMed Central

Bahrami, Susan; Hasanpour, Marzieh; Rajaeepour, Saeed; Aghahosseni, Taghi; Hodhodineghad, Nilofar

2012-01-01

Context: Management of health care organizations based on employee’s mutual trust will increase the improvement in functions and tasks. Aims: The present study was performed to investigate the relationship between organizational trust and the nurse administrators’ productivity in educational health centers of in Health-Education Centers of Isfahan University of Medical Sciences. Settings and Design: This research was a descriptive and correlational study. Materials and Methods: The population included all nurse administrators. In this research, 165 nurses were selected through random sampling method. Data collection instruments were organizational trust questionnaire based on Robbins’s model and productivity questionnaire based on Hersy and Blanchard’s model. Validity of these questionnaires was determined through content validity and their reliability was calculated through Cranach’s alpha. Statistical analysis was used: The data analysis was done using the SPSS (18) statistical software. Results: The indicators of organizational trust such as loyalty, competence, honesty, and stability were more than average level but explicitness indicator was at average level. The components of productivity such as ability, job knowledge, environmental compatibility, performance feedback, and validity were more than average level but motivation factor was at average level and organizational support was less than average level. There were a significant multiple correlations between organizational trust and productivity. Beta coefficients among organizational trust and productivity were significant and no autocorrelation existed and regression model was significant. Conclusions: Committed employees, timely performing the tasks and developing the sense of responsibility among employees can enhance production and productivity in the health care organizations. PMID:23922588

Development of an extemporaneous oral liquid formulation of oxandrolone and its stability evaluation.

PubMed

Garg, Alka; Garg, Sanjay; She, Richard Wong

2011-11-01

Many references exist in the literature identifying the usefulness of oxandrolone in treating muscle wasting due to various conditions including severe burns. However, there is an absence of dosage form alternatives as it is only available as tablets. The dose for children is weight based (0.1 mg/kg) which is difficult to achieve with the currently available tablets of 2.5 mg and 10 mg. The literature provides ample evidence of clinical importance but little guidance on extemporaneous oral liquid formulation of oxandrolone. In order to develop and validate an extemporaneous liquid formulation, suspensions of oxandrolone were developed using locally available (New Zealand) vehicles. Combinations of these vehicles with ethanol, as advised in some articles were also tried. Assay method was developed for oxandrolone using High Performance Liquid Chromatography (HPLC) and Mass Spectroscopy (LC-MS). The formulations were evaluated for stability as per the International Conference on Harmonization (ICH) stability guidelines. They were observed for physical and chemical stability at different time points over a period of 28 days. A stable and validated liquid formulation of oxandrolone has been developed which can be made under the hospital and community pharmacy conditions. The formula utilises commercially available oxandrolone tablets, crushed and dispersed in Simple Syrup BP or Orablend(®) vehicle. The formulation has confirmed stability for 21 days and can be easily made with locally available vehicles. Copyright © 2011 Elsevier Ltd and ISBI. All rights reserved.

Development and validation of a high throughput assay for the quantification of multiple green tea-derived catechins in human plasma.

PubMed

Mawson, Deborah H; Jeffrey, Keon L; Teale, Philip; Grace, Philip B

2018-06-19

A rapid, accurate and robust method for the determination of catechin (C), epicatechin (EC), gallocatechin (GC), epigallocatechin (EGC), catechin gallate (Cg), epicatechin gallate (ECg), gallocatechin gallate (GCg) and epigallocatechin gallate (EGCg) concentrations in human plasma has been developed. The method utilises protein precipitation following enzyme hydrolysis, with chromatographic separation and detection using reversed-phase liquid chromatography - tandem mass spectrometry (LC-MS/MS). Traditional issues such as lengthy chromatographic run times, sample and extract stability, and lack of suitable internal standards have been addressed. The method has been evaluated using a comprehensive validation procedure, confirming linearity over appropriate concentration ranges, and inter/intra batch precision and accuracies within suitable thresholds (precisions within 13.8% and accuracies within 12.4%). Recoveries of analytes were found to be consistent between different matrix samples, compensated for using suitable internal markers and within the performance of the instrumentation used. Similarly, chromatographic interferences have been corrected using the internal markers selected. Stability of all analytes in matrix is demonstrated over 32 days and throughout extraction conditions. This method is suitable for high throughput sample analysis studies. This article is protected by copyright. All rights reserved.

A high-performance liquid chromatography method for the serotonin release assay is equivalent to the radioactive method.

PubMed

Sono-Koree, N K; Crist, R A; Frank, E L; Rodgers, G M; Smock, K J

2016-02-01

The serotonin release assay (SRA) is considered the gold standard laboratory test for heparin-induced thrombocytopenia (HIT). The historic SRA method uses platelets loaded with radiolabeled serotonin to evaluate platelet activation by HIT immune complexes. However, a nonradioactive method is desirable. We report the performance characteristics of a high-performance liquid chromatography (HPLC) SRA method. We validated the performance characteristics of an HPLC-SRA method, including correlation with a reference laboratory using the radioactive method. Serotonin released from reagent platelets was quantified by HPLC using fluorescent detection. Results were expressed as % release and classified as positive, negative, or indeterminate based on previously published cutoffs. Serum samples from 250 subjects with suspected HIT were tested in the HPLC-SRA and with the radioactive method. Concordant classifications were observed in 230 samples (92%). Sera from 41 healthy individuals tested negative. Between-run imprecision studies showed standard deviation of <6 (% release) for positive, weak positive, and negative serum pools. Stability studies demonstrated stability after two freeze-thaw cycles or up to a week of refrigeration. The HPLC-SRA has robust performance characteristics, equivalent to the historic radioactive method, but avoids the complexities of working with radioactivity. © 2015 John Wiley & Sons Ltd.

Investigation of arterial gas occlusions. [effect of noncondensable gases on high performance heat pipes

NASA Technical Reports Server (NTRS)

Saaski, E. W.

1974-01-01

The effect of noncondensable gases on high-performance arterial heat pipes was investigated both analytically and experimentally. Models have been generated which characterize the dissolution of gases in condensate, and the diffusional loss of dissolved gases from condensate in arterial flow. These processes, and others, were used to postulate stability criteria for arterial heat pipes under isothermal and non-isothermal condensate flow conditions. A rigorous second-order gas-loaded heat pipe model, incorporating axial conduction and one-dimensional vapor transport, was produced and used for thermal and gas studies. A Freon-22 (CHCIF2) heat pipe was used with helium and xenon to validate modeling. With helium, experimental data compared well with theory. Unusual gas-control effects with xenon were attributed to high solubility.

A Malay version of the Child Oral Impacts on Daily Performances (Child-OIDP) index: assessing validity and reliability.

PubMed

Yusof, Zamros Y M; Jaafar, Nasruddin

2012-06-08

The study aimed to develop and test a Malay version of the Child-OIDP index, evaluate its psychometric properties and report on the prevalence of oral impacts on eight daily performances in a sample of 11-12 year old Malaysian schoolchildren. The Child-OIDP index was translated from English into Malay. The Malay version was tested for reliability and validity on a non-random sample of 132, 11-12 year old schoolchildren from two urban schools in Kuala Lumpur. Psychometric analysis of the Malay Child-OIDP involved face, content, criterion and construct validity tests as well as internal and test-retest reliability. Non-parametric statistical methods were used to assess relationships between Child-OIDP scores and other subjective outcome measures. The standardised Cronbach's alpha was 0.80 and the weighted Kappa was 0.84 (intraclass correlation = 0.79). The index showed significant associations with different subjective measures viz. perceived satisfaction with mouth, perceived needs for dental treatment, perceived oral health status and toothache experience in the previous 3 months (p < 0.05). Two-thirds (66.7%) of the sample had oral impacts affecting one or more performances in the past 3 months. The three most frequently affected performances were cleaning teeth (36.4%), eating foods (34.8%) and maintaining emotional stability (26.5%). In terms of severity of impact, the ability to relax was most severely affected by their oral conditions, followed by ability to socialise and doing schoolwork. Almost three-quarters (74.2%) of schoolchildren with oral impacts had up to three performances affected by their oral conditions. This study indicated that the Malay Child-OIDP index is a valid and reliable instrument to measure the oral impacts of daily performances in 11-12 year old urban schoolchildren in Malaysia.

The controlling mechanism for potential loss in CH 3NH 3PbBr 3 hybrid solar cells

DOE PAGES

Zheng, Xiaojia; Chen, Bo; Yang, Mengjin; ...

2016-07-25

In this study, we investigated moisture and thermal stability of MAPbBr 3 perovskite material. Cubic MAPbBr 3 was found to be moisture-insensitive and can avoid the thermal stability issues introduced by low-temperature phase transition in MAPbI 3. MAPbBr 3 and MAPbI 3 hybrid solar cells with efficiencies of ~7.1% and ~15.5%, respectively, were fabricated, and we identified the correlation between the working temperature, light intensity, and the photovoltaic performance. No charge-carrier transport barriers were found in the MAPbBr 3 and MAPbI 3 solar cells. The MAPbBr 3 solar cell displays a better stability under high working temperature because of itsmore » close-packed crystal structure. Temperature-dependent photocurrent-voltage characteristics indicate that, unlike the MAPbI 3 solar cell with an activation energy (E A) nearly equal to its band gap (E g), the E A for the MAPbBr 3 solar cell is much lower than its E g. This indicates that a high interface recombination process limits the photovoltage and consequently the device performance of the MAPbBr 3 solar cell.« less

High-Contrast Coronagraph Performance in the Presence of DM Actuator Defects

NASA Technical Reports Server (NTRS)

Sidick, Erkin; Shaklan, Stuart; Cady, Eric

2015-01-01

Deformable Mirrors (DMs) are critical elements in high contrast coronagraphs, requiring precision and stability measured in picometers to enable detection of Earth-like exoplanets. Occasionally DM actuators or their associated cables or electronics fail, requiring a wavefront control algorithm to compensate for actuators that may be displaced from their neighbors by hundreds of nanometers. We have carried out experiments on our High-Contrast Imaging Testbed (HCIT) to study the impact of failed actuators in partial fulfillment of the Terrestrial Planet Finder Coronagraph optical model validation milestone. We show that the wavefront control algorithm adapts to several broken actuators and maintains dark-hole contrast in broadband light.

High-contrast coronagraph performance in the presence of DM actuator defects

NASA Astrophysics Data System (ADS)

Sidick, Erkin; Shaklan, Stuart; Cady, Eric

2015-09-01

Deformable Mirrors (DMs) are critical elements in high contrast coronagraphs, requiring precision and stability measured in picometers to enable detection of Earth-like exoplanets. Occasionally DM actuators or their associated cables or electronics fail, requiring a wavefront control algorithm to compensate for actuators that may be displaced from their neighbors by hundreds of nanometers. We have carried out experiments on our High-Contrast Imaging Testbed (HCIT) to study the impact of failed actuators in partial fulfilment of the Terrestrial Planet Finder Coronagraph optical model validation milestone. We show that the wavefront control algorithm adapts to several broken actuators and maintains dark-hole contrast in broadband light.

Development and Validation of a Stability-indicating Reversed-phase UPLC-UV Method for the Assay of Imidacloprid and Estimation of its Related Compounds.

PubMed

Tian, Jingzhi; Rustum, Abu

2018-02-01

Imidacloprid is used as an active pharmaceutical ingredient (API) in veterinary drugs to control fleas and ticks for dogs and cats. Here we are reporting for the first time a validated stability-indicating reversed-phase UPLC-UV method for the assay of imidacloprid and estimation of its related compounds. The stability-indicating capability of this method has been demonstrated by a forced degradation study. All related compounds including processing impurities, imidacloprid API and degradates from stressed samples were well separated from each other. Structures of major degradates from forced degradation study were elucidated through UPLC-MS/MS and key degradation pathways were proposed from the proposed chemical structures of major degradates. The UPLC-UV method is carried out using an HSS T3 column (C18, 2.1 × 30 mm, 1.8 μm particle size) maintained at 30°C with mobile phase A (0.05% v/v of phosphoric acid in water) and mobile phase B (methanol/acetonitrile 75/25 v/v). Analytes are separated by a gradient elution and detected at 270 nm. The UPLC method is green and fast with only 6.5 min run time and about 3.5 ml mobile phase consumption for each sample analysis. The UPLC-UV method was validated according to ICH guidelines. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Validation of a stability-indicating hydrophilic interaction liquid chromatographic method for the quantitative determination of vitamin k3 (menadione sodium bisulfite) in injectable solution formulation.

PubMed

Ghanem, Mashhour M; Abu-Lafi, Saleh A; Hallak, Hussein O

2013-01-01

A simple, specific, accurate, and stability-indicating method was developed and validated for the quantitative determination of menadione sodium bisulfite in the injectable solution formulation. The method is based on zwitterionic hydrophilic interaction liquid chromatography (ZIC-HILIC) coupled with a photodiode array detector. The desired separation was achieved on the ZIC-HILIC column (250 mm × 4.6 mm, 5 μm) at 25°C temperature. The optimized mobile phase consisted of an isocratic solvent mixture of 200mM ammonium acetate (NH4AC) solution and acetonitrile (ACN) (20:80; v/v) pH-adjusted to 5.7 by glacial acetic acid. The mobile phase was fixed at 0.5 ml/min and the analytes were monitored at 261 nm using a photodiode array detector. The effects of the chromatographic conditions on the peak retention, peak USP tailing factor, and column efficiency were systematically optimized. Forced degradation experiments were carried out by exposing menadione sodium bisulfite standard and the injectable solution formulation to thermal, photolytic, oxidative, and acid-base hydrolytic stress conditions. The degradation products were well-resolved from the main peak and the excipients, thus proving that the method is a reliable, stability-indicating tool. The method was validated as per ICH and USP guidelines (USP34/NF29) and found to be adequate for the routine quantitative estimation of menadione sodium bisulfite in commercially available menadione sodium bisulfite injectable solution dosage forms.

Facultative Stabilization Pond: Measuring Biological Oxygen Demand using Mathematical Approaches

NASA Astrophysics Data System (ADS)

Wira S, Ihsan; Sunarsih, Sunarsih

2018-02-01

Pollution is a man-made phenomenon. Some pollutants which discharged directly to the environment could create serious pollution problems. Untreated wastewater will cause contamination and even pollution on the water body. Biological Oxygen Demand (BOD) is the amount of oxygen required for the oxidation by bacteria. The higher the BOD concentration, the greater the organic matter would be. The purpose of this study was to predict the value of BOD contained in wastewater. Mathematical modeling methods were chosen in this study to depict and predict the BOD values contained in facultative wastewater stabilization ponds. Measurements of sampling data were carried out to validate the model. The results of this study indicated that a mathematical approach can be applied to predict the BOD contained in the facultative wastewater stabilization ponds. The model was validated using Absolute Means Error with 10% tolerance limit, and AME for model was 7.38% (< 10%), so the model is valid. Furthermore, a mathematical approach can also be applied to illustrate and predict the contents of wastewater.

Edge Stabilized Ribbon (ESR); Stress, Dislocation Density and Electronic Performance

NASA Technical Reports Server (NTRS)

Sachs, E. M.

1984-01-01

The edge stabilized ribbon (ESR) silicon ribbon was grown in widths of 1, 2.2 and 4.0 inches at speeds ranging from .6 to 7 in/min, which result in ribbon thicknesses of 5 to 400 microns. One of the primary problems remaining in ESR growth is that of thermally induced mechanical stresses. This problem is manifested as ribbon with a high degree of residual stress or as ribbon with buckled ribbon. Thermal stresses result in a high dislocation density in the grown material, resulting in compromised electronic performance. Improvements in ribbon flatness were accomplished by modification of the ribbon cooling profile. Ribbon flatness and other experimental observations of ESR ribbon are discussed. Laser scanner measurements show a good correlation between diffusion length and dislocation density which indicates that the high dislocation densities are the primary cause of the poor current performance of ESR materials. Dislocation densities were reduced and improved electronic performance resulted. Laser scanner data on new and old material are presented.

A comparative study between three stability indicating spectrophotometric methods for the determination of diatrizoate sodium in presence of its cytotoxic degradation product based on two-wavelength selection

NASA Astrophysics Data System (ADS)

Riad, Safaa M.; El-Rahman, Mohamed K. Abd; Fawaz, Esraa M.; Shehata, Mostafa A.

2015-06-01

Three sensitive, selective, and precise stability indicating spectrophotometric methods for the determination of the X-ray contrast agent, diatrizoate sodium (DTA) in the presence of its acidic degradation product (highly cytotoxic 3,5-diamino metabolite) and in pharmaceutical formulation, were developed and validated. The first method is ratio difference, the second one is the bivariate method, and the third one is the dual wavelength method. The calibration curves for the three proposed methods are linear over a concentration range of 2-24 μg/mL. The selectivity of the proposed methods was tested using laboratory prepared mixtures. The proposed methods have been successfully applied to the analysis of DTA in pharmaceutical dosage forms without interference from other dosage form additives. The results were statistically compared with the official US pharmacopeial method. No significant difference for either accuracy or precision was observed.

A comparative study between three stability indicating spectrophotometric methods for the determination of diatrizoate sodium in presence of its cytotoxic degradation product based on two-wavelength selection.

PubMed

Riad, Safaa M; El-Rahman, Mohamed K Abd; Fawaz, Esraa M; Shehata, Mostafa A

2015-06-15

Three sensitive, selective, and precise stability indicating spectrophotometric methods for the determination of the X-ray contrast agent, diatrizoate sodium (DTA) in the presence of its acidic degradation product (highly cytotoxic 3,5-diamino metabolite) and in pharmaceutical formulation, were developed and validated. The first method is ratio difference, the second one is the bivariate method, and the third one is the dual wavelength method. The calibration curves for the three proposed methods are linear over a concentration range of 2-24 μg/mL. The selectivity of the proposed methods was tested using laboratory prepared mixtures. The proposed methods have been successfully applied to the analysis of DTA in pharmaceutical dosage forms without interference from other dosage form additives. The results were statistically compared with the official US pharmacopeial method. No significant difference for either accuracy or precision was observed. Copyright © 2015 Elsevier B.V. All rights reserved.

Comparative study of a novel application of automated HR HPV assay and stability in a previously untested Preservative media.

PubMed

Morel, Mike E; McBride, Simon E; Gomez, Maria P

2017-12-01

The suitability and stability of cervical cells in Novaprep media (NHQ) for certain HPV assays is unknown. We evaluated the accuracy of an automated HPV assay (Abbott RealTime HR HPV) for cervical cells prepared in NHQ and NHQ with a pre-treatment to mimic a worst case clinical use, compared to the assay manufacturers media; repeatability and reproducibility of HPV results and the stability of detectable HPV in NHQ over time compared to CE marked liquid based cytology preservatives. Cell lines were used to simulate patient samples. Cells stored in NHQ produced accurate, repeatable and reproducible results. Stability in NHQ was comparable to the best performing LBC, with at least 7 months' stability at 18-25°C, 2-8°C, -20°C and -80°C; and at least 3 months' stability at 40°C. Similar results were obtained for pre-treated NHQ except only 3.5 months' stability at 18-25°C. Cell line samples in all media and concentrations tested were detected appropriately by the assay. Based on this first stage validation analytical study, cervical cells stored in NHQ are suitable for the Realtime HPV assay. There should be no reservations for inclusion of NHQ in any further validation and clinical performance evaluation of this assay. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

Stability indicating validated HPLC method for quantification of levothyroxine with eight degradation peaks in the presence of excipients.

PubMed

Shah, R B; Bryant, A; Collier, J; Habib, M J; Khan, M A

2008-08-06

A simple, sensitive, accurate, and robust stability indicating analytical method is presented for identification, separation, and quantitation of l-thyroxine and eight degradation impurities with an internal standard. The method was used in the presence of commonly used formulation excipients such as butylated hydroxyanisole, povidone, crospovidone, croscarmellose sodium, mannitol, sucrose, acacia, lactose monohydrate, confectionary sugar, microcrystalline cellulose, sodium laurel sulfate, magnesium stearate, talc, and silicon dioxide. The two active thyroid hormones: 3,3',5,5'-tetra-iodo-l-thyronine (l-thyroxine-T4) and 3,3',5-tri-iodo-l-thyronine (T3) and degradation products including di-iodothyronine (T2), thyronine (T0), tyrosine (Tyr), di-iodotyrosine (DIT), mono-iodotyrosine (MIT), 3,3',5,5'-tetra-iodothyroacetic acid (T4AA) and 3,3',5-tri-iodothyroacetic acid (T3AA) were assayed by the current method. The separation of l-thyroxine and eight metabolites along with theophylline (internal standard) was achieved using a C18 column (25 degrees C) with a mobile phase of trifluoroacetic acid (0.1%, v/v, pH 3)-acetonitrile in gradient elution at 0.8 ml/min at 223 nm. The sample diluent was 0.01 M methanolic NaOH. Method was validated according to FDA, USP, and ICH guidelines for inter-day accuracy, precision, and robustness after checking performance with system suitability. Tyr (4.97 min), theophylline (9.09 min), MIT (9.55 min), DIT (11.37 min), T0 (11.63 min), T2 (14.47 min), T3 (16.29 min), T4 (17.60 min), T3AA (22.71 min), and T4AA (24.83 min) separated in a single chromatographic run. Linear relationship (r2>0.99) was observed between the peak area ratio and the concentrations for all of the compounds within the range of 2-20 microg/ml. The total time for analysis, equilibration and recovery was 40 min. The method was shown to separate well from commonly employed formulation excipients. Accuracy ranged from 95 to 105% for T4 and 90 to 110% for all other compounds. Precision was <2% for all the compounds. The method was found to be robust with minor changes in injection volume, flow rate, column temperature, and gradient ratio. Validation results indicated that the method shows satisfactory linearity, precision, accuracy, and ruggedness and also stress degradation studies indicated that the method can be used as stability indicating method for l-thyroxine in the presence of excipients.

An investigation of new toxicity test method performance in validation studies: 1. Toxicity test methods that have predictive capacity no greater than chance.

PubMed

Bruner, L H; Carr, G J; Harbell, J W; Curren, R D

2002-06-01

An approach commonly used to measure new toxicity test method (NTM) performance in validation studies is to divide toxicity results into positive and negative classifications, and the identify true positive (TP), true negative (TN), false positive (FP) and false negative (FN) results. After this step is completed, the contingent probability statistics (CPS), sensitivity, specificity, positive predictive value (PPV), and negative predictive value (NPV) are calculated. Although these statistics are widely used and often the only statistics used to assess the performance of toxicity test methods, there is little specific guidance in the validation literature on what values for these statistics indicate adequate performance. The purpose of this study was to begin developing data-based answers to this question by characterizing the CPS obtained from an NTM whose data have a completely random association with a reference test method (RTM). Determining the CPS of this worst-case scenario is useful because it provides a lower baseline from which the performance of an NTM can be judged in future validation studies. It also provides an indication of relationships in the CPS that help identify random or near-random relationships in the data. The results from this study of randomly associated tests show that the values obtained for the statistics vary significantly depending on the cut-offs chosen, that high values can be obtained for individual statistics, and that the different measures cannot be considered independently when evaluating the performance of an NTM. When the association between results of an NTM and RTM is random the sum of the complementary pairs of statistics (sensitivity + specificity, NPV + PPV) is approximately 1, and the prevalence (i.e., the proportion of toxic chemicals in the population of chemicals) and PPV are equal. Given that combinations of high sensitivity-low specificity or low specificity-high sensitivity (i.e., the sum of the sensitivity and specificity equal to approximately 1) indicate lack of predictive capacity, an NTM having these performance characteristics should be considered no better for predicting toxicity than by chance alone.

Experiments study on attitude coupling control method for flexible spacecraft

NASA Astrophysics Data System (ADS)

Wang, Jie; Li, Dongxu

2018-06-01

High pointing accuracy and stabilization are significant for spacecrafts to carry out Earth observing, laser communication and space exploration missions. However, when a spacecraft undergoes large angle maneuver, the excited elastic oscillation of flexible appendages, for instance, solar wing and onboard antenna, would downgrade the performance of the spacecraft platform. This paper proposes a coupling control method, which synthesizes the adaptive sliding mode controller and the positive position feedback (PPF) controller, to control the attitude and suppress the elastic vibration simultaneously. Because of its prominent performance for attitude tracking and stabilization, the proposed method is capable of slewing the flexible spacecraft with a large angle. Also, the method is robust to parametric uncertainties of the spacecraft model. Numerical simulations are carried out with a hub-plate system which undergoes a single-axis attitude maneuver. An attitude control testbed for the flexible spacecraft is established and experiments are conducted to validate the coupling control method. Both numerical and experimental results demonstrate that the method discussed above can effectively decrease the stabilization time and improve the attitude accuracy of the flexible spacecraft.

A New Symptom Model for Autism Cross-Validated in an Independent Sample

ERIC Educational Resources Information Center

Boomsma, A.; Van Lang, N. D. J.; De Jonge, M. V.; De Bildt, A. A.; Van Engeland, H.; Minderaa, R. B.

2008-01-01

Background: Results from several studies indicated that a symptom model other than the DSM triad might better describe symptom domains of autism. The present study focused on a) investigating the stability of a new symptom model for autism by cross-validating it in an independent sample and b) examining the invariance of the model regarding three…

Thermal Testing and Analysis of an Efficient High-Temperature Multi-Screen Internal Insulation

NASA Technical Reports Server (NTRS)

Weiland, Stefan; Handrick, Karin; Daryabeigi, Kamran

2007-01-01

Conventional multi-layer insulations exhibit excellent insulation performance but they are limited to the temperature range to which their components reflective foils and spacer materials are compatible. For high temperature applications, the internal multi-screen insulation IMI has been developed that utilizes unique ceramic material technology to produce reflective screens with high temperature stability. For analytical insulation sizing a parametric material model is developed that includes the main contributors for heat flow which are radiation and conduction. The adaptation of model-parameters based on effective steady-state thermal conductivity measurements performed at NASA Langley Research Center (LaRC) allows for extrapolation to arbitrary stack configurations and temperature ranges beyond the ones that were covered in the conductivity measurements. Experimental validation of the parametric material model was performed during the thermal qualification test of the X-38 Chin-panel, where test results and predictions showed a good agreement.

Optical mounts for harsh environments

NASA Astrophysics Data System (ADS)

Mimovich, Mark E.; Griffee, Jonathan C.; Goodding, James C.

2009-08-01

Development and testing of a lightweight-kinematic optical mount with integrated passive vibration-and-shock mitigation technologies and simple / robust optical alignment functionality is presented. Traditionally, optical mounts are designed for use in laboratory environments where the thermal-mechanical environments are carefully controlled to preserve beam path conditions and background disturbances are minimized to facilitate precise optically based measurements. Today's weapon and surveillance systems, however, have optical sensor suites where static and dynamic alignment performance in the presence of harsh operating environments is required to nearly the same precision and where the system cannot afford the mass of laboratory-grade stabilized mounting systems. Jitter and alignment stability is particularly challenging for larger optics operating within moving vehicles and aircraft where high shock and significant temperature excursions occur. The design intent is to have the mount be suitable for integration into existing defense and security optical systems while also targeting new commercial and military components for improved structural dynamic and thermal distortion performance. A mount suitable for moderate-sized optics and an integrated disturbance-optical metrology system are described. The mount design has performance enhancements derived from the integration of proven aerospace mechanical vibration and shock mitigation technologies (i.e. multi-axis passive isolation and integral damping), precision alignment adjustment and lock-out functionality, high dimensional stability materials and design practices which provide benign optical surface figure errors under harsh thermal-mechanical loading. Optical jitter, alignment, and wave-front performance testing of an eight-inch-aperture optical mount based on this design approach are presented to validate predicted performance improvements over an existing commercial off-the-shelf (COTS) design.

Changes in the Balance Performance of Polish Recreational Skiers after Seven Days of Alpine Skiing

PubMed Central

Wojtyczek, Beata; Pasławska, Małgorzata; Raschner, Christian

2014-01-01

Alpine skiing is one of the most popular leisure time winter sporting activities. Skiing imposes high requirements concerning physical fitness, particularly regarding balance abilities. The main objective of this study was to evaluate the changes in balance performance of recreational skiers after a seven-day ski camp. A total of 78 students - 24 women and 54 men - participated in the study. The ski course was held in accordance with the official program of the Polish Ski Federation. The study sample was comprised of 43 beginners and 35 intermediate skiers. All students were tested with the MFT S3-Check, the day before and the day after the ski camp. The test system consisted of an unstable uniaxial platform, with an integrated sensor and corresponding software. Changes in balance performance (sensory and stability index) were evaluated using paired t-tests. Additionally, changes in sensory and stability categories, which were based on the norm data, were analyzed. Female and male participants showed significantly better sensory and stability indices after skiing. Considerable changes from weak or very weak to average or good balance categories could be seen after skiing for both sexes. Regarding skiing experience, both beginners and intermediate skiers improved their sensory and stability indices significantly after skiing. Hence, recreational alpine skiing resulted in better balance performance regardless of sex or skiing experience. Skiing as an outdoor activity offers the opportunity to improve balance performance with a positive impact on everyday life activities. PMID:25713663

Changes in the balance performance of polish recreational skiers after seven days of alpine skiing.

PubMed

Wojtyczek, Beata; Pasławska, Małgorzata; Raschner, Christian

2014-12-09

Alpine skiing is one of the most popular leisure time winter sporting activities. Skiing imposes high requirements concerning physical fitness, particularly regarding balance abilities. The main objective of this study was to evaluate the changes in balance performance of recreational skiers after a seven-day ski camp. A total of 78 students - 24 women and 54 men - participated in the study. The ski course was held in accordance with the official program of the Polish Ski Federation. The study sample was comprised of 43 beginners and 35 intermediate skiers. All students were tested with the MFT S3-Check, the day before and the day after the ski camp. The test system consisted of an unstable uniaxial platform, with an integrated sensor and corresponding software. Changes in balance performance (sensory and stability index) were evaluated using paired t-tests. Additionally, changes in sensory and stability categories, which were based on the norm data, were analyzed. Female and male participants showed significantly better sensory and stability indices after skiing. Considerable changes from weak or very weak to average or good balance categories could be seen after skiing for both sexes. Regarding skiing experience, both beginners and intermediate skiers improved their sensory and stability indices significantly after skiing. Hence, recreational alpine skiing resulted in better balance performance regardless of sex or skiing experience. Skiing as an outdoor activity offers the opportunity to improve balance performance with a positive impact on everyday life activities.

Experimental and Numerical Optimization of a High-Lift System to Improve Low-Speed Performance, Stability, and Control of an Arrow-Wing Supersonic Transport

NASA Technical Reports Server (NTRS)

Hahne, David E.; Glaab, Louis J.

1999-01-01

An investigation was performed to evaluate leading-and trailing-edge flap deflections for optimal aerodynamic performance of a High-Speed Civil Transport concept during takeoff and approach-to-landing conditions. The configuration used for this study was designed by the Douglas Aircraft Company during the 1970's. A 0.1-scale model of this configuration was tested in the Langley 30- by 60-Foot Tunnel with both the original leading-edge flap system and a new leading-edge flap system, which was designed with modem computational flow analysis and optimization tools. Leading-and trailing-edge flap deflections were generated for the original and modified leading-edge flap systems with the computational flow analysis and optimization tools. Although wind tunnel data indicated improvements in aerodynamic performance for the analytically derived flap deflections for both leading-edge flap systems, perturbations of the analytically derived leading-edge flap deflections yielded significant additional improvements in aerodynamic performance. In addition to the aerodynamic performance optimization testing, stability and control data were also obtained. An evaluation of the crosswind landing capability of the aircraft configuration revealed that insufficient lateral control existed as a result of high levels of lateral stability. Deflection of the leading-and trailing-edge flaps improved the crosswind landing capability of the vehicle considerably; however, additional improvements are required.

The Stability and Validity of Automated Vocal Analysis in Preverbal Preschoolers With Autism Spectrum Disorder

PubMed Central

Woynaroski, Tiffany; Oller, D. Kimbrough; Keceli-Kaysili, Bahar; Xu, Dongxin; Richards, Jeffrey A.; Gilkerson, Jill; Gray, Sharmistha; Yoder, Paul

2017-01-01

Theory and research suggest that vocal development predicts “useful speech” in preschoolers with autism spectrum disorder (ASD), but conventional methods for measurement of vocal development are costly and time consuming. This longitudinal correlational study examines the reliability and validity of several automated indices of vocalization development relative to an index derived from human coded, conventional communication samples in a sample of preverbal preschoolers with ASD. Automated indices of vocal development were derived using software that is presently “in development” and/or only available for research purposes and using commercially available Language ENvironment Analysis (LENA) software. Indices of vocal development that could be derived using the software available for research purposes: (a) were highly stable with a single day-long audio recording, (b) predicted future spoken vocabulary to a degree that was nonsignificantly different from the index derived from conventional communication samples, and (c) continued to predict future spoken vocabulary even after controlling for concurrent vocabulary in our sample. The score derived from standard LENA software was similarly stable, but was not significantly correlated with future spoken vocabulary. Findings suggest that automated vocal analysis is a valid and reliable alternative to time intensive and expensive conventional communication samples for measurement of vocal development of preverbal preschoolers with ASD in research and clinical practice. PMID:27459107

[Simultaneous determination of 9 ultraviolet stabilizers in food plastic packaging materials by solid phase extraction-high performance liquid chromatography].

PubMed

Zhang, Juzhou; Li, Jing; Shao, Dongliang; Yao, Bangben; Jiang, Junshu

2012-02-01

An effective high performance liquid chromatographic (HPLC) method has been developed for the simultaneous determination of 9 ultraviolet stabilizers in food plastic packaging materials. The food packaging samples were firstly extracted by methanol-ethyl acetate, and then purified by a C18 solid-phase extraction (SPE) column. The target compounds were separated on a ZORBAX SB-C18 column (250 mm x 4.6 mm, 5 microm) in gradient elution mode using methanol and water as mobile phases. The detection wavelength was at 310 nm. The linear plots of the nine ultraviolet stabilizers were obtained between 0.2 and 10 mg/L, with the correlation coefficients of above 0. 999 for the nine ultraviolet stabilizers. The limits of detection for this method were in the range from 0.05 to 0.1 mg/L. The recoveries spiked in commercial food plastic packaging materials were in the range of 70.2% - 89.0% with the relative standard deviations of 0.4% - 4.5%. The results indicated that the method is simple, accurate, and suitable for the simultaneous determination of the nine ultraviolet stabilizers in food plastic packaging materials.

Modeling and optimization of lime-based stabilization in high alkaline arsenic-bearing sludges with a central composite design.

PubMed

Lei, Jie; Peng, Bing; Min, Xiaobo; Liang, Yanjie; You, Yang; Chai, Liyuan

2017-04-16

This study focuses on the modeling and optimization of lime-based stabilization in high alkaline arsenic-bearing sludges (HAABS) and describes the relationship between the arsenic leachate concentration (ALC) and stabilization parameters to develop a prediction model for obtaining the optimal process parameters and conditions. A central composite design (CCD) along with response surface methodology (RSM) was conducted to model and investigate the stabilization process with three independent variables: the Ca/As mole ratio, reaction time and liquid/solid ratio, along with their interactions. The obvious characteristic changes of the HAABS before and after stabilization were verified by X-ray diffraction (XRD), scanning electron microscopy (SEM), particle size distribution (PSD) and the community bureau of reference (BCR) sequential extraction procedure. A prediction model Y (ALC) with a statistically significant P-value <0.01 and high correlation coefficient R 2 = 93.22% was obtained. The optimal parameters were successfully predicted by the model for the minimum ALC of 0.312 mg/L, which was validated with the experimental result (0.306 mg/L). The XRD, SEM and PSD results indicated that crystal calcium arsenate Ca 5 (AsO 4 ) 3 OH and Ca 4 (OH) 2 (AsO 4 ) 2 ·4H 2 O formation played an important role in minimizing the ALC. The BCR sequential extraction results demonstrated that the treated HAABS were stable in a weak acidic environment for a short time but posed a potential environmental risk after a long time. The results clearly confirm that the proposed three-factor CCD is an effective approach for modeling the stabilization of HAABS. However, further solidification technology is suggested for use after lime-based stabilization treatment of arsenic-bearing sludges.

Validity of Various Methods for Determining Velocity, Force, and Power in the Back Squat.

PubMed

Banyard, Harry G; Nosaka, Ken; Sato, Kimitake; Haff, G Gregory

2017-10-01

To examine the validity of 2 kinematic systems for assessing mean velocity (MV), peak velocity (PV), mean force (MF), peak force (PF), mean power (MP), and peak power (PP) during the full-depth free-weight back squat performed with maximal concentric effort. Ten strength-trained men (26.1 ± 3.0 y, 1.81 ± 0.07 m, 82.0 ± 10.6 kg) performed three 1-repetition-maximum (1RM) trials on 3 separate days, encompassing lifts performed at 6 relative intensities including 20%, 40%, 60%, 80%, 90%, and 100% of 1RM. Each repetition was simultaneously recorded by a PUSH band and commercial linear position transducer (LPT) (GymAware [GYM]) and compared with measurements collected by a laboratory-based testing device consisting of 4 LPTs and a force plate. Trials 2 and 3 were used for validity analyses. Combining all 120 repetitions indicated that the GYM was highly valid for assessing all criterion variables while the PUSH was only highly valid for estimations of PF (r = .94, CV = 5.4%, ES = 0.28, SEE = 135.5 N). At each relative intensity, the GYM was highly valid for assessing all criterion variables except for PP at 20% (ES = 0.81) and 40% (ES = 0.67) of 1RM. Moreover, the PUSH was only able to accurately estimate PF across all relative intensities (r = .92-.98, CV = 4.0-8.3%, ES = 0.04-0.26, SEE = 79.8-213.1 N). PUSH accuracy for determining MV, PV, MF, MP, and PP across all 6 relative intensities was questionable for the back squat, yet the GYM was highly valid at assessing all criterion variables, with some caution given to estimations of MP and PP performed at lighter loads.

Ares I-X Flight Test Validation of Control Design Tools in the Frequency-Domain

NASA Technical Reports Server (NTRS)

Johnson, Matthew; Hannan, Mike; Brandon, Jay; Derry, Stephen

2011-01-01

A major motivation of the Ares I-X flight test program was to Design for Data, in order to maximize the usefulness of the data recorded in support of Ares I modeling and validation of design and analysis tools. The Design for Data effort was intended to enable good post-flight characterizations of the flight control system, the vehicle structural dynamics, and also the aerodynamic characteristics of the vehicle. To extract the necessary data from the system during flight, a set of small predetermined Programmed Test Inputs (PTIs) was injected directly into the TVC signal. These PTIs were designed to excite the necessary vehicle dynamics while exhibiting a minimal impact on loads. The method is similar to common approaches in aircraft flight test programs, but with unique launch vehicle challenges due to rapidly changing states, short duration of flight, a tight flight envelope, and an inability to repeat any test. This paper documents the validation effort of the stability analysis tools to the flight data which was performed by comparing the post-flight calculated frequency response of the vehicle to the frequency response calculated by the stability analysis tools used to design and analyze the preflight models during the control design effort. The comparison between flight day frequency response and stability tool analysis for flight of the simulated vehicle shows good agreement and provides a high level of confidence in the stability analysis tools for use in any future program. This is true for both a nominal model as well as for dispersed analysis, which shows that the flight day frequency response is enveloped by the vehicle s preflight uncertainty models.

Stability-Indicating HPTLC Method for Studying Stress Degradation Behavior of Sulbutiamine HCl.

PubMed

Farid, Nehal F; Abdelwahab, Nada S

2016-04-01

Sulbutiamine (SUL) is an ester of thiazides with neurotropic action. A new stability indicating HPTLC method has been developed and validated for the determination of SUL in the presence of different degradation products. The drug was subjected to different stress conditions following ICH strategy such as hydrolytic degradation (neutral, alkaline and acidic hydrolysis), oxidation, photodegradation and dry heat degradation. The drug demonstrated degradation under all decomposition conditions except neutral hydrolysis and dry heat, where the drug was completely degraded with 0.1 N NaOH, 1 N HCl and 30% H2O2 while it was partially degradaed by 0.1 N HCl, 3% H2O2 and UV light. Structure elucidation of the resulting degradation products was performed using ESI-Q-MS-MS. A well-defined peak for SUL was obtained at Rf = 0.46 and was completely separated from all obtained degradation products. Chromatographic separation was carried out on HPTLC aluminum plates precoated with silica gel 60 F254 using acetone-methylene chloride-ammonia buffer (pH 8.5 ± 0.2) (7:3:0.5, v/v) as a developing system. Densitometric scanning of the separated peaks was performed at 254 nm. System suitability testing parameters were calculated to ascertain the quality performance of the developed method. The method was validated with respect to USP guidelines regarding accuracy, precision, specificity, robustness and ruggedness. Good correlation coefficients were achieved in the range of 0.4-5.0 µg/band, and the limit of detection and limit of quantitation were found to be 0.11 and 0.33 µg/band, respectively. The utility of the suggested method was verified by application to Arcalion forte® tablets where no interference from additives was found. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Development of a titanium dioxide-coated microfluidic-based photocatalyst-assisted reduction device to couple high-performance liquid chromatography with inductively coupled plasma-mass spectrometry for determination of inorganic selenium species.

PubMed

Shih, Tsung-Ting; Lin, Cheng-Hsing; Hsu, I-Hsiang; Chen, Jian-Yi; Sun, Yuh-Chang

2013-11-05

We developed a selective and sensitive hyphenated system employing a microfluidic-based vapor generation (VG) system in conjunction with high-performance liquid chromatography (HPLC) separation and inductively coupled plasma-mass spectrometry (ICPMS) detection for the determination of trace inorganic selenium (Se) species. The VG system exploited poly(methyl methacrylate) (PMMA) substrates of high optical quality to fabricate a microfluidic-based photocatalyst-assisted reduction device (microfluidic-based PCARD). Moreover, to reduce the consumption of photocatalysts during analytical procedures, a microfluidic-based PCARD coated with titanium dioxide nanoparticles (nano-TiO2) was employed to avoid consecutive loading. Notably, to simplify the coating procedure and improve the stability of the coating materials, a dynamic coating method was utilized. Under the optimized conditions for the selenicals of interest, the online HPLC/TiO2-coated microfluidic-based PCARD/ICPMS system enabled us to achieve detection limits (based on 3σ) of 0.043 and 0.042 μg L(-1) for Se(IV) and Se(VI), respectively. Both Se(IV) and Se(VI) could be efficiently vaporized within 15 s, while a series of validation experiments indicated that our proposed method could be satisfactorily applied to the determination of inorganic Se species in the environmental water samples.

Intramedullary nailing in opening wedge high tibial osteotomy-in vitro test for validation of a method of fixation.

PubMed

Burchard, Rene; Katerla, Denise; Hammer, Marina; Pahlkötter, Anke; Soost, Christian; Dietrich, Gerhard; Ohrndorf, Arne; Richter, Wolfgang; Lengsfeld, Markus; Christ, Hans-Jürgen; Graw, Jan Adriaan; Fritzen, Claus-Peter

2018-02-01

Opening wedge high tibial osteotomy (HTO) as a treatment in unicompartimental osteoarthritis of the knee can significantly relieve pain and prevent or at least delay an early joint replacement. The fixation of the osteotomy has undergone development and refinements during the last years. The angle-stable plate fixator is currently one of the most commonly used plates in HTOs. The angular stable fixation between screws and the plate offers a high primary stability to retain the correction with early weight-bearing protocols. This surgical technique is performed as a standard of care and generally well tolerated by the patients. Nevertheless, some studies observed that many patients complained about discomfort related to the implant. Therefore, the stability of two different intramedullary nails, a short implant used in humeral fractures and a long device used in tibial fractures for stabilization in valgus HTOs, was investigated as an alternative fixation technique. The plate fixator was defined as reference standard. Nine synthetic tibia models were standardly osteotomized and stabilized by one of the fixation devices. Axial compression was realized using a special testing machine and two protocols were performed: a multi-step fatigue test and a load-to-failure test. Overall motion, medial, and lateral displacements were documented. Fractures always occurred at the lateral cortex. Axial cyclic loading up to 800 N was tolerated by all implants without failure. The tibia nail provided highest fatigue strength under the load-to-failure conditions. The results suggest that intramedullary nailing might be used as an alternative concept in HTO.

Nonlinear SVM-DTC for induction motor drive using input-output feedback linearization and high order sliding mode control.

PubMed

Ammar, Abdelkarim; Bourek, Amor; Benakcha, Abdelhamid

2017-03-01

This paper presents a nonlinear Direct Torque Control (DTC) strategy with Space Vector Modulation (SVM) for an induction motor. A nonlinear input-output feedback linearization (IOFL) is implemented to achieve a decoupled torque and flux control and the SVM is employed to reduce high torque and flux ripples. Furthermore, the control scheme performance is improved by inserting a super twisting speed controller in the outer loop and a load torque observer to enhance the speed regulation. The combining of dual nonlinear strategies ensures a good dynamic and robustness against parameters variation and disturbance. The system stability has been analyzed using Lyapunov stability theory. The effectiveness of the control algorithm is investigated by simulation and experimental validation using Matlab/Simulink software with real-time interface based on dSpace 1104. Copyright © 2017 ISA. Published by Elsevier Ltd. All rights reserved.

Analysis of anti-neoplastic drug in bacterial ghost matrix, w/o/w double nanoemulsion and w/o nanoemulsion by a validated 'green' liquid chromatographic method.

PubMed

Youssof, Abdullah M E; Salem-Bekhit, Mounir M; Shakeel, Faiyaz; Alanazi, Fars K; Haq, Nazrul

2016-07-01

The objective of the present investigation was to develop and validate a 'green' reversed phase high-performance liquid chromatography (RP-HPLC) method for rapid analysis of a cytotoxic drug 5-fluorouracil (5-FU) in bulk drug, marketed injection, water-in-oil (w/o) nanoemulsion, double water-in-oil-in-water (w/o/w) nanoemulsion and bacterial ghost (BG) matrix. The chromatography study was carried out at room temperature (25±1°C) using an HPLC system with the help of ultraviolet (UV)-visible detector. The chromatographic performance was achieved with a Nucleodur 150mm×4.6mm RP C8 column filled with 5µm filler as a static phase. The mobile phase consisted of ethyl acetate: methanol (7:3% v/v) which was delivered at a flow rate of 1.0mLmin(-1) and the drug was detected in UV mode at 254nm. The developed method was validated in terms of linearity (r(2)=0.998), accuracy (98.19-102.09%), precision (% RSD=0.58-1.17), robustness (% RSD=0.12-0.53) and sensitivity with satisfactory results. The efficiency of the method was demonstrated by the assay of the drug in marketed injection, w/o nanoemulsion, w/o/w nanoemulsion and BG with satisfactory results. The successful resolution of the drug along with its degradation products clearly established the stability-indicating nature of the proposed method. Overall, these results suggested that the proposed analytical method could be effectively applied to the routine analysis of 5-FU in bulk drug, various pharmaceutical dosage forms and BG. Copyright © 2016 Elsevier B.V. All rights reserved.

Design and Validation of a Low-Cost Portable Device to Quantify Postural Stability.

PubMed

Zhu, Yong

2017-03-18

Measurement of the displacement of the center-of-pressure (COP) is an important tool used in biomechanics to assess postural stability and human balance. The goal of this research was to design and validate a low-cost portable device that can offer a quick indication of the state of postural stability and human balance related conditions. Approximate entropy (ApEn) values reflecting the amount of irregularity hiding in COP oscillations were used to calculate the index. The prototype adopted a portable design using the measurements of the load cells located at the four corners of a low-cost force platform. The test subject was asked to stand on the device in a quiet, normal, upright stance for 30 s with eyes open and subsequently for 30 s with eyes closed. Based on the COP displacement signals, the ApEn values were calculated. The results indicated that the prototype device was capable of capturing the increase in regularity of postural control in the visual-deprivation conditions. It was also able to decipher the subtle postural control differences along anterior-posterior and medial-lateral directions. The data analysis demonstrated that the prototype would enable the quantification of postural stability and thus provide a low-cost portable device to assess many conditions related to postural stability and human balance such as aging and pathologies.

Transonic aeroelastic analysis of launch vehicle configurations. Ph.D. Thesis

NASA Technical Reports Server (NTRS)

Filgueirasdeazevedo, Joao Luiz

1988-01-01

A numerical study of the aeroelastic stability of typical launch vehicle configurations in transonic flight is performed. Recent computational fluid dynamics techniques are used to simulate the transonic aerodynamic flow fields, as opposed to relying on experimental data for the unsteady aerodynamic pressures. The flow solver is coupled to an appropriate structural representation of the vehicle. The aerodynamic formulation is based on the thin layer approximation to the Reynolds-Averaged Navier-Stokes equations, where the account for turbulent mixing is done by the two-layer Baldwin and Lomax algebraic eddy viscosity model. The structural-dynamic equations are developed considering free-free flexural vibration of an elongated beam with variable properties and are cast in modal form. Aeroelastic analyses are performed by integrating simultaneously in the two sets of equations. By tracing the growth or decay of a perturbed oscillation, the aeroelastic stability of a given constant configuration can be ascertained. The method is described in detail, and results that indicate its application are presented. Applications include some validation cases for the algorithm developed, as well as the study of configurations known to have presented flutter programs in the past.

Advanced stability indicating chemometric methods for quantitation of amlodipine and atorvastatin in their quinary mixture with acidic degradation products

NASA Astrophysics Data System (ADS)

Darwish, Hany W.; Hassan, Said A.; Salem, Maissa Y.; El-Zeany, Badr A.

2016-02-01

Two advanced, accurate and precise chemometric methods are developed for the simultaneous determination of amlodipine besylate (AML) and atorvastatin calcium (ATV) in the presence of their acidic degradation products in tablet dosage forms. The first method was Partial Least Squares (PLS-1) and the second was Artificial Neural Networks (ANN). PLS was compared to ANN models with and without variable selection procedure (genetic algorithm (GA)). For proper analysis, a 5-factor 5-level experimental design was established resulting in 25 mixtures containing different ratios of the interfering species. Fifteen mixtures were used as calibration set and the other ten mixtures were used as validation set to validate the prediction ability of the suggested models. The proposed methods were successfully applied to the analysis of pharmaceutical tablets containing AML and ATV. The methods indicated the ability of the mentioned models to solve the highly overlapped spectra of the quinary mixture, yet using inexpensive and easy to handle instruments like the UV-VIS spectrophotometer.

A measure of satisfaction with food-related life.

PubMed

Grunert, Klaus G; Dean, Moira; Raats, Monique M; Nielsen, Niels Asger; Lumbers, Margaret

2007-09-01

A measure of satisfaction with food-related life is developed and tested in three studies in eight European countries. Five items are retained from an original pool of seven; these items exhibit good reliability as measured by Cronbach's alpha, good temporal stability, convergent validity with two related measures, and construct validity as indicated by relationships with other indicators of quality of life, including the Satisfaction With Life and the SF-8 scales. It is concluded that this scale will be useful in studies trying to identify factors contributing to satisfaction with food-related life.

A Case Study on a Combination NDVI Forecasting Model Based on the Entropy Weight Method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, Shengzhi; Ming, Bo; Huang, Qiang

It is critically meaningful to accurately predict NDVI (Normalized Difference Vegetation Index), which helps guide regional ecological remediation and environmental managements. In this study, a combination forecasting model (CFM) was proposed to improve the performance of NDVI predictions in the Yellow River Basin (YRB) based on three individual forecasting models, i.e., the Multiple Linear Regression (MLR), Artificial Neural Network (ANN), and Support Vector Machine (SVM) models. The entropy weight method was employed to determine the weight coefficient for each individual model depending on its predictive performance. Results showed that: (1) ANN exhibits the highest fitting capability among the four orecastingmore » models in the calibration period, whilst its generalization ability becomes weak in the validation period; MLR has a poor performance in both calibration and validation periods; the predicted results of CFM in the calibration period have the highest stability; (2) CFM generally outperforms all individual models in the validation period, and can improve the reliability and stability of predicted results through combining the strengths while reducing the weaknesses of individual models; (3) the performances of all forecasting models are better in dense vegetation areas than in sparse vegetation areas.« less

Validation of a method for quantitation of the clopidogrel active metabolite, clopidogrel, clopidogrel carboxylic acid, and 2-oxo-clopidogrel in feline plasma.

PubMed

Lyngby, Janne G; Court, Michael H; Lee, Pamela M

2017-08-01

The clopidogrel active metabolite (CAM) is unstable and challenging to quantitate. The objective was to validate a new method for stabilization and quantitation of CAM, clopidogrel, and the inactive metabolites clopidogrel carboxylic acid and 2-oxo-clopiodgrel in feline plasma. Two healthy cats administered clopidogrel to demonstrate assay in vivo utility. Stabilization of CAM was achieved by adding 2-bromo-3'methoxyacetophenone to blood tubes to form a derivatized CAM (CAM-D). Method validation included evaluation of calibration curve linearity, accuracy, and precision; within and between assay precision and accuracy; and compound stability using spiked blank feline plasma. Analytes were measured by high performance liquid chromatography with tandem mass spectrometry. In vivo utility was demonstrated by a pharmacokinetic study of cats given a single oral dose of 18.75mg clopidogrel. The 2-oxo-clopidogrel metabolite was unstable. Clopidogrel, CAM-D, and clopidogrel carboxylic acid appear stable for 1 week at room temperature and 9 months at -80°C. Standard curves showed linearity for CAM-D, clopidogrel, and clopidogrel carboxylic acid (r > 0.99). Between assay accuracy and precision was ≤2.6% and ≤7.1% for CAM-D and ≤17.9% and ≤11.3% for clopidogrel and clopidogrel carboxylic acid. Within assay precision for all three compounds was ≤7%. All three compounds were detected in plasma from healthy cats receiving clopidogrel. This methodology is accurate and precise for simultaneous quantitation of CAM-D, clopidogrel, and clopidogrel carboxylic acid in feline plasma but not 2-oxo-clopidogrel. Validation of this assay is the first step to more fully understanding the use of clopidogrel in cats. Copyright © 2017 Elsevier B.V. All rights reserved.

Advanced UVOIR Mirror Technology Development for Very Large Space Telescopes

NASA Technical Reports Server (NTRS)

Stahl, H. Philip

2011-01-01

Objective of this work is to define and initiate a long-term program to mature six inter-linked critical technologies for future UVOIR space telescope mirrors to TRL6 by 2018 so that a viable flight mission can be proposed to the 2020 Decadal Review. (1) Large-Aperture, Low Areal Density, High Stiffness Mirrors: 4 to 8 m monolithic & 8 to 16 m segmented primary mirrors require larger, thicker, stiffer substrates. (2) Support System:Large-aperture mirrors require large support systems to ensure that they survive launch and deploy on orbit in a stress-free and undistorted shape. (3) Mid/High Spatial Frequency Figure Error:A very smooth mirror is critical for producing a high-quality point spread function (PSF) for high-contrast imaging. (4) Segment Edges:Edges impact PSF for high-contrast imaging applications, contributes to stray light noise, and affects the total collecting aperture. (5) Segment-to-Segment Gap Phasing:Segment phasing is critical for producing a high-quality temporally stable PSF. (6) Integrated Model Validation:On-orbit performance is determined by mechanical and thermal stability. Future systems require validated performance models. We are pursuing multiple design paths give the science community the option to enable either a future monolithic or segmented space telescope.

Pumped storage system model and experimental investigations on S-induced issues during transients

NASA Astrophysics Data System (ADS)

Zeng, Wei; Yang, Jiandong; Hu, Jinhong

2017-06-01

Because of the important role of pumped storage stations in the peak regulation and frequency control of a power grid, pump turbines must rapidly switch between different operating modes, such as fast startup and load rejection. However, pump turbines go through the unstable S region in these transition processes, threatening the security and stability of the pumped storage station. This issue has mainly been investigated through numerical simulations, while field experiments generally involve high risks and are difficult to perform. Therefore, in this work, the model test method was employed to study S-induced security and stability issues for a pumped storage station in transition processes. First, a pumped storage system model was set up, including the piping system, model units, electrical control systems and measurement system. In this model, two pump turbines with different S-shaped characteristics were installed to determine the influence of S-shaped characteristics on transition processes. The model platform can be applied to simulate any hydraulic transition process that occurs in real power stations, such as load rejection, startup, and grid connection. On the experimental platform, the S-shaped characteristic curves were measured to be the basis of other experiments. Runaway experiments were performed to verify the impact of the S-shaped characteristics on the pump turbine runaway stability. Full load rejection tests were performed to validate the effect of the S-shaped characteristics on the water-hammer pressure. The condition of one pump turbine rejecting its load after another defined as one-after-another (OAA) load rejection was performed to validate the possibility of S-induced extreme draft tube pressure. Load rejection experiments with different guide vane closing schemes were performed to determine a suitable scheme to adapt the S-shaped characteristics. Through these experiments, the threats existing in the station were verified, the appropriate measures were summarized, and an important experimental basis for the safe and stable operation of a pumped storage station was provided.

Further examination of embedded performance validity indicators for the Conners' Continuous Performance Test and Brief Test of Attention in a large outpatient clinical sample.

PubMed

Sharland, Michael J; Waring, Stephen C; Johnson, Brian P; Taran, Allise M; Rusin, Travis A; Pattock, Andrew M; Palcher, Jeanette A

2018-01-01

Assessing test performance validity is a standard clinical practice and although studies have examined the utility of cognitive/memory measures, few have examined attention measures as indicators of performance validity beyond the Reliable Digit Span. The current study further investigates the classification probability of embedded Performance Validity Tests (PVTs) within the Brief Test of Attention (BTA) and the Conners' Continuous Performance Test (CPT-II), in a large clinical sample. This was a retrospective study of 615 patients consecutively referred for comprehensive outpatient neuropsychological evaluation. Non-credible performance was defined two ways: failure on one or more PVTs and failure on two or more PVTs. Classification probability of the BTA and CPT-II into non-credible groups was assessed. Sensitivity, specificity, positive predictive value, and negative predictive value were derived to identify clinically relevant cut-off scores. When using failure on two or more PVTs as the indicator for non-credible responding compared to failure on one or more PVTs, highest classification probability, or area under the curve (AUC), was achieved by the BTA (AUC = .87 vs. .79). CPT-II Omission, Commission, and Total Errors exhibited higher classification probability as well. Overall, these findings corroborate previous findings, extending them to a large clinical sample. BTA and CPT-II are useful embedded performance validity indicators within a clinical battery but should not be used in isolation without other performance validity indicators.

Five-Kilometers Time Trial: Preliminary Validation of a Short Test for Cycling Performance Evaluation.

PubMed

Dantas, Jose Luiz; Pereira, Gleber; Nakamura, Fabio Yuzo

2015-09-01

The five-kilometer time trial (TT5km) has been used to assess aerobic endurance performance without further investigation of its validity. This study aimed to perform a preliminary validation of the TT5km to rank well-trained cyclists based on aerobic endurance fitness and assess changes of the aerobic endurance performance. After the incremental test, 20 cyclists (age = 31.3 ± 7.9 years; body mass index = 22.7 ± 1.5 kg/m(2); maximal aerobic power = 360.5 ± 49.5 W) performed the TT5km twice, collecting performance (time to complete, absolute and relative power output, average speed) and physiological responses (heart rate and electromyography activity). The validation criteria were pacing strategy, absolute and relative reliability, validity, and sensitivity. Sensitivity index was obtained from the ratio between the smallest worthwhile change and typical error. The TT5km showed high absolute (coefficient of variation < 3%) and relative (intraclass coefficient correlation > 0.95) reliability of performance variables, whereas it presented low reliability of physiological responses. The TT5km performance variables were highly correlated with the aerobic endurance indices obtained from incremental test (r > 0.70). These variables showed adequate sensitivity index (> 1). TT5km is a valid test to rank the aerobic endurance fitness of well-trained cyclists and to differentiate changes on aerobic endurance performance. Coaches can detect performance changes through either absolute (± 17.7 W) or relative power output (± 0.3 W.kg(-1)), the time to complete the test (± 13.4 s) and the average speed (± 1.0 km.h(-1)). Furthermore, TT5km performance can also be used to rank the athletes according to their aerobic endurance fitness.

Engineering a highly active thermophilic β-glucosidase to enhance its pH stability and saccharification performance.

PubMed

Xia, Wei; Xu, Xinxin; Qian, Lichun; Shi, Pengjun; Bai, Yingguo; Luo, Huiying; Ma, Rui; Yao, Bin

2016-01-01

β-Glucosidase is an important member of the biomass-degrading enzyme system, and plays vital roles in enzymatic saccharification for biofuels production. Candidates with high activity and great stability over high temperature and varied pHs are always preferred in industrial practice. To achieve cost-effective biomass conversion, exploring natural enzymes, developing high level expression systems and engineering superior mutants are effective approaches commonly used. A newly identified β-glucosidase of GH3, Bgl3A, from Talaromyces leycettanus JCM12802, was overexpressed in yeast strain Pichia pastoris GS115, yielding a crude enzyme activity of 6000 U/ml in a 3 L fermentation tank. The purified enzyme exhibited outstanding enzymatic properties, including favorable temperature and pH optima (75 °C and pH 4.5), good thermostability (maintaining stable at 60 °C), and high catalytic performance (with a specific activity and catalytic efficiency of 905 U/mg and 9096/s/mM on pNPG, respectively). However, the narrow stability of Bgl3A at pH 4.0-5.0 would limit its industrial applications. Further site-directed mutagenesis indicated the role of excessive O-glycosylation in pH liability. By removing the potential O-glycosylation sites, two mutants showed improved pH stability over a broader pH range (3.0-10.0). Besides, with better stability under pH 5.0 and 50 °C compared with wild type Bgl3A, saccharification efficiency of mutant M1 was improved substantially cooperating with cellulase Celluclast 1.5L. And mutant M1 reached approximately equivalent saccharification performance to commercial β-glucosidase Novozyme 188 with identical β-glucosidase activity, suggesting its great prospect in biofuels production. In this study, we overexpressed a novel β-glucosidase Bgl3A with high specific activity and high catalytic efficiency in P. pastoris. We further proved the negative effect of excessive O-glycosylation on the pH stability of Bgl3A, and enhanced the pH stability by reducing the O-glycosylation. And the enhanced mutants showed much better application prospect with substantially improved saccharification efficiency on cellulosic materials.

Stability of Allopurinol, Amitriptyline Hydrochloride, Carbamazepine, Domperidone, Isoniazid, Ketoconazole, Lisinopril, Naproxen, Paracetamol (Acetaminophen), and Sertraline Hydrochloride in SyrSpend SF PH4 Oral Suspensions.

PubMed

Polonini, Hudson C; Loures, Sharlene; de Araujo, Edson Peter; Brandão, Marcos Antônio F; Ferreira, Anderson O

2016-01-01

Oral liquids are safe alternatives to solid dosage forms, notably for elderly and pediatric patients that present dysphagia. The use of ready-to-use suspending vehicles such as SyrSpend SF PH4 is a suitable resource for pharmacists as they constitute a safe and timesaving option that has been studied often. The objective of this study was to evaluate the stability of 10 commonly used active pharmaceutical ingredients (allopurinol 20 mg/mL; amitriptyline hydrochloride 10 mg/mL; carbamazepine 25 mg/mL; domperidone 5 mg/mL; isoniazid 10 mg/mL; ketoconazole 20 mg/mL; lisinopril 1 mg/mL; naproxen 25 mg/mL; paracetamol [acetaminophen] 50 mg/mL; and sertraline hydrochloride 10 mg/mL) compounded in oral suspensions using SyrSpend SF PH4 as the vehicle throughout the study period and stored both at controlled refrigerated (2°C to 8°C) and room temperature (20°C to 25°C). Stability was assessed by means of measuring the percent recovery at varying time points throughout a 90-day period. The quantification of the active pharmaceutical ingredients was performed by high-performance liquid chromatography through a stability-indicating method. Methods were adequately validated. Forced-degradation studies showed that at least one parameter influenced the stability of the active pharmaceutical ingredients. All suspensions were assayed and showed active pharmaceutical ingredient contents between 90% and 110% during the 90-day study period. Although the forced-degradation experiments led to visible fluctuations in the chromatographic responses, the final preparations were stable in the storage conditions. The beyond-use dates of the preparations were found to be at least 90 days for all suspensions, both for controlled refrigerated temperature and room temperature. This confirms that SyrSpend SF PH4 is a stable suspending vehicle for compounding with a broad range of different active pharmaceutical ingredients for different medical usages. Copyright© by International Journal of Pharmaceutical Compounding, Inc.

Does early childhood callous-unemotional behavior uniquely predict behavior problems or callous-unemotional behavior in late childhood?

PubMed Central

Waller, Rebecca; Dishion, Thomas J.; Shaw, Daniel S.; Gardner, Frances; Wilson, Melvin N.; Hyde, Luke W.

2016-01-01

Callous unemotional (CU) behavior has been linked to behavior problems in children and adolescents. However, few studies have examined whether CU behavior in early childhood predicts behavior problems or CU behavior in late childhood. This study examined whether indicators of CU behavior at ages 2–4 predicted aggression, rule-breaking, and CU behavior across informants at age 9.5. To test the unique predictive and convergent validity of CU behavior in early childhood, we accounted for stability in behavior problems and method effects to rule out the possibility that rater biases inflated the magnitude of any associations found. Cross-informant data were collected from a multi-ethnic, high-risk sample (N = 731; female = 49%) at ages 2–4 and again at age 9.5. From age 3, CU behavior uniquely predicted aggression and rule-breaking across informants. There were also unique associations between CU behavior assessed at ages 3 and 4 and CU behavior assessed at age 9.5. Findings demonstrate that early-childhood indicators of CU behavior account for unique variance in later childhood behavior problems and CU behavior, taking into account stability in behavior problems over time and method effects. Convergence with a traditional measure of CU behavior in late childhood provides support for the construct validity of a brief early childhood measure of CU behavior. PMID:27598253

Modeling synchronous voltage source converters in transmission system planning studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kosterev, D.N.

1997-04-01

A Voltage Source Converter (VSC) can be beneficial to power utilities in many ways. To evaluate the VSC performance in potential applications, the device has to be represented appropriately in planning studies. This paper addresses VSC modeling for EMTP, powerflow, and transient stability studies. First, the VSC operating principles are overviewed, and the device model for EMTP studies is presented. The ratings of VSC components are discussed, and the device operating characteristics are derived based on these ratings. A powerflow model is presented and various control modes are proposed. A detailed stability model is developed, and its step-by-step initialization proceduremore » is described. A simplified stability model is also derived under stated assumptions. Finally, validation studies are performed to demonstrate performance of developed stability models and to compare it with EMTP simulations.« less

Energy absorption as a predictor of leg impedance in highly trained females.

PubMed

Kulas, Anthony S; Schmitz, Randy J; Schultz, Sandra J; Watson, Mary Allen; Perrin, David H

2006-08-01

Although leg spring stiffness represents active muscular recruitment of the lower extremity during dynamic tasks such as hopping and running, the joint-specific characteristics comprising the damping portion of this measure, leg impedance, are uncertain. The purpose of this investigation was to assess the relationship between leg impedance and energy absorption at the ankle, knee, and hip during early (impact) and late (stabilization) phases of landing. Twenty highly trained female dancers (age = 20.3 +/- 1.4 years, height = 163.7 +/- 6.0 cm, mass = 62.1 +/- 8.1 kg) were instrumented for biomechanical analysis. Subjects performed three sets of double-leg landings from under preferred, stiff, and soft landing conditions. A stepwise linear regression analysis revealed that ankle and knee energy absorption at impact, and knee and hip energy absorption during the stabilization phases of landing explained 75.5% of the variance in leg impedance. The primary predictor of leg impedance was knee energy absorption during the stabilization phase, independently accounting for 55% of the variance. Future validation studies applying this regression model to other groups of individuals are warranted.

Development and validation of a stability-indicating gas chromatographic method for quality control of residual solvents in blonanserin: a novel atypical antipsychotic agent.

PubMed

Peng, Ming; Liu, Jin; Lu, Dan; Yang, Yong-Jian

2012-09-01

Blonanserin is a novel atypical antipsychotic agent for the treatment of schizophrenia. Ethyl alcohol, isopropyl alcohol and toluene are utilized in the synthesis route of this bulk drug. A new validated gas chromatographic (GC) method for the simultaneous determination of residual solvents in blonanserin is described in this paper. Blonanserin was dissolved in N, N-dimethylformamide to make a sample solution that was directly injected into a DB-624 column. A postrun oven temperature at 240°C for approximately 2 h after the analysis cycle was performed to wash out blonanserin residue in the GC column. Quantitation was performed by external standard analyses and the validation was carried out according to International Conference on Harmonization validation guidelines Q2A and Q2B. The method was shown to be specific (no interference in the blank solution), linear (correlation coefficients ≥0.99998, n = 10), accurate (average recoveries between 94.1 and 101.7%), precise (intra-day and inter-day precision ≤2.6%), sensitive (limit of detection ≤0.2 ng, and limit of quantitation ≤0.7 ng), robust (small variations of carrier gas flow, initial oven temperature, temperature ramping rate, injector and detector temperatures did not significantly affect the system suitability test parameters and peak areas) and stable (reference standard and sample solutions were stable over 48 h). This extensively validated method is ready to be used for the quality control of blonanserin.

Physical and chemical stability of high-dose ifosfamide and mesna for prolonged 14-day continuous infusion.

PubMed

Zhang, YanPing; Kawedia, Jitesh D; Myers, Alan L; McIntyre, Chelsey M; Anderson, Peter M; Kramer, Mark A; Culotta, Kirk S

2014-02-01

Ifosfamide plus mesna have been used recently in a high-dose regimen that allows this chemotherapy to be given to outpatients with less toxicity over 14 days using a portable pump. However, there is a need for published stability information. The aim of this study was to investigate the physicochemical stability of ifosfamide with mesna in normal saline at room temperature over a prolonged period of 14 days. Infusion solutions of 1:1 ifosfamide and mesna at final concentrations of 10, 20 and 30 mg/mL were prepared with 0.9% sodium chloride in PVC bags. Solutions were stored at room temperature. Concentrations of ifosfamide and mesna were measured at 0 and 1, 3, 7 and 14 days using a stability-indicating reversed phase high-performance liquid chromatography (HPLC) assay with ultraviolet detection. Ifosfamide and mesna were both physicochemically stable (>94%) for 14 days in all tested infusion solutions (10, 20 and 30 mg/mL). Our stability data indicate that ifosfamide and mesna (1:1) combination can be administered as a prolonged continuous infusion with portable pump in an outpatient setting without replacement of the infusion bag. We suggest 20 mg/mL as a reasonable concentration for infusion rates of about 2-4 cc/hr over prolonged periods of time.

Rotordynamic Instability Problems in High-Performance Turbomachinery 1996

NASA Technical Reports Server (NTRS)

1997-01-01

The first rotordynamics workshop proceedings emphasized a feeling of uncertainty in predicting the stability of characteristics of high-performance turbomachinery. In the second workshop proceedings these uncertainties were reduced through programs established to systematically resolve problems, with emphasis on experimental validation of the forces that influence rotordynamics. In the third proceedings many programs for predicting or measuring forces and force coefficients in high-performance turbomachinery produced results. Data became available for designing new machines with enhanced stability characteristics or for upgrading existing machines. In the fourth proceedings there emerged trends towards a more unified view of rotordynamic instability problems and several encouraging new analytical developments. The fifth workshop supported the continuing trend toward a unified view with several new developments in the design and manufacture of new turbomachineries with enhanced stability characteristics along with new data and associated numerical/theoretical results. The sixth workshop report provided field experience and experimental results, and expanded the use of computational and control techniques with integration of damper, bearing, and eccentric seal operation results. The seventh workshop report provided field experiences, numerical, theoretical, and experimental results and control methods for seals, bearings, and dampers with some attention given to variable thermophysical properties and turbulence measurements, and introduction of two-phase flow results. In the present workshop, active magnetic bearings (AMB's) evolve into a new method of measuring rotordynamic coefficients with discussions on honeycomb seals, drop of magnetically supported rotors, seals, bearings and dampers with new data being reported. The intent of the workshop and this proceedings is to provide a continuing impetus for an understanding and resolution of these problems.

Parental Flooding During Conflict: A Psychometric Evaluation of a New Scale

PubMed Central

Del Vecchio, Tamara; Lorber, Michael F.; Slep, Amy M. Smith; Malik, Jill; Heyman, Richard E.; Foran, Heather M.

2016-01-01

Parents who are overwhelmed by the intensity and aversive nature of child negative affect — those who are experiencing flooding — may be less likely to react effectively and instead may focus on escaping the aversive situation, disciplining either overly permissively or punitively to escape quickly from child negative affect. However, there are no validated self-report measures of the degree to which parents experience flooding, impeding the exploration of these relations. Thus, we created and evaluated the Parent Flooding scale (PFS), assessing the extent to which parents believe their children's negative affect during parent-child conflicts is unexpected, overwhelming and distressing. We studied its factorial validity, reliability, and concurrent validity in a community sample of 453 couples with 3- to 7-year-old children (51.9% girls) recruited via random digit dialing. Confirmatory factor analyses indicated a one-factor solution with excellent internal consistency. Test-retest stability over an average of 5.6 months was high. Concurrent validity was suggested by the associations of flooding with parents’ aggression toward their children, overreactive and lax discipline, parenting satisfaction, and parents’ anger, as well as with child externalizing behavior and negative affect. Incrementally concurrent validity analyses indicated that flooding was a unique predictor of mothers’ and fathers’ overreactive discipline and fathers’ parent-child aggression and lax discipline, over and above the contributions of parents’ anger and children's negative affect. The present results support the psychometric validity of the PFS. PMID:26909682

A multicenter prospective cohort study on camera navigation training for key user groups in minimally invasive surgery.

PubMed

Graafland, Maurits; Bok, Kiki; Schreuder, Henk W R; Schijven, Marlies P

2014-06-01

Untrained laparoscopic camera assistants in minimally invasive surgery (MIS) may cause suboptimal view of the operating field, thereby increasing risk for errors. Camera navigation is often performed by the least experienced member of the operating team, such as inexperienced surgical residents, operating room nurses, and medical students. The operating room nurses and medical students are currently not included as key user groups in structured laparoscopic training programs. A new virtual reality laparoscopic camera navigation (LCN) module was specifically developed for these key user groups. This multicenter prospective cohort study assesses face validity and construct validity of the LCN module on the Simendo virtual reality simulator. Face validity was assessed through a questionnaire on resemblance to reality and perceived usability of the instrument among experts and trainees. Construct validity was assessed by comparing scores of groups with different levels of experience on outcome parameters of speed and movement proficiency. The results obtained show uniform and positive evaluation of the LCN module among expert users and trainees, signifying face validity. Experts and intermediate experience groups performed significantly better in task time and camera stability during three repetitions, compared to the less experienced user groups (P < .007). Comparison of learning curves showed significant improvement of proficiency in time and camera stability for all groups during three repetitions (P < .007). The results of this study show face validity and construct validity of the LCN module. The module is suitable for use in training curricula for operating room nurses and novice surgical trainees, aimed at improving team performance in minimally invasive surgery. © The Author(s) 2013.

Development and psychometric properties of a new social support scale for self-care in middle-aged patients with type II diabetes (S4-MAD)

PubMed Central

2012-01-01

Background Social support has proved to be one of the most effective factors on the success of diabetic self-care. This study aimed to develop a scale for evaluating social support for self-care in middle-aged patients (30–60 years old) with type II diabetes. Methods This was a two-phase qualitative and quantitative study. The study was conducted during 2009 to 2011 in Tehran, Iran. In the qualitative part, a sample of diabetic patients participated in four focus group discussions in order to develop a preliminary item pool. Consequently, content and face validity were performed to provide a pre-final version of the questionnaire. Then, in a quantitative study, reliability (internal consistency and test-retest analysis), validity and factor analysis (both exploratory and confirmatory) were performed to assess psychometric properties of the scale. Results A 38-item questionnaire was developed through the qualitative phase. It was reduced to a 33-item after content validity. Exploratory factor analysis loaded a 30-item with a five-factor solution (nutrition, physical activity, self monitoring of blood glucose, foot care and smoking) that jointly accounted for 72.3% of observed variance. The confirmatory factor analysis indicated a good fit to the data. The Cronbach’s alpha coefficient showed excellent internal consistency (alpha=0.94), and test-retest of the scale with 2-weeks intervals indicated an appropriate stability for the scale (ICC=0.87). Conclusion The findings showed that the designed questionnaire was a valid and reliable instrument for measuring social support for self-care in middle-aged patients with type II diabetes. It is an easy to use questionnaire and contains the most significant diabetes related behaviors that need continuous support for self-care. PMID:23190685

Evaluating 8 pillars of Total Productive Maintenance (TPM) implementation and their contribution to manufacturing performance

NASA Astrophysics Data System (ADS)

Adesta, E. Y. T.; Prabowo, H. A.; Agusman, D.

2018-01-01

TPM is one method to improve manufacturing performance through an emphasis on maintenance that involves everyone in the organization. Research on the application of TPM and its relevance to the manufacturing performance has been performed quite a lot. However, to the best of our knowledge, a study that deliberates how the application of 8 pillars TPM (especially in developing countries) is still hard to find. This paper attempts to evaluate in more detail about how the 8 pillars of TPM are applied in Indonesia and their impact on manufacturing performance. This research is a pilot study with a target of 50 companies. From the results of data collection, only 22 companies (44%) are eligible to process. Data processing was performed using SPSS and Smart PLS tools. From the validity and reliability tests, it can be seen that all items/indicators for TPM pillars are valid and reliable with correlation value (R) of 0.614 - 0.914 and with Cronbach’s alpha equal to 0.753. As for the Manufacturing Performance construct, the Delivery indicator was not valid. In overall, the model is reliable with Cronbach’s alpha of 0.710. From the results of Confirmatory Factors Analysis (CFA) for TPM, it can be seen that four indicators (pillars) are highly significant while four other indicators are less significant. For MP, three indicators are significant, and two are not significant. In general, the structural model of the relationship between TPM and MP is relatively strong and positive with values R = 0.791, and R squared = 0.626. This means that the TPM Pillars can explain 62.6% MP variability construct variable, while the other 37.4% can be explained by unrelated variables.

Validation of the Karolinska sleepiness scale against performance and EEG variables.

PubMed

Kaida, Kosuke; Takahashi, Masaya; Akerstedt, Torbjörn; Nakata, Akinori; Otsuka, Yasumasa; Haratani, Takashi; Fukasawa, Kenji

2006-07-01

The Karolinska sleepiness scale (KSS) is frequently used for evaluating subjective sleepiness. The main aim of the present study was to investigate the validity and reliability of the KSS with electroencephalographic, behavioral and other subjective indicators of sleepiness. Participants were 16 healthy females aged 33-43 (38.1+/-2.68) years. The experiment involved 8 measurement sessions per day for 3 consecutive days. Each session contained the psychomotor vigilance task (PVT), the Karolinska drowsiness test (KDT-EEG alpha & theta power), the alpha attenuation test (AAT-alpha power ratio open/closed eyes) and the KSS. Median reaction time, number of lapses, alpha and theta power density and the alpha attenuation coefficients (AAC) showed highly significant increase with increasing KSS. The same variables were also significantly correlated with KSS, with a mean value for lapses (r=0.56). The KSS was closely related to EEG and behavioral variables, indicating a high validity in measuring sleepiness. KSS ratings may be a useful proxy for EEG or behavioral indicators of sleepiness.

Computational evaluation of load carriage effects on gait balance stability.

PubMed

Mummolo, Carlotta; Park, Sukyung; Mangialardi, Luigi; Kim, Joo H

2016-01-01

Evaluating the effects of load carriage on gait balance stability is important in various applications. However, their quantification has not been rigorously addressed in the current literature, partially due to the lack of relevant computational indices. The novel Dynamic Gait Measure (DGM) characterizes gait balance stability by quantifying the relative effects of inertia in terms of zero-moment point, ground projection of center of mass, and time-varying foot support region. In this study, the DGM is formulated in terms of the gait parameters that explicitly reflect the gait strategy of a given walking pattern and is used for computational evaluation of the distinct balance stability of loaded walking. The observed gait adaptations caused by load carriage (decreased single support duration, inertia effects, and step length) result in decreased DGM values (p < 0.0001), which indicate that loaded walking motions are more statically stable compared with the unloaded normal walking. Comparison of the DGM with other common gait stability indices (the maximum Floquet multiplier and the margin of stability) validates the unique characterization capability of the DGM, which is consistently informative of the presence of the added load.

Unbalance Response Analysis and Experimental Validation of an Ultra High Speed Motor-Generator for Microturbine Generators Considering Balancing

PubMed Central

Hong, Do-Kwan; Joo, Dae-Suk; Woo, Byung-Chul; Koo, Dae-Hyun; Ahn, Chan-Woo

2014-01-01

The objective of the present study was to deal with the rotordynamics of the rotor of an ultra-high speed PM type synchronous motor-generator for a 500 W rated micro gas turbine generator. This paper introduces dynamic analysis, and experiments on the motor-generator. The focus is placed on an analytical approach considering the mechanical dynamic problems. It is essential to deal with dynamic stability at ultra-high speeds. Unbalance response analysis is performed by calculating the unbalance with and without balancing using a balancing machine. Critical speed analysis is performed to determine the operating speed with sufficient separation margin. The unbalance response analysis is compared with the experimental results considering the balancing grade (ISO 1940-1) and predicted vibration displacement with and without balancing. Based on these results, a high-speed motor-generator was successfully developed. PMID:25177804

Implementation and Validation of Bioplausible Visual Servoing Control

DTIC Science & Technology

2013-03-01

achieve pose stabilization in the context of one -dimensional (1-D) attitude stabilization. These results have been benchmarked against an ideal...scenes representing low (bottom) and high (top) contrast environments used in testing the TurtleBot on the two algorithms...The graph on the left corresponds to the high-contrast simulation environment, and the image on the right corresponds to the low-contrast

Physical and chemical stability of nanostructured lipid drug carriers (NLC) based on natural lipids from Baikal region (Siberia, Russia).

PubMed

Averina, E S; Müller, R H; Popov, D V; Radnaeva, L D

2011-05-01

At the turn of the millennium, a new generation of lipid nanoparticles for pharmacology was developed, nanostructured lipid carriers (NLC). The features of NLC structure which allow the inclusion of natural biologically active lipids in the NLC matrix open a wide prospect for the creation of high performance drug carriers. In this study NLC formulations were developed based on natural lipids from the Siberia region (Russia): fish oil from Lake Baikal fish; polyunsaturated fatty acid fractions and monounsaturated and saturated fatty acid fractions from fish oil and Siberian pine seed oil. Formulation parameters of NLC such as as type of surfactant and storage conditions were evaluated. The data obtained indicated high physical stability of NLC formulated on the basis of pure fish oil stabilized by Tween 80 and NLC formulated on the basis of free fatty acids stabilized by Poloxamer 188. The good chemical stability of the lipid matrix and the high concentrations of the biologically active polyunsaturated fatty acids in the NLC developed open wide prospects for their use in pharmaceutics and cosmetics.

Clinical validation of the nursing diagnosis of ineffective protection in haemodialysis patients.

PubMed

de Sá Tinôco, Jéssica Dantas; de Paiva, Maria das Graças Mariano Nunes; de Queiroz Frazão, Cecília Maria Farias; Lucio, Kadyjina Daiane Batista; Fernandes, Maria Isabel da Conceição Dias; de Oliveira Lopes, Marcos Venicios; de Carvalho Lira, Ana Luisa Brandão

2018-01-01

To evaluate the clinical validity of indicators of the nursing diagnosis of "ineffective protection" in haemodialysis patients. Haemodialysis patients have reduced protection. Studies on the nursing diagnosis of "ineffective protection" are scarce in the literature. The use of indicators to diagnose "ineffective protection" could improve the care of haemodialysis patients. The clinical usefulness of the indicators requires clinical validation. This was a diagnostic accuracy study. This study assessed a sample of 200 patients undergoing haemodialysis in a reference clinic for nephrology during the first half of 2015. Operational definitions were created for each clinical indicator based on concept analysis and content validation by experts for these indicators. Diagnostic accuracy measurement was performed with latent class analysis with randomised effects. The clinical indicator of "fatigue" had high sensitivity (p = .999) and specificity (p = 1.000) for the identification of "ineffective protection." Additionally, "maladaptive response to stress" (p = .711) and "coagulation change" (p = .653) were sensitive indicators. The main indicators that showed high specificity were "fever" (p = .987), "increased number of hospitalisations" (p = .911), "weakness" (p = .937), "infected vascular access" (p = .962) and "vascular access dysfunction" (p = .722). A set of nine clinical indicators of "ineffective protection" were accurate and statistically significant for haemodialysis patients. Three clinical indicators showed sensitivity, and six indicators showed specificity. Accurate measures for nursing diagnoses can help nurses confirm or rule out the probability of the occurrence of "ineffective protection" in patients undergoing haemodialysis. © 2017 John Wiley & Sons Ltd.

[Validity of indicators on physical activity and sedentary behavior from the Brazilian National School-Based Health Survey among adolescents in Rio de Janeiro, Brazil].

PubMed

Tavares, Letícia Ferreira; Castro, Inês Rugani Ribeiro de; Cardoso, Letícia Oliveira; Levy, Renata Bertazzi; Claro, Rafael Moreira; Oliveira, Andreia Ferreira de

2014-09-01

This study evaluated the relative validity of physical activity indicators from the questionnaire used in the Brazilian National School-Based Health Survey (PeNSE) in the city of Rio de Janeiro, Brazil, based on a sample of 174 students. The following indicators of weekly physical activity were evaluated: ACTIVE-300MIN (≥ 300 minutes/week); ACTIVE-150MIN (≥ 150 minutes), INACTIVE (no physical activity). Additionally, indicators of sedentary behavior were also assessed, as daily screen time (TV, videogames, and computer). The results from the questionnaire were compared with three 24-hour recalls. The results of ACTIVE-300MIN, ACTIVE-150MIN, and INACTIVE generated by PeNSE showed high accuracy. These indicators performed better than those of sedentary behavior in relation to frequency estimates as well as sensitivity, specificity, and correct classification rate. The indicators of physical activity from PeNSE showed satisfactory relative validity.

Selecting clinical quality indicators for laboratory medicine.

PubMed

Barth, Julian H

2012-05-01

Quality in laboratory medicine is often described as doing the right test at the right time for the right person. Laboratory processes currently operate under the oversight of an accreditation body which gives confidence that the process is good. However, there are aspects of quality that are not measured by these processes. These are largely focused on ensuring that the most clinically appropriate test is performed and interpreted correctly. Clinical quality indicators were selected through a two-phase process. Firstly, a series of focus groups of clinical scientists were held with the aim of developing a list of quality indicators. These were subsequently ranked in order by an expert panel of primary and secondary care physicians. The 10 top indicators included the communication of critical results, comprehensive education to all users and adequate quality assurance for point-of-care testing. Laboratories should ensure their tests are used to national standards, that they have clinical utility, are calibrated to national standards and have long-term stability for chronic disease management. Laboratories should have error logs and demonstrate evidence of measures introduced to reduce chances of similar future errors. Laboratories should make a formal scientific evaluation of analytical quality. This paper describes the process of selection of quality indicators for laboratory medicine that have been validated sequentially by deliverers and users of the service. They now need to be converted into measureable variables related to outcome and validated in practice.

A validated stability-indicating HPLC method for determination of varenicline in its bulk and tablets

PubMed Central

2011-01-01

A simple, sensitive and accurate stability-indicating HPLC method has been developed and validated for determination of varenicline (VRC) in its bulk form and pharmaceutical tablets. Chromatographic separation was achieved on a Zorbax Eclipse XDB-C8 column (150 mm × 4.6 mm i.d., particle size 5 μm, maintained at ambient temperature) by a mobile phase consisted of acetonitrile and 50 mM potassium dihydrogen phosphate buffer (10:90, v/v) with apparent pH of 3.5 ± 0.1 and a flow rate of 1.0 ml/min. The detection wavelength was set at 235 nm. VRC was subjected to different accelerated stress conditions. The degradation products, when any, were well resolved from the pure drug with significantly different retention time values. The method was linear (r = 0.9998) at a concentration range of 2 - 14 μg/ml. The limit of detection and limit of quantitation were 0.38 and 1.11 μg/ml, respectively. The intra- and inter-assay precisions were satisfactory; the relative standard deviations did not exceed 2%. The accuracy of the method was proved; the mean recovery of VRC was 100.10 ± 1.08%. The proposed method has high throughput as the analysis involved short run-time (~ 6 min). The method met the ICH/FDA regulatory requirements. The proposed method was successfully applied for the determination of VRC in bulk and tablets with acceptable accuracy and precisions; the label claim percentages were 99.65 ± 0.32%. The results demonstrated that the method would have a great value when applied in quality control and stability studies for VRC. PMID:21672253

RBANS Validity Indices: a Systematic Review and Meta-Analysis.

PubMed

Shura, Robert D; Brearly, Timothy W; Rowland, Jared A; Martindale, Sarah L; Miskey, Holly M; Duff, Kevin

2018-05-16

Neuropsychology practice organizations have highlighted the need for thorough evaluation of performance validity as part of the neuropsychological assessment process. Embedded validity indices are derived from existing measures and expand the scope of validity assessment. The Repeatable Battery for the Assessment of Neuropsychological Status (RBANS) is a brief instrument that quickly allows a clinician to assess a variety of cognitive domains. The RBANS also contains multiple embedded validity indicators. The purpose of this study was to synthesize the utility of those indicators to assess performance validity. A systematic search was completed, resulting in 11 studies for synthesis and 10 for meta-analysis. Data were synthesized on four indices and three subtests across samples of civilians, service members, and veterans. Sufficient data for meta-analysis were only available for the Effort Index, and related analyses indicated optimal cutoff scores of ≥1 (AUC = .86) and ≥ 3 (AUC = .85). However, outliers and heterogeneity were present indicating the importance of age and evaluation context. Overall, embedded validity indicators have shown adequate diagnostic accuracy across a variety of populations. Recommendations for interpreting these measures and future studies are provided.

[Balanced scorecard for performance measurement of a nursing organization in a Korean hospital].

PubMed

Hong, Yoonmi; Hwang, Kyung Ja; Kim, Mi Ja; Park, Chang Gi

2008-02-01

The purpose of this study was to develop a balanced scorecard (BSC) for performance measurement of a Korean hospital nursing organization and to evaluate the validity and reliability of performance measurement indicators. Two hundred fifty-nine nurses in a Korean hospital participated in a survey questionnaire that included 29-item performance evaluation indicators developed by investigators of this study based on the Kaplan and Norton's BSC (1992). Cronbach's alpha was used to test the reliability of the BSC. Exploratory and confirmatory factor analysis with a structure equation model (SEM) was applied to assess the construct validity of the BSC. Cronbach's alpha of 29 items was .948. Factor analysis of the BSC showed 5 principal components (eigen value >1.0) which explained 62.7% of the total variance, and it included a new one, community service. The SEM analysis results showed that 5 components were significant for the hospital BSC tool. High degree of reliability and validity of this BSC suggests that it may be used for performance measurements of a Korean hospital nursing organization. Future studies may consider including a balanced number of nurse managers and staff nurses in the study. Further data analysis on the relationships among factors is recommended.

Molecular gated-AlGaN/GaN high electron mobility transistor for pH detection.

PubMed

Ding, Xiangzhen; Yang, Shuai; Miao, Bin; Gu, Le; Gu, Zhiqi; Zhang, Jian; Wu, Baojun; Wang, Hong; Wu, Dongmin; Li, Jiadong

2018-04-18

A molecular gated-AlGaN/GaN high electron mobility transistor has been developed for pH detection. The sensing surface of the sensor was modified with 3-aminopropyltriethoxysilane to provide amphoteric amine groups, which would play the role of receptors for pH detection. On modification with 3-aminopropyltriethoxysilane, the transistor exhibits good chemical stability in hydrochloric acid solution and is sensitive for pH detection. Thus, our molecular gated-AlGaN/GaN high electron mobility transistor acheived good electrical performances such as chemical stability (remained stable in hydrochloric acid solution), good sensitivity (37.17 μA/pH) and low hysteresis. The results indicate a promising future for high-quality sensors for pH detection.

Validation of reference genes aiming accurate normalization of qRT-PCR data in Dendrocalamus latiflorus Munro.

PubMed

Liu, Mingying; Jiang, Jing; Han, Xiaojiao; Qiao, Guirong; Zhuo, Renying

2014-01-01

Dendrocalamus latiflorus Munro distributes widely in subtropical areas and plays vital roles as valuable natural resources. The transcriptome sequencing for D. latiflorus Munro has been performed and numerous genes especially those predicted to be unique to D. latiflorus Munro were revealed. qRT-PCR has become a feasible approach to uncover gene expression profiling, and the accuracy and reliability of the results obtained depends upon the proper selection of stable reference genes for accurate normalization. Therefore, a set of suitable internal controls should be validated for D. latiflorus Munro. In this report, twelve candidate reference genes were selected and the assessment of gene expression stability was performed in ten tissue samples and four leaf samples from seedlings and anther-regenerated plants of different ploidy. The PCR amplification efficiency was estimated, and the candidate genes were ranked according to their expression stability using three software packages: geNorm, NormFinder and Bestkeeper. GAPDH and EF1α were characterized to be the most stable genes among different tissues or in all the sample pools, while CYP showed low expression stability. RPL3 had the optimal performance among four leaf samples. The application of verified reference genes was illustrated by analyzing ferritin and laccase expression profiles among different experimental sets. The analysis revealed the biological variation in ferritin and laccase transcript expression among the tissues studied and the individual plants. geNorm, NormFinder, and BestKeeper analyses recommended different suitable reference gene(s) for normalization according to the experimental sets. GAPDH and EF1α had the highest expression stability across different tissues and RPL3 for the other sample set. This study emphasizes the importance of validating superior reference genes for qRT-PCR analysis to accurately normalize gene expression of D. latiflorus Munro.

A framework to assess management performance in district health systems: a qualitative and quantitative case study in Iran.

PubMed

Tabrizi, Jafar Sadegh; Gholipour, Kamal; Iezadi, Shabnam; Farahbakhsh, Mostafa; Ghiasi, Akbar

2018-01-01

The aim was to design a district health management performance framework for Iran's healthcare system. The mixed-method study was conducted between September 2015 and May 2016 in Tabriz, Iran. In this study, the indicators of district health management performance were obtained by analyzing the 45 semi-structured surveys of experts in the public health system. Content validity of performance indicators which were generated in qualitative part were reviewed and confirmed based on content validity index (CVI). Also content validity ratio (CVR) was calculated using data acquired from a survey of 21 experts in quantitative part. The result of this study indicated that, initially, 81 indicators were considered in framework of district health management performance and, at the end, 53 indicators were validated and confirmed. These indicators were classified in 11 categories which include: human resources and organizational creativity, management and leadership, rules and ethics, planning and evaluation, district managing, health resources management and economics, community participation, quality improvement, research in health system, health information management, epidemiology and situation analysis. The designed framework model can be used to assess the district health management and facilitates performance improvement at the district level.

Guidelines for the practical stability studies of anticancer drugs: a European consensus conference.

PubMed

Bardin, C; Astier, A; Vulto, A; Sewell, G; Vigneron, J; Trittler, R; Daouphars, M; Paul, M; Trojniak, M; Pinguet, F

2011-07-01

Stability studies performed by the pharmaceutical industry are only designed to fulfill licensing requirements. Thus, post-dilution or -reconstitution stability data are frequently limited to 24h only for bacteriological reasons regardless of the true chemical stability which could, in many cases, be longer. In practice, the pharmacy-based centralized preparation may require infusions to be made several days in advance to provide, for example, the filling of ambulatory devices for continuous infusions or batch preparations for dose banding. Furthermore, a non-justified limited stability for expensive products is obviously very costly. Thus, there is a compelling need for additional stability data covering practical uses of anticancer drugs. A European conference consensus was held in France, May 2010, under the auspices of the French Society of Oncology Pharmacy (SFPO) to propose adapted rules on stability in practical situations and guidelines to perform corresponding stability studies. For each anticancer drug, considering their therapeutic index, the pharmacokinetics/pharmacodynamics (PK/PD) variability, specific clinical use and risks related to degradation products, the classical limit of 10% of degradation can be inappropriate. Therefore, acceptance limits must be clinically relevant and should be defined for each drug individually. Design of stability studies has to reflect the different needs of the clinical practice (preparation for the week-ends, outpatient transportations, implantable devices, dose banding…). It is essential to use validated stability-indicating methods, separating degradation products being formed in the practical use of the drug. Sequential temperature designs should be encouraged to replicate problems seen in daily practice such as rupture of the cold-chain or temperature-cycling between refrigerated storage and ambient in-use conditions. Stressed conditions are recommended to evaluate not only the role of classical variables (pH, temperature, light) but also the mechanical stress. Physical stability such as particles' formation should be systematically evaluated. The consensus conference focused on the need to perform more studies on the stability of biotherapies, including a minimum of three complementary separating methods and a careful evaluation of submicron aggregates. The determination of the biological activity of proteins could be also useful. A guideline on the practical stability of anticancer drugs is proposed to cover current clinical and pharmaceutical practice. It should contribute to improved security of use, optimization of centralized handling and reduced costs. Finally, we have attempted to establish a new drug stability paradigm based on practical clinical needs, to complement regulatory guidelines which are essentially orientated to the stability of manufactured drugs. Copyright © 2011 Elsevier Masson SAS. All rights reserved.

Green Synthesis of Robust, Biocompatible Silver Nanoparticles Using Garlic Extract

PubMed Central

Von White, Gregory; Kerscher, Petra; Brown, Ryan M.; Morella, Jacob D.; McAllister, William; Dean, Delphine; Kitchens, Christopher L.

2012-01-01

This paper details a facile approach for the synthesis of stable and monodisperse silver nanoparticles performed at ambient/low temperature where Allium sativum (garlic) extract functions as the silver salt reducing agent during nanoparticle synthesis as well as the post-synthesis stabilizing ligands. Varying the synthesis conditions provides control of particle size, size-distribution, and kinetics of particle formation. Infrared spectroscopy, energy dispersive x-ray chemical analysis, and high performance liquid chromatography indicated that the carbohydrates present in the garlic extract are the most likely nanoparticle stabilizing chemistry. The synthesized silver nanoparticles also demonstrate potential for biomeical applications, owing to the 1) enhanced stability in biological media, 2) resistance to oxidation by the addition of H2O2, 3) ease and scalability of synthesis, and 4) lack of harsh chemicals required for synthesis. Cytotoxicity assays indicated no decrease in cellular proliferation for vascular smooth muscle cells and 3T3 fibroblasts at a concentration of 25 μg/ml, confirming that garlic extract prepared silver nanoparticles are ideal candidates for future experimentation and implementation into biomedical applications. PMID:24683414

Green Synthesis of Robust, Biocompatible Silver Nanoparticles Using Garlic Extract.

PubMed

Von White, Gregory; Kerscher, Petra; Brown, Ryan M; Morella, Jacob D; McAllister, William; Dean, Delphine; Kitchens, Christopher L

2012-01-01

This paper details a facile approach for the synthesis of stable and monodisperse silver nanoparticles performed at ambient/low temperature where Allium sativum (garlic) extract functions as the silver salt reducing agent during nanoparticle synthesis as well as the post-synthesis stabilizing ligands. Varying the synthesis conditions provides control of particle size, size-distribution, and kinetics of particle formation. Infrared spectroscopy, energy dispersive x-ray chemical analysis, and high performance liquid chromatography indicated that the carbohydrates present in the garlic extract are the most likely nanoparticle stabilizing chemistry. The synthesized silver nanoparticles also demonstrate potential for biomeical applications, owing to the 1) enhanced stability in biological media, 2) resistance to oxidation by the addition of H 2 O 2 , 3) ease and scalability of synthesis, and 4) lack of harsh chemicals required for synthesis. Cytotoxicity assays indicated no decrease in cellular proliferation for vascular smooth muscle cells and 3T3 fibroblasts at a concentration of 25 μg/ml, confirming that garlic extract prepared silver nanoparticles are ideal candidates for future experimentation and implementation into biomedical applications.

Vibrational Properties of High- Superconductors Levitated Above a Bipolar Permanent Magnetic Guideway

NASA Astrophysics Data System (ADS)

Liu, Lu; Wang, Jiasu

2014-05-01

A bipolar permanent magnetic guideway (PMG) has a unique magnetic field distribution profile which may introduce a better levitation performance and stability to the high- superconducting (HTS) maglev system. The dynamic vibration properties of multiple YBCO bulks arranged into different arrays positioned above a bipolar PMG and free to levitate were investigated. The acceleration and resonance frequencies were experimentally measured, and the stiffness and damping coefficients were evaluated for dynamic stability. Results indicate that the levitation stiffness is closely related to the field-cooling-height and sample positioning. The damping ratio was found to be low and nonlinear for the Halbach bipolar HTS-PMG system.

Reliability and criterion-related validity testing (construct) of the Endotracheal Suction Assessment Tool (ESAT©).

PubMed

Davies, Kylie; Bulsara, Max K; Ramelet, Anne-Sylvie; Monterosso, Leanne

2018-05-01

To establish criterion-related construct validity and test-retest reliability for the Endotracheal Suction Assessment Tool© (ESAT©). Endotracheal tube suction performed in children can significantly affect clinical stability. Previously identified clinical indicators for endotracheal tube suction were used as criteria when designing the ESAT©. Content validity was reported previously. The final stages of psychometric testing are presented. Observational testing was used to measure construct validity and determine whether the ESAT© could guide "inexperienced" paediatric intensive care nurses' decision-making regarding endotracheal tube suction. Test-retest reliability of the ESAT© was performed at two time points. The researchers and paediatric intensive care nurse "experts" developed 10 hypothetical clinical scenarios with predetermined endotracheal tube suction outcomes. "Experienced" (n = 12) and "inexperienced" (n = 14) paediatric intensive care nurses were presented with the scenarios and the ESAT© guiding decision-making about whether to perform endotracheal tube suction for each scenario. Outcomes were compared with those predetermined by the "experts" (n = 9). Test-retest reliability of the ESAT© was measured at two consecutive time points (4 weeks apart) with "experienced" and "inexperienced" paediatric intensive care nurses using the same scenarios and tool to guide decision-making. No differences were observed between endotracheal tube suction decisions made by "experts" (n = 9), "inexperienced" (n = 14) and "experienced" (n = 12) nurses confirming the tool's construct validity. No differences were observed between groups for endotracheal tube suction decisions at T1 and T2. Criterion-related construct validity and test-retest reliability of the ESAT© were demonstrated. Further testing is recommended to confirm reliability in the clinical setting with the "inexperienced" nurse to guide decision-making related to endotracheal tube suction. The ESAT© is the first validated tool to systematically guide endotracheal nursing practice for the "inexperienced" nurse. © 2018 John Wiley & Sons Ltd.

Clinical Validation of the Nursing Outcome "Swallowing Status" in People with Stroke: Analysis According to the Classical and Item Response Theories.

PubMed

Oliveira-Kumakura, Ana Railka de Souza; de Araujo, Thelma Leite; Costa, Alice Gabrielle de Sousa; Cavalcante, Tahissa Frota; Lopes, Marcos Venícios de Oliveira; Carvalho, Emilia Campos

2017-09-19

To validate clinically the nursing outcome "Swallowing status". The adjustment of the nursing outcome was investigated according to the Classical and Item Response Theories. The models were compared regarding information loss, goodness-of-fit, and differential item functioning. Stability and internal consistency were examined. The nursing outcome has the best fit in the generalized partial credit model with different discrimination parameters. Strong correlations among the scores of each indicator were observed. There was no differential item functioning of the outcome indicators. The scale presented high internal consistency (Cronbach's α = .954) and stability (and > .800). This study presents a valid nursing outcome. Most accurate monitoring of sensitivity to an intervention. Validar clinicamente o resultado de enefermagem "Estado da Deglutição". MÉTODOS: O ajustamento do resultado foi investigado de acordo com as teorias Clássica e de Resposta ao Item. Os modelos foram comparados assumindo parâmetros de itens cruzados de igual discriminação. Investigaram-se as propriedades de bondade do ajuste, funcionamento diferencial dos itens, estabilidade e consistência interna. O resultado se ajustou melhor a partir do Modelo de crédito parcial generalizado, o qual demonstrou unidimensionalidade do resultado e forte correlação entre os escores de cada indicador. Não houve funcionamento diferencial dos indicadores. A consistência interna para a escala global (Cronbach's α = .954) e a estabilidade (>.800) mantiveram-se elevadas. CONCLUSÃO: O estudo apresenta um resultado de enfermagem válido. RELEVÂNCIA PARA A PRÁTICA CLÍNICA: Maior acurácia para monitorar a sensibilidade da intervenção. © 2017 NANDA International, Inc.

Validity and reliability of Arabic MOS social support survey.

PubMed

Dafaalla, Mohamed; Farah, Abdulraheem; Bashir, Sheima; Khalil, Ammar; Abdulhamid, Rabab; Mokhtar, Mousab; Mahadi, Mohamed; Omer, Zulfa; Suliman, Asgad; Elkhalifa, Mohammed; Abdelgadir, Hanin; Kheir, Abdelmoneim E M; Abdalrahman, Ihab

2016-01-01

We aimed to generate a valid reliable Arabic version of MOS social support survey (MOS-SSS). We did a cross sectional study in medical students of Faculty of Medicine in Khartoum, Sudan. We did a clustered random sampling in 500 students of which 487 were suitable for analysis. We followed the standard translation process for translating the MOS-SSS. We accomplished factor analysis to assess construct validity, and generated item-scales correlations to evaluate the convergent and discriminant validity. We extracted the Cronbach's α and Spearman Brown coefficient of spit half method to determine internal consistency. We measured stability by correlation between the scores of the MOS survey taken at two different occasions with ten days apart in 252 participants. All items correlated highly (0.788 or greater) with their hypothesized scales. All items in subscales correlated higher by two standard errors with their own scale than with any other scale. Principle component analysis with varimax rotation was conducted on the 19 items and examination of scree plot graphically suggested 4 predominant factors that account for 72 % of variance. It showed high loadings, ranging from 0.720 to 0.84 for items of emotional support, 0.699-0.845 for tangible support, 0.518-0.823 for affectionate support, and 0.740-0.816 for positive social interaction. Cronbach's alpha for overall MOS scale and subscales indicated high internal consistency. The test-retest correlation showed weak correlation between the test and retest (ranges from 0.04 to 0.104). The Arabic MOS-SSS had high validity and internal consistency.

Validation of the INCEPT: A Multisource Feedback Tool for Capturing Different Perspectives on Physicians' Professional Performance.

PubMed

van der Meulen, Mirja W; Boerebach, Benjamin C M; Smirnova, Alina; Heeneman, Sylvia; Oude Egbrink, Mirjam G A; van der Vleuten, Cees P M; Arah, Onyebuchi A; Lombarts, Kiki M J M H

2017-01-01

Multisource feedback (MSF) instruments are used to and must feasibly provide reliable and valid data on physicians' performance from multiple perspectives. The "INviting Co-workers to Evaluate Physicians Tool" (INCEPT) is a multisource feedback instrument used to evaluate physicians' professional performance as perceived by peers, residents, and coworkers. In this study, we report on the validity, reliability, and feasibility of the INCEPT. The performance of 218 physicians was assessed by 597 peers, 344 residents, and 822 coworkers. Using explorative and confirmatory factor analyses, multilevel regression analyses between narrative and numerical feedback, item-total correlations, interscale correlations, Cronbach's α and generalizability analyses, the psychometric qualities, and feasibility of the INCEPT were investigated. For all respondent groups, three factors were identified, although constructed slightly different: "professional attitude," "patient-centeredness," and "organization and (self)-management." Internal consistency was high for all constructs (Cronbach's α ≥ 0.84 and item-total correlations ≥ 0.52). Confirmatory factor analyses indicated acceptable to good fit. Further validity evidence was given by the associations between narrative and numerical feedback. For reliable total INCEPT scores, three peer, two resident and three coworker evaluations were needed; for subscale scores, evaluations of three peers, three residents and three to four coworkers were sufficient. The INCEPT instrument provides physicians performance feedback in a valid and reliable way. The number of evaluations to establish reliable scores is achievable in a regular clinical department. When interpreting feedback, physicians should consider that respondent groups' perceptions differ as indicated by the different item clustering per performance factor.

Analysis of the aging/stability process of organic solar cells based on PTB7:[70]PCBM and an alternative free-vacuum deposited cathode: the effect of active layer scaling

NASA Astrophysics Data System (ADS)

Barreiro-Argüelles, Denisse; Ramos-Ortiz, Gabriel; Maldonado, José-Luis L.; Romero-Borja, Daniel; Meneses-Nava, Marco-Antonio; Pérez-Gutiérrez, Enrique

2017-08-01

The PV performance and aging/stability of organic photovoltaic (OPV) devices based on the well-known system PTB7:[70]PCBM and an alternative air-stable electrode deposited at room conditions are fully studied when the active area is scaled by a factor of 25. On the other hand, the aging/stability processes were also studied through single diode model, impedance spectroscopy and light-beam induced current (LBIC) measurements in accordance with the established ISOS-D1 (dark storage) and ISOS-L1 (illumination conditions) protocols. Results are a good indication that the alternative cathode Field's metal (FM) cathode works as an encapsulating material and provides excellent PV performance comparable with the common and costly high-vacuum evaporated Al cathode.

A Multi-Domain Self-Report Measure of Coparenting

PubMed Central

Feinberg, Mark E.; Brown, Louis D.; Kan, Marni L.

2012-01-01

SYNOPSIS Objective This study reports the psychometric properties of a multi-domain measure of the coparenting relationship in dual-parent families. Method 152 couples participating in a transition to parenthood study completed the Coparenting Relationship Scale and additional measures during home visits at child age 6 months, 1 year, and 3 years. Results Psychometric and construct validity assessments indicated the measure performed satisfactorily. The 35-item measure demonstrated good reliability and strong stability. Subscales measuring theoretically and empirically important aspects of coparenting (coparenting agreement, coparenting closeness, exposure of child to conflict, coparenting support, coparenting undermining, endorsement of partner’s parenting, and division of labor) demonstrated good reliability as well. A 14-item brief overall measure showed very strong associations with the overall measure. Relations of the full scale with a measure of social desirability were weak, and the full scale was positively associated with positive dimensions of the dyadic couple relationship (love, sex/romance, couple efficacy) and inversely associated with negative dimensions (conflict, ineffective arguing)—as expected. Conclusions This initial examination of the Coparenting Relationship Scale suggests that it possesses good psychometric properties (reliability, stability, construct validity, and inter-rater agreement), can be flexibly administered in short and long forms, and is positioned to promote further conceptual and methodological progress in the study of coparenting. PMID:23166477

Stability analysis of implicit time discretizations for the Compton-scattering Fokker-Planck equation

NASA Astrophysics Data System (ADS)

Densmore, Jeffery D.; Warsa, James S.; Lowrie, Robert B.; Morel, Jim E.

2009-09-01

The Fokker-Planck equation is a widely used approximation for modeling the Compton scattering of photons in high energy density applications. In this paper, we perform a stability analysis of three implicit time discretizations for the Compton-Scattering Fokker-Planck equation. Specifically, we examine (i) a Semi-Implicit (SI) scheme that employs backward-Euler differencing but evaluates temperature-dependent coefficients at their beginning-of-time-step values, (ii) a Fully Implicit (FI) discretization that instead evaluates temperature-dependent coefficients at their end-of-time-step values, and (iii) a Linearized Implicit (LI) scheme, which is developed by linearizing the temperature dependence of the FI discretization within each time step. Our stability analysis shows that the FI and LI schemes are unconditionally stable and cannot generate oscillatory solutions regardless of time-step size, whereas the SI discretization can suffer from instabilities and nonphysical oscillations for sufficiently large time steps. With the results of this analysis, we present time-step limits for the SI scheme that prevent undesirable behavior. We test the validity of our stability analysis and time-step limits with a set of numerical examples.

Development and Validation of a High-Performance Thin-Layer Chromatographic Method for the Simultaneous Determination of Two Binary Mixtures Containing Ketorolac Tromethamine with Phenylephrine Hydrochloride and with Febuxostat

PubMed Central

El Yazbi, Fawzy A.; Hassan, Ekram M.; Khamis, Essam F.; Ragab, Marwa A.A.; Hamdy, Mohamed M.A.

2016-01-01

A validated and highly selective high-performance thin-layer chromatography (HPTLC) method was developed for the determination of ketorolac tromethamine (KTC) with phenylephrine hydrochloride (PHE) (Mixture 1) and with febuxostat (FBX) (Mixture 2) in bulk drug and in combined dosage forms. The proposed method was based on HPTLC separation of the drugs followed by densitometric measurements of their spots at 273 and 320 nm for Mixtures 1 and 2, respectively. The separation was carried out on Merck HPTLC aluminum sheets of silica gel 60 F254 using chloroform–methanol–ammonia (7:3:0.1, v/v) and (7.5:2.5:0.1, v/v) as mobile phase for KTC/PHE and KTC/FBX mixtures, respectively. Linear regression lines were obtained over the concentration ranges 0.20–0.60 and 0.60–1.95 µg band−1 for KTC and PHE (Mixture 1), respectively, and 0.10–1.00 and 0.25–2.50 µg band−1 for KTC and FBX (Mixture 2), respectively, with correlation coefficients higher than 0.999. The method was successfully applied to the analysis of the two drugs in their synthetic mixtures and in their dosage forms. The mean percentage recoveries were in the range of 98–102%, and the RSD did not exceed 2%. The method was validated according to ICH guidelines and showed good performances in terms of linearity, sensitivity, precision, accuracy and stability. PMID:26847918

The stability of liquid-filled matrix ionization chamber electronic portal imaging devices for dosimetry purposes.

PubMed

Louwe, R J W; Tielenburg, R; van Ingen, K M; Mijnheer, B J; van Herk, M B

2004-04-01

This study was performed to determine the stability of liquid-filled matrix ionization chamber (LiFi-type) electronic portal imaging devices (EPID) for dosimetric purposes. The short- and long-term stability of the response was investigated, as well as the importance of factors influencing the response (e.g., temperature fluctuations, radiation damage, and the performance of the electronic hardware). It was shown that testing the performance of the electronic hardware as well as the short-term stability of the imagers may reveal the cause of a poor long-term stability of the imager response. In addition, the short-term stability was measured to verify the validity of the fitted dose-response curve immediately after beam startup. The long-term stability of these imagers could be considerably improved by correcting for room temperature fluctuations and gradual changes in response due to radiation damage. As a result, the reproducibility was better than 1% (1 SD) over a period of two years. The results of this study were used to formulate recommendations for a quality control program for portal dosimetry. The effect of such a program was assessed by comparing the results of portal dosimetry and in vivo dosimetry using diodes during the treatment of 31 prostate patients. The improvement of the results for portal dosimetry was consistent with the deviations observed with the reproducibility tests in that particular period. After a correction for the variation in response of the imager, the average difference between the measured and prescribed dose during the treatment of prostate patients was -0.7%+/-1.5% (1 SD), and -0.6%+/-1.1% (1 SD) for EPID and diode in vivo dosimetry, respectively. It can be concluded that a high stability of the response can be achieved for this type of EPID by applying a rigorous quality control program.

High fidelity simulation and analysis of liquid jet atomization in a gaseous crossflow at intermediate Weber numbers

NASA Astrophysics Data System (ADS)

Li, Xiaoyi; Soteriou, Marios C.

2016-08-01

Recent advances in numerical methods coupled with the substantial enhancements in computing power and the advent of high performance computing have presented first principle, high fidelity simulation as a viable tool in the prediction and analysis of spray atomization processes. The credibility and potential impact of such simulations, however, has been hampered by the relative absence of detailed validation against experimental evidence. The numerical stability and accuracy challenges arising from the need to simulate the high liquid-gas density ratio across the sharp interfaces encountered in these flows are key reasons for this. In this work we challenge this status quo by presenting a numerical model able to deal with these challenges, employing it in simulations of liquid jet in crossflow atomization and performing extensive validation of its results against a carefully executed experiment with detailed measurements in the atomization region. We then proceed to the detailed analysis of the flow physics. The computational model employs the coupled level set and volume of fluid approach to directly capture the spatiotemporal evolution of the liquid-gas interface and the sharp-interface ghost fluid method to stably handle high liquid-air density ratio. Adaptive mesh refinement and Lagrangian droplet models are shown to be viable options for computational cost reduction. Moreover, high performance computing is leveraged to manage the computational cost. The experiment selected for validation eliminates the impact of inlet liquid and gas turbulence and focuses on the impact of the crossflow aerodynamic forces on the atomization physics. Validation is demonstrated by comparing column surface wavelengths, deformation, breakup locations, column trajectories and droplet sizes, velocities, and mass rates for a range of intermediate Weber numbers. Analysis of the physics is performed in terms of the instability and breakup characteristics and the features of downstream flow recirculation, and vortex shedding. Formation of "Λ" shape windward column waves is observed and explained by the combined upward and lateral surface motion. The existence of Rayleigh-Taylor instability as the primary mechanism for the windward column waves is verified for this case by comparing wavelengths from the simulations to those predicted by linear stability analyses. Physical arguments are employed to postulate that the type of instability manifested may be related to conditions such as the gas Weber number and the inlet turbulence level. The decreased column wavelength with increasing Weber number is found to cause enhanced surface stripping and early depletion of liquid core at higher Weber number. A peculiar "three-streak-two-membrane" liquid structure is identified at the lowest Weber number and explained as the consequence of the symmetric recirculation zones behind the jet column. It is found that the vortical flow downstream of the liquid column resembles a von Karman vortex street and that the coupling between the gas flow and droplet transport is weak for the conditions explored.

High fidelity simulation and analysis of liquid jet atomization in a gaseous crossflow at intermediate Weber numbers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Xiaoyi, E-mail: lixy2@utrc.utc.com; Soteriou, Marios C.

Recent advances in numerical methods coupled with the substantial enhancements in computing power and the advent of high performance computing have presented first principle, high fidelity simulation as a viable tool in the prediction and analysis of spray atomization processes. The credibility and potential impact of such simulations, however, has been hampered by the relative absence of detailed validation against experimental evidence. The numerical stability and accuracy challenges arising from the need to simulate the high liquid-gas density ratio across the sharp interfaces encountered in these flows are key reasons for this. In this work we challenge this status quomore » by presenting a numerical model able to deal with these challenges, employing it in simulations of liquid jet in crossflow atomization and performing extensive validation of its results against a carefully executed experiment with detailed measurements in the atomization region. We then proceed to the detailed analysis of the flow physics. The computational model employs the coupled level set and volume of fluid approach to directly capture the spatiotemporal evolution of the liquid-gas interface and the sharp-interface ghost fluid method to stably handle high liquid-air density ratio. Adaptive mesh refinement and Lagrangian droplet models are shown to be viable options for computational cost reduction. Moreover, high performance computing is leveraged to manage the computational cost. The experiment selected for validation eliminates the impact of inlet liquid and gas turbulence and focuses on the impact of the crossflow aerodynamic forces on the atomization physics. Validation is demonstrated by comparing column surface wavelengths, deformation, breakup locations, column trajectories and droplet sizes, velocities, and mass rates for a range of intermediate Weber numbers. Analysis of the physics is performed in terms of the instability and breakup characteristics and the features of downstream flow recirculation, and vortex shedding. Formation of “Λ” shape windward column waves is observed and explained by the combined upward and lateral surface motion. The existence of Rayleigh-Taylor instability as the primary mechanism for the windward column waves is verified for this case by comparing wavelengths from the simulations to those predicted by linear stability analyses. Physical arguments are employed to postulate that the type of instability manifested may be related to conditions such as the gas Weber number and the inlet turbulence level. The decreased column wavelength with increasing Weber number is found to cause enhanced surface stripping and early depletion of liquid core at higher Weber number. A peculiar “three-streak-two-membrane” liquid structure is identified at the lowest Weber number and explained as the consequence of the symmetric recirculation zones behind the jet column. It is found that the vortical flow downstream of the liquid column resembles a von Karman vortex street and that the coupling between the gas flow and droplet transport is weak for the conditions explored.« less

Towards a "Golden Standard" for computing globin stability: Stability and structure sensitivity of myoglobin mutants.

PubMed

Kepp, Kasper P

2015-10-01

Fast and accurate computation of protein stability is increasingly important for e.g. protein engineering and protein misfolding diseases, but no consensus methods exist for important proteins such as globins, and performance may depend on the type of structural input given. This paper reports benchmarking of six protein stability calculators (POPMUSIC 2.1, I-Mutant 2.0, I-Mutant 3.0, CUPSAT, SDM, and mCSM) against 134 experimental stability changes for mutations of sperm-whale myoglobin. Six different high-resolution structures were used to test structure sensitivity that may impair protein calculations. The trend accuracy of the methods decreased as I-Mutant 2.0 (R=0.64-0.65), SDM (R=0.57-0.60), POPMUSIC2.1 (R=0.54-0.57), I-Mutant 3.0 (R=0.53-0.55), mCSM (R=0.35-0.47), and CUPSAT (R=0.25-0.48). The mean signed errors increased as SDM

Space Environment Effects on Stability of Medications Flown on Space Shuttles and the International Space Station (ISS)

NASA Technical Reports Server (NTRS)

Daniels, Vernie; Du, Jianping; Crady, Camille; Satterfield, Rick; Putcha, Lakshmi

2007-01-01

The purpose is to assess physical and chemical degradation of select pharmaceutical formulations from the Shuttle and ISS medical kits. Eleven pharmaceuticals dispensed as different dosage forms were selected based on their physical / chemical characteristics and susceptibility to environmental factors such as, temperature, humidity and light sensitivity. When available, ground-controls of the study medications with matching brand and lot numbers were used for comparison. Samples retrieved from flight were stored along with their matching controls in a temperature and humidity controlled environmental chamber. Temperature, humidity, and radiation data from the Shuttle and ISS were retrieved from onboard HOBO U12 Temp/RH Data Loggers, and from passive dosimeters. Physical and chemical analyses of the pharmaceuticals were conducted using validated United States Pharmacopeia (USP) methods. Results indicated degradation of 6 of the 11 formulations returned from space flights. Four formulations, Amoxicillin / Clavulanate, promethazine, sulfamethoxazole / trimethoprim, and ciprofloxacin tablets depicted discoloration after flight. Chemical content analyses using High or Ultra Performance Liquid Chromatography (HPLC / UPLC) methods revealed that dosage forms of Amoxicillin / Clavulanate, promethazine, sulfamethoxazole / trimethoprim, lidocaine, ciprofloxacin and mupirocin contained less than 95% of manufacturer s labeled claim of active drug compound. Shuttle and ISS environments affect stability and shelf life of certain mediations flown on these missions. Data analysis is in progress to examine the effect of specific space flight environmental factors on pharmaceutical stability. The degradation profiles generated from ground studies in analog environments will be useful in establishing predictive shelf-life profiles for medications intended for use during long-term space exploration missions.

Long-Term Stability of Tramadol and Ketamine Solutions for Patient-Controlled Analgesia Delivery.

PubMed

Gu, Junfeng; Qin, Wengang; Chen, Fuchao; Xia, Zhongyuan

2015-08-26

Subanesthetic doses of ketamine as an adjuvant to tramadol in patient-controlled analgesia (PCA) for postoperative pain have been shown to improve the quality of analgesia. However, there are no such commercially available drug mixtures, and the stability of the combination has rarely been assessed. Admixtures were assessed for periods of up to 14 days at 4°C and 25°C. Three different mixtures of tramadol and ketamine (tramadol 5.0 mg/mL + ketamine 0.5 mg/mL, tramadol 5.0 mg/mL + ketamine 1.0 mg/mL, and tramadol 5.0 mg/mL + ketamine 2.0 mg/mL) were prepared in polyolefin bags by combining these 2 drugs with 0.9% sodium chloride (normal saline [NS]). The chemical stability of the admixtures was evaluated by a validated high-performance liquid chromatography (HPLC) method and by measurement of pH values. Solution appearance and color were assessed by observing the samples against black and white backgrounds. Solutions were considered stable if they maintained 90% of the initial concentration of each drug. The percentages of initial concentration of tramadol and ketamine in the various solutions remained above 98% when stored at 4°C or 25°C over the testing period. No changes in color or turbidity were observed in any of the prepared solutions. Throughout this period, pH values remained stable. The results indicate that the drug mixtures of tramadol with ketamine in NS for PCA delivery systems were stable for 14 days when stored in polyolefin bags at 4°C or 25°C.

Enzyme stabilization via computationally guided protein stapling.

PubMed

Moore, Eric J; Zorine, Dmitri; Hansen, William A; Khare, Sagar D; Fasan, Rudi

2017-11-21

Thermostabilization represents a critical and often obligatory step toward enhancing the robustness of enzymes for organic synthesis and other applications. While directed evolution methods have provided valuable tools for this purpose, these protocols are laborious and time-consuming and typically require the accumulation of several mutations, potentially at the expense of catalytic function. Here, we report a minimally invasive strategy for enzyme stabilization that relies on the installation of genetically encoded, nonreducible covalent staples in a target protein scaffold using computational design. This methodology enables the rapid development of myoglobin-based cyclopropanation biocatalysts featuring dramatically enhanced thermostability (Δ T m = +18.0 °C and Δ T 50 = +16.0 °C) as well as increased stability against chemical denaturation [Δ C m (GndHCl) = 0.53 M], without altering their catalytic efficiency and stereoselectivity properties. In addition, the stabilized variants offer superior performance and selectivity compared with the parent enzyme in the presence of a high concentration of organic cosolvents, enabling the more efficient cyclopropanation of a water-insoluble substrate. This work introduces and validates an approach for protein stabilization which should be applicable to a variety of other proteins and enzymes.

Boundary-Layer Stability Analysis of the Mean Flows Obtained Using Unstructured Grids

NASA Technical Reports Server (NTRS)

Liao, Wei; Malik, Mujeeb R.; Lee-Rausch, Elizabeth M.; Li, Fei; Nielsen, Eric J.; Buning, Pieter G.; Chang, Chau-Lyan; Choudhari, Meelan M.

2012-01-01

Boundary-layer stability analyses of mean flows extracted from unstructured-grid Navier- Stokes solutions have been performed. A procedure has been developed to extract mean flow profiles from the FUN3D unstructured-grid solutions. Extensive code-to-code validations have been performed by comparing the extracted mean ows as well as the corresponding stability characteristics to the predictions based on structured-grid solutions. Comparisons are made on a range of problems from a simple at plate to a full aircraft configuration-a modified Gulfstream-III with a natural laminar flow glove. The future aim of the project is to extend the adjoint-based design capability in FUN3D to include natural laminar flow and laminar flow control by integrating it with boundary-layer stability analysis codes, such as LASTRAC.

Assessing Fan Flutter Stability in the Presence of Inlet Distortion Using One-way and Two-way Coupled Methods

NASA Technical Reports Server (NTRS)

Herrick, Gregory P.

2014-01-01

Concerns regarding noise, propulsive efficiency, and fuel burn are inspiring aircraft designs wherein the propulsive turbomachines are partially (or fully)embedded within the airframe; such designs present serious concerns with regard to aerodynamic and aeromechanic performance of the compression system in response to inlet distortion. Previously, a preliminary design of a forward-swept high-speed fan exhibited flutter concerns in clean-inlet flows, and the present author then studied this fan further in the presence of off-design distorted in-flows. A three-dimensional, unsteady, Navier-Stokes computational fluid dynamics code is applied to analyze and corroborate fan performance with clean inlet flow. This code, already validated in its application to assess aerodynamic damping of vibrating blades at various flow conditions using a loosely-coupled approach, is modified to include a tightly-coupled aeroelastic simulation capability, and then loosely-coupled and tightly-coupled methods arecompared in their evaluation of flutter stability in distorted in-flows.

Advantages of MgAlOx over gamma-Al2O3 as a support material for potassium-based high temperature lean NOx traps

DOE Office of Scientific and Technical Information (OSTI.GOV)

Luo, Jinyong; Gao, Feng; Karim, Ayman M.

MgAlOx mixed oxides were employed as supports for potassium-based lean NOx traps (LNTs) targeted for high temperature applications. Effects of support compositions, K/Pt loadings, thermal aging and catalyst regeneration on NOx storage capacity were systematically investigated. The catalysts were characterized by XRD, NOx-TPD, TEM, STEM-HAADF and in-situ XAFS. The results indicate that MgAlOx mixed oxides have significant advantages over conventional gamma-Al2O3-supports for LNT catalysts, in terms of high temperature NOx trapping capacity and thermal stability. First, as a basic support, MgAlOx stabilizes stored nitrates (in the form of KNO3) to much higher temperatures than mildly acidic gamma-Al2O3. Second, MgAlOx minimizesmore » Pt sintering during thermal aging, which is not possible for gamma-Al2O3 supports. Notably, combined XRD, in-situ XAFS and STEM-HAADF results indicate that Pt species in the thermally aged Pt/MgAlOx samples are finely dispersed in the oxide matrix as isolated atoms. This strong metal-support interaction stabilizes Pt and minimizes the extent of sintering. However, such strong interactions result in Pt oxidation via coordination with the support so that NO oxidation activity can be adversely affected after aging which, in turn, decreases NOx trapping ability for these catalysts. Interestingly, a high-temperature reduction treatment regenerates essentially full NOx trapping performance. In fact, regenerated Pt/K/MgAlOx catalyst exhibits much better NOx trapping performance than fresh Pt/K/Al2O3 LNTs over the entire temperature range investigated here. In addition to thermal aging, Pt/K loading effects were systemically studied over the fresh samples. The results indicate that NOx trapping is kinetically limited at low temperatures, while thermodynamically limited at high temperatures. A simple conceptual model was developed to explain the Pt and K loading effects on NOx storage. An optimized K loading, which allows balancing between the stability of nitrates and exposed Pt surface, gives the best NOx trapping capability.« less

Identification and characterization of stress degradants of lacosamide by LC-MS and ESI-Q-TOF-MS/MS: development and validation of a stability indicating RP-HPLC method.

PubMed

Ramisetti, Nageswara Rao; Kuntamukkala, Ramakrishna; Lakshetti, Sridhar; Sripadi, Prabhakar

2014-07-01

The current study dealt with the degradation behavior of lacosamide (LAC) under ICH prescribed stress conditions. LAC was found to be labile under acid and base hydrolytic stress conditions, while it was stable to neutral hydrolytic, oxidative, photolytic and thermal stress. In total, seven degradation products (DPs) were formed, which were separated on a C18 column using a stability-indicating method. LC-MS analyses indicated that one of the DPs had the same molecular mass as that of the drug. Structural characterization of DPs was carried out using ESI-Q-TOF-MS/MS technique. The degradation pathways and mechanisms of degradation of the drug were delineated by carrying out the degradation in different co-solvents viz. methanol, deuterated methanol, ethanol, 1-propanol and acetonitrile. The developed LC method was validated for the determination of related substances and assay of LAC as per ICH guidelines. This study demonstrates a comprehensive approach of LAC degradation studies during its development phase. Copyright © 2014. Published by Elsevier B.V.

Stability analysis of free piston Stirling engines

NASA Astrophysics Data System (ADS)

Bégot, Sylvie; Layes, Guillaume; Lanzetta, François; Nika, Philippe

2013-03-01

This paper presents a stability analysis of a free piston Stirling engine. The model and the detailed calculation of pressures losses are exposed. Stability of the machine is studied by the observation of the eigenvalues of the model matrix. Model validation based on the comparison with NASA experimental results is described. The influence of operational and construction parameters on performance and stability issues is exposed. The results show that most parameters that are beneficial for machine power seem to induce irregular mechanical characteristics with load, suggesting that self-sustained oscillations could be difficult to maintain and control.

Spectroscopic characterization and quantitative determination of atorvastatin calcium impurities by novel HPLC method

NASA Astrophysics Data System (ADS)

Gupta, Lokesh Kumar

2012-11-01

Seven process related impurities were identified by LC-MS in the atorvastatin calcium drug substance. These impurities were identified by LC-MS. The structure of impurities was confirmed by modern spectroscopic techniques like 1H NMR and IR and physicochemical studies conducted by using synthesized authentic reference compounds. The synthesized reference samples of the impurity compounds were used for the quantitative HPLC determination. These impurities were detected by newly developed gradient, reverse phase high performance liquid chromatographic (HPLC) method. The system suitability of HPLC analysis established the validity of the separation. The analytical method was validated according to International Conference of Harmonization (ICH) with respect to specificity, precision, accuracy, linearity, robustness and stability of analytical solutions to demonstrate the power of newly developed HPLC method.

SU-E-T-675: Remote Dosimetry with a Novel PRESAGE Formulation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mein, S; Juang, T; Malcolm, J

2015-06-15

Purpose: 3D-gel dosimetry provides high-resolution treatment validation; however, scanners aren’t widely available. In remote dosimetry, dosimeters are shipped out from a central base institution to a remote site for irradiation, then shipped back for scanning and analysis, affording a convenient service for treatment validation to institutions lacking the necessary equipment and resources. Previous works demonstrated the high-resolution performance and temporal stability of PRESAGE. Here the newest formulation is investigated for remote dosimetry use. Methods: A new formulation of PRESAGE was created with the aim of improved color stability post irradiation. Dose sensitivity was determined by irradiating cuvettes on a Varianmore » Linac (6MV) from 0–15Gy and measuring change in optical density at 633nm. Sensitivity readings were tracked over time in a temperature control study to determine long-term stability. A large volume study was performed to evaluate the accuracy for remote dosimetry. A 1kg dosimeter was pre-scanned, irradiated on-site with an 8Gy 4field box treatment, post-scanned and shipped to Princess Margaret Hospital for remote reading on an identical scanner. Results: Dose sensitivities ranged from 0.0194–0.0295 ΔOD/(Gy*cm)—similar to previous formulations. Post-irradiated cuvettes stored at 10°C retained 100% initial sensitivity over 5 days and 98.6% over 10 weeks while cuvettes stored at room temperature fell to 95.8% after 5 days and 37.4% after 10 weeks. The immediate and 5-day scans of the 4field box dosimeter data was reconstructed, registered to the corresponding eclipse dose-distribution, and compared with analytical tools in CERR. Immediate and 5-day scans looked visually similar. Line profiles revealed close agreement aside from a slight elevation in dose at the edge in the 5-day readout. Conclusion: The remote dosimetry formulation exhibits excellent temporal stability in small volumes. While immediate and 5-day readout scans of large volume dosimeters show promising agreement, further development is required to reduce an apparent time dependent edge elevation.« less

Preliminary validation of the Perceived Locus of Causality scale for academic motivation in the context of university studies (PLOC-U).

PubMed

Sánchez de Miguel, Manuel; Lizaso, Izarne; Hermosilla, Daniel; Alcover, Carlos-Maria; Goudas, Marios; Arranz-Freijó, Enrique

2017-12-01

Research has shown that self-determination theory can be useful in the study of motivation in sport and other forms of physical activity. The Perceived Locus of Causality (PLOC) scale was originally designed to study both. The current research presents and validates the new PLOC-U scale to measure academic motivation in the university context. We tested levels of self-determination before and after academic examinations. Also, we analysed degree of internalization of extrinsic motivation in students' practical activities. Two hundred and eighty-seven Spanish university students participated in the study. Data were collected at two time points to check the reliability and stability of PLOC-U by a test-retest procedure. Confirmatory factor analysis was performed on the PLOC-U. Also convergent validity was tested against the Academic Motivation Scale (EME-E). Confirmatory factor analysis showed optimum fit and good reliability of PLOC-U. It also presented excellent convergent validity with the EME-E and good stability over time. Our findings did not show any significant correlation between self-determination and expected results before academic examinations, but it did so afterwards, revealing greater regulation by and integration of extrinsic motivation. The high score obtained for extrinsic motivation points to a greater regulation associated with an external contingency (rewards in the practical coursework). PLOC-U is a good instrument for the measurement of academic motivation and provides a new tool to analyse self-determination among university students. © 2017 The British Psychological Society.

Frequency stabilization for mobile satellite terminals via LORAN

NASA Technical Reports Server (NTRS)

Ernst, Gregory J.; Kee, Steven M.; Marquart, Robert C.

1990-01-01

Digital satellite communication systems require careful management of frequency stability. Historically, frequency stability has been accomplished by continuously powered, high cost, high performance reference oscillators. Today's low cost mobile satellite communication equipment must operate under wide ranging environmental conditions, stabilize quickly after application of power, and provide adequate performance margin to overcome RF link impairments unique to the land mobile environment. Methods for frequency stabilization in land mobile applications must meet these objectives without incurring excessive performance degradation. A frequency stabilization scheme utilizing the LORAN (Long Range Navigation) system is presented.

Validity and Reliability of Accelerometers in Patients With COPD: A SYSTEMATIC REVIEW.

PubMed

Gore, Shweta; Blackwood, Jennifer; Guyette, Mary; Alsalaheen, Bara

2018-05-01

Reduced physical activity is associated with poor prognosis in chronic obstructive pulmonary disease (COPD). Accelerometers have greatly improved quantification of physical activity by providing information on step counts, body positions, energy expenditure, and magnitude of force. The purpose of this systematic review was to compare the validity and reliability of accelerometers used in patients with COPD. An electronic database search of MEDLINE and CINAHL was performed. Study quality was assessed with the Strengthening the Reporting of Observational Studies in Epidemiology checklist while methodological quality was assessed using the modified Quality Appraisal Tool for Reliability Studies. The search yielded 5392 studies; 25 met inclusion criteria. The SenseWear Pro armband reported high criterion validity under controlled conditions (r = 0.75-0.93) and high reliability (ICC = 0.84-0.86) for step counts. The DynaPort MiniMod demonstrated highest concurrent validity for step count using both video and manual methods. Validity of the SenseWear Pro armband varied between studies especially in free-living conditions, slower walking speeds, and with addition of weights during gait. A high degree of variability was found in the outcomes used and statistical analyses performed between studies, indicating a need for further studies to measure reliability and validity of accelerometers in COPD. The SenseWear Pro armband is the most commonly used accelerometer in COPD, but measurement properties are limited by gait speed variability and assistive device use. DynaPort MiniMod and Stepwatch accelerometers demonstrated high validity in patients with COPD but lack reliability data.

High-performance liquid chromatographic method for potency determination of amoxicillin in commercial preparations and for stability studies.

PubMed Central

Hsu, M C; Hsu, P W

1992-01-01

A reversed-phase column liquid chromatographic method was developed for the assay of amoxicillin and its preparations. The linear calibration range was 0.2 to 2.0 mg/ml (r = 0.9998), and recoveries were generally greater than 99%. The high-performance liquid chromatographic assay results were compared with those obtained from a microbiological assay of bulk drug substance and capsule, injection, and granule formulations containing amoxicillin and degraded amoxicillin. At the 99% confidence level, no significant intermethod differences were noted for the paired results. Commercial formulations were also analyzed, and the results obtained by the proposed method closely agreed with those found by the microbiological method. The results indicated that the proposed method is a suitable substitute for the microbiological method for assays and stability studies of amoxicillin preparations. PMID:1416827

Development and application of a validated stability-indicating HPLC method for simultaneous determination of granisetron hydrochloride, benzyl alcohol and their main degradation products in parenteral dosage forms.

PubMed

Hewala, Ismail; El-Fatatre, Hamed; Emam, Ehab; Mubrouk, Mokhtar

2010-06-30

A simple, rapid and sensitive reversed phase high performance liquid chromatographic method using photodiode array detection was developed and validated for the simultaneous determination of granisetron hydrochloride, benzyl alcohol, 1-methyl-1H-indazole-3-carboxylic acid (the main degradation product of granisetron) and benzaldehyde (the main degradation product of benzyl alcohol) in granisetron injections. The separation was achieved on Hypersil BDS C8 (250 mm x 4.6 mm i.d., 5 microm particle diameter) column using a mobile phase consisted of acetonitrile:0.05 M KH(2)PO(4):triethylamine (22:100:0.15) adjusted to pH 4.8. The column was maintained at 25 degrees C and 20 microL of solutions was injected. Photodiode array detector was used to test the peak purity and the chromatograms were extracted at 210 nm. Naphazoline hydrochloride was used as internal standard. The method was validated with respect to specificity, linearity, accuracy, precision, limit of quantitation and limit of detection. The validation acceptance criteria were met in all cases. Identification of the pure peaks was carried out using library match programmer and wavelengths of derivative optima of the spectrograms of the peaks. The method was successfully applied to the determination of the investigated drugs and their degradation products in different batches of granisetron injections. The method was proved to be sensitive for the determination down to 0.03 and 0.01% of granisetron degradation product and benzaldehyde, respectively, which are far below the compendia limits for testing these degradation products in their corresponding intact drugs. Copyright 2010 Elsevier B.V. All rights reserved.

High drug load, stable, manufacturable and bioavailable fenofibrate formulations in mesoporous silica: a comparison of spray drying versus solvent impregnation methods.

PubMed

Hong, Shiqi; Shen, Shoucang; Tan, David Cheng Thiam; Ng, Wai Kiong; Liu, Xueming; Chia, Leonard S O; Irwan, Anastasia W; Tan, Reginald; Nowak, Steven A; Marsh, Kennan; Gokhale, Rajeev

2016-01-01

Encapsulation of drugs in mesoporous silica using co-spray drying process has been recently explored as potential industrial method. However, the impact of spray drying on manufacturability, physiochemical stability and bioavailability in relation to conventional drug load processes are yet to be fully investigated. Using a 2(3) factorial design, this study aims to investigate the effect of drug-loading process (co-spray drying and solvent impregnation), mesoporous silica pore size (SBA-15, 6.5 nm and MCM-41, 2.5 nm) and percentage drug load (30% w/w and 50% w/w) on material properties, crystallinity, physicochemical stability, release profiles and bioavailability of fenofibrate (FEN) loaded into mesoporous silica. From the scanning electronic microscopy (SEM) images, powder X-ray diffraction and Differential scanning calorimetry measurements, it is indicated that the co-spray drying process was able to load up to 50% (w/w) FEN in amorphous form onto the mesoporous silica as compared to the 30% (w/w) for solvent impregnation. The in vitro dissolution rate of the co-spray dried formulations was also significantly (p = 0.044) better than solvent impregnated formulations at the same drug loading. Six-month accelerated stability test at 40 °C/75 RH in open dish indicated excellent physical and chemical stability of formulations prepared by both methods. The amorphous state of FEN and the enhanced dissolution profiles were well preserved, and very low levels of degradation were detected after storage. The dog data for the three selected co-spray-dried formulations revealed multiple fold increment in FEN bioavailability compared to the reference crystalline FEN. These results validate the viability of co-spray-dried mesoporous silica formulations with high amorphous drug load as potential drug delivery systems for poorly water soluble drugs.

Chiral stability of an extemporaneously prepared clopidogrel bisulfate oral suspension.

PubMed

Tynes, Clay R; Livingston, Brad; Patel, Hetesh; Arnold, John J

2014-01-01

The purpose of this study was to evaluate the chiral stability of clopidogrel bisulfate in an extemporaneously compounded oral suspension for a period of 60 days. A 5 mg/mL oral suspension of clopidogrel bisulfate was prepared from commercially available Plavix tablets. The clopidogrel suspension was then evenly divided between two light-resistant prescription bottles and stored either under refrigeration (4°C) or at room temperature (25°C). Samples were drawn from the stored suspensions immediately after preparation and on days 7, 14, 28, and 60. Samples were subsequently analyzed at each time point by high-performance liquid chromatography using a reversed-phase column, with chemical stability defined as the retention of at least 90% of the initial intact clopidogrel concentration measured. To determine the chiral stability of the suspension, samples were also analyzed by high-performance liquid chromatography using a chiral column to investigate possible enantiomeric inversion. Chiral stability was defined as the retention of at least 90% of the initial concentration of the suspension as the S-enantiomer, the active moiety of Plavix. Regardless of storage conditions, the oral suspension of clopidogrel retained at least 98% of the active S-enantiomer for 60 days after preparation. Compared with the clopidogrel suspension stored in the refrigerator, more chiral inversion was noted in the clopidogrel suspension stored at room temperature. Our investigation of chiral stability indicates that a 5 mg/mL clopidogrel oral suspension stored under refrigeration and at room temperature maintains chiral stability as the active S-enantiomer.

Reliability and Concurrent Validity of Dynamic Rotator Stability Test-A Cross Sectional study.

PubMed

Binoy Mathew, K V; Eapen, Charu; Kumar, P Senthil

2012-01-01

To find intra rater and inter rater reliability of Dynamic Rotator Stability Test (DRST) and to find concurrent validity of Dynamic Rotator Stability Test (DRST) with University of Pennsylvania Shoulder Score (PENN) Scale. 40 subjects of either gender between the age group of 18-70 with painful shoulder conditions of musculoskeletal origin was selected through convenient sampling. Tester 1 and tester 2 administered DRST and PENN scale randomly. In a subgroup of 20 subjects DRST was administered by both the testers to find the inter rater reliability. 180° Standard Universal Goniometer was used to take measurements. For intra-rater reliability, all the test variables were showing highly significant correlation (p=.94 - 1). For inter -rater, with tester 2, test variables like position, ROM, force, direction of abnormal translation, pain during the test, compensatory movement during test were found to be significant (p=.71-1).only some variables of DRST showed significant correlation with PENN scale (P=.320-.450). Dynamic Rotator Stability Test has good intra rater and moderate inter rater reliability. Concurrent validity of Dynamic Rotator Stability Test was found to be poor when compared to PENN Shoulder Score.

Spray drying egg using either maltodextrin or nopal mucilage as stabilizer agents.

PubMed

Medina-Torres, L; Calderas, F; Nuñez Ramírez, D M; Herrera-Valencia, E E; Bernad Bernad, M J; Manero, O

2017-12-01

In this work, a comparative study between spray drying (SD) of fresh egg by either maltodextrin (MD) or nopal-mucilage (MN) as stabilizing vectors was made. The powders obtained were characterized for drying performance, moisture content, chemical proximate analysis, thermal analysis (TGA), chemical composition (FTIR), microscopy (SEM) and rheology (viscoelasticity and steady state simple shear viscosity). Infrared analysis showed that MN has the effect of a thickening agent rather than an encapsulating one. Results indicated that SD egg with MN produced a high thermal and mechanical stable product and rendered the highest drying performance, producing a more uniform and defined sphere-shaped morphology in comparison to egg SD either alone and with MD.

Comparative Assessment of the Effect of Hyper-glycosylation on the Pattern and Kinetics of Degradation of Darbepoetin Alfa using a Stability-Indicating Orthogonal Testing Protocol.

PubMed

Moenes, Eman M; Al-Ghobashy, Medhat A; Mohamed, Abeer A; Salem, Maissa Y

2018-01-01

Darbepoetin alfa (DA); hyper-glycosylated Erythropoietin alfa (EPO) is an essential treatment of anemia in patients with chronic kidney failure and cancer. In this study, DA and EPO were subjected to physicochemical stress factors that might be encountered during production, transport and storage (pH, temperature, agitation, repeated freeze-thaw and oxidation). An orthogonal stability-indicating assay protocol comprised of SE-HPLC, RP-HPLC, ELISA and SDS-PAGE was developed and validated to investigate the effect of further glycosylation of DA on the pattern and kinetics of degradation. Results showed a relatively higher stability and lower tendency to form high molecular weight aggregates in the case of DA when compared to EPO, under equivalent stress conditions. Dimers and aggregates were formed for both drugs across the whole pH range and following incubation at temperatures higher than 2-8°C or repeated freeze/thaw. The same observation was noted upon agitation of standard samples prepared in the formulation buffers at high speed and upon oxidation with hydrogen peroxide. The agreement between SE-HPLC, supported with spectral purity data and ELISA confirmed the specificity of both techniques for the intact drugs. Results of RP-HPLC and SDS-PAGE indicated that dimerization occurred through disulfide and bi-tyrosine covalent bonds in the case of pH and oxidation, respectively. It was evident that aggregation was significantly suppressed upon increasing the glycan size and under any of the studied stress factors loss of the glycan has not been observed. These observations supported with the slow kinetics of degradation confirmed the superiority of glyco-engineering over chemical pegylation to enhance the stability of EPO. Formation of such potentially immunogenic product-related impurities at all tested stress factors confirmed the need for orthogonal testing protocols to investigate the complex pattern of degradation of such sensitive products. Copyright © 2017 Elsevier B.V. All rights reserved.

Design, motivation, and on-sky tests of an efficient fiber coupling unit for 1-meter class telescopes

NASA Astrophysics Data System (ADS)

Bottom, Michael; Muirhead, Philip S.; Swift, Jonathan J.; Zhao, Ming; Gardner, Paul; Plavchan, Peter P.; Riddle, Reed L.; Herzig, Erich; Johnson, John A.; Wright, Jason T.; McCrady, Nate; Wittenmyer, Robert A.

2014-08-01

We present the science motivation, design, and on-sky test data of a high-throughput fiber coupling unit suitable for automated 1-meter class telescopes. The optical and mechanical design of the fiber coupling is detailed and we describe a flexible controller software designed specifically for this unit. The system performance is characterized with a set of numerical simulations, and we present on-sky results that validate the performance of the controller and the expected throughput of the fiber coupling. This unit was designed specifically for the MINERVA array, a robotic observatory consisting of multiple 0.7 m telescopes linked to a single high-resolution stabilized spectrograph for the purpose of exoplanet discovery using high-cadence radial velocimetry. However, this unit could easily be used for general astronomical purposes requiring fiber coupling or precise guiding.

Machine-Learning Based Channel Quality and Stability Estimation for Stream-Based Multichannel Wireless Sensor Networks.

PubMed

Rehan, Waqas; Fischer, Stefan; Rehan, Maaz

2016-09-12

Wireless sensor networks (WSNs) have become more and more diversified and are today able to also support high data rate applications, such as multimedia. In this case, per-packet channel handshaking/switching may result in inducing additional overheads, such as energy consumption, delays and, therefore, data loss. One of the solutions is to perform stream-based channel allocation where channel handshaking is performed once before transmitting the whole data stream. Deciding stream-based channel allocation is more critical in case of multichannel WSNs where channels of different quality/stability are available and the wish for high performance requires sensor nodes to switch to the best among the available channels. In this work, we will focus on devising mechanisms that perform channel quality/stability estimation in order to improve the accommodation of stream-based communication in multichannel wireless sensor networks. For performing channel quality assessment, we have formulated a composite metric, which we call channel rank measurement (CRM), that can demarcate channels into good, intermediate and bad quality on the basis of the standard deviation of the received signal strength indicator (RSSI) and the average of the link quality indicator (LQI) of the received packets. CRM is then used to generate a data set for training a supervised machine learning-based algorithm (which we call Normal Equation based Channel quality prediction (NEC) algorithm) in such a way that it may perform instantaneous channel rank estimation of any channel. Subsequently, two robust extensions of the NEC algorithm are proposed (which we call Normal Equation based Weighted Moving Average Channel quality prediction (NEWMAC) algorithm and Normal Equation based Aggregate Maturity Criteria with Beta Tracking based Channel weight prediction (NEAMCBTC) algorithm), that can perform channel quality estimation on the basis of both current and past values of channel rank estimation. In the end, simulations are made using MATLAB, and the results show that the Extended version of NEAMCBTC algorithm (Ext-NEAMCBTC) outperforms the compared techniques in terms of channel quality and stability assessment. It also minimizes channel switching overheads (in terms of switching delays and energy consumption) for accommodating stream-based communication in multichannel WSNs.

Machine-Learning Based Channel Quality and Stability Estimation for Stream-Based Multichannel Wireless Sensor Networks

PubMed Central

Rehan, Waqas; Fischer, Stefan; Rehan, Maaz

2016-01-01

Wireless sensor networks (WSNs) have become more and more diversified and are today able to also support high data rate applications, such as multimedia. In this case, per-packet channel handshaking/switching may result in inducing additional overheads, such as energy consumption, delays and, therefore, data loss. One of the solutions is to perform stream-based channel allocation where channel handshaking is performed once before transmitting the whole data stream. Deciding stream-based channel allocation is more critical in case of multichannel WSNs where channels of different quality/stability are available and the wish for high performance requires sensor nodes to switch to the best among the available channels. In this work, we will focus on devising mechanisms that perform channel quality/stability estimation in order to improve the accommodation of stream-based communication in multichannel wireless sensor networks. For performing channel quality assessment, we have formulated a composite metric, which we call channel rank measurement (CRM), that can demarcate channels into good, intermediate and bad quality on the basis of the standard deviation of the received signal strength indicator (RSSI) and the average of the link quality indicator (LQI) of the received packets. CRM is then used to generate a data set for training a supervised machine learning-based algorithm (which we call Normal Equation based Channel quality prediction (NEC) algorithm) in such a way that it may perform instantaneous channel rank estimation of any channel. Subsequently, two robust extensions of the NEC algorithm are proposed (which we call Normal Equation based Weighted Moving Average Channel quality prediction (NEWMAC) algorithm and Normal Equation based Aggregate Maturity Criteria with Beta Tracking based Channel weight prediction (NEAMCBTC) algorithm), that can perform channel quality estimation on the basis of both current and past values of channel rank estimation. In the end, simulations are made using MATLAB, and the results show that the Extended version of NEAMCBTC algorithm (Ext-NEAMCBTC) outperforms the compared techniques in terms of channel quality and stability assessment. It also minimizes channel switching overheads (in terms of switching delays and energy consumption) for accommodating stream-based communication in multichannel WSNs. PMID:27626429

Solid State Stability of Extemporaneously Prepared Levothyroxine Aliquots and Capsules.

PubMed

Fortner, Jeff; Salton, Jason; Carlson, Christie; Wheeler, Rich; Cote, Brianna; Rao, Deepa

2015-01-01

The purpose of this research was to collect, analyze, and compare stability data for levothyroxine (T4) powder in the anhydrous and pentahydrate form when prepared as an aliquot and in capsules. Two different compounding pharmacies, Central Iowa Compounding and Gateway Medical Pharmacy, used different forms of T4 and aliquot formulations, which were studied to determine the beyond-use date at ±5% or ±10% of labeled strength. T4 was extracted from aliquot and capsule formulations and assessed using reverse-phase high- performance liquid chromatography validated to differentiate between the degraded and original forms of T4. The results indicate that T4 1:100 aliquot formulation prepared with silica gel or Avicel as filler are stable for 120 days at ±10% labeled potency, but at ±5% labeled potency, the silica gel and Avicel aliquot formulations are stable for 45 and 30 days, respectively. The silica gel capsules prepared from fresh aliquot were stable for 120 days at ±10% labeled potency and 90 days at ±5% labeled potency, while the Avicel capsules prepared from fresh aliquot were stable for 180 days at both ±10% and ±5% labeled potency. Avicel capsules prepared from old aliquot (120 days) and fresh aliquot (1 day) were also compared for stability. The old aliquot Avicel capsules were stable for 14 days at ±5% labeled potency and 150 days at ±10% labeled potency, while new aliquot Avicel capsules were stable for 180 days at both ±10% and ±5% labeled potency. Based on our data, there can be significant variation in the beyond-use dates assigned to T4 capsules based on the diluents used for aliquots, the final capsule formulations, and the potency standards applied. These results also indicate that pharmacists must exercise caution when using older aliquots and may have to assign shorter beyond-use dates.

Recent Advances in Heliogyro Solar Sail Structural Dynamics, Stability, and Control Research

NASA Technical Reports Server (NTRS)

Wilkie, W. Keats; Warren, Jerry E.; Horta, Lucas G.; Lyle, Karen H.; Juang, Jer-Nan; Gibbs, S. Chad; Dowell, Earl H.; Guerrant, Daniel V.; Lawrence, Dale

2015-01-01

Results from recent NASA sponsored research on the structural dynamics, stability, and control characteristics of heliogyro solar sails are summarized. Specific areas under investigation include coupled nonlinear finite element analysis of heliogyro membrane blade with solar radiation pressure effects, system identification of spinning membrane structures, and solarelastic stability analysis of heliogyro solar sails, including stability during blade deployment. Recent results from terrestrial 1-g blade dynamics and control experiments on "rope ladder" membrane blade analogs, and small-scale in vacuo system identification experiments with hanging and spinning high-aspect ratio membranes will also be presented. A low-cost, rideshare payload heliogyro technology demonstration mission concept is used as a mission context for these heliogyro structural dynamics and solarelasticity investigations, and is also described. Blade torsional dynamic response and control are also shown to be significantly improved through the use of edge stiffening structural features or inclusion of modest tip masses to increase centrifugal stiffening of the blade structure. An output-only system identification procedure suitable for on-orbit blade dynamics investigations is also developed and validated using ground tests of spinning sub-scale heliogyro blade models. Overall, analytical and experimental investigations to date indicate no intractable stability or control issues for the heliogyro solar sail concept.

Development and psychometric evaluation of a cardiovascular risk and disease management knowledge assessment tool.

PubMed

Rosneck, James S; Hughes, Joel; Gunstad, John; Josephson, Richard; Noe, Donald A; Waechter, Donna

2014-01-01

This article describes the systematic construction and psychometric analysis of a knowledge assessment instrument for phase II cardiac rehabilitation (CR) patients measuring risk modification disease management knowledge and behavioral outcomes derived from national standards relevant to secondary prevention and management of cardiovascular disease. First, using adult curriculum based on disease-specific learning outcomes and competencies, a systematic test item development process was completed by clinical staff. Second, a panel of educational and clinical experts used an iterative process to identify test content domain and arrive at consensus in selecting items meeting criteria. Third, the resulting 31-question instrument, the Cardiac Knowledge Assessment Tool (CKAT), was piloted in CR patients to ensure use of application. Validity and reliability analyses were performed on 3638 adults before test administrations with additional focused analyses on 1999 individuals completing both pretreatment and posttreatment administrations within 6 months. Evidence of CKAT content validity was substantiated, with 85% agreement among content experts. Evidence of construct validity was demonstrated via factor analysis identifying key underlying factors. Estimates of internal consistency, for example, Cronbach's α = .852 and Spearman-Brown split-half reliability = 0.817 on pretesting, support test reliability. Item analysis, using point biserial correlation, measured relationships between performance on single items and total score (P < .01). Analyses using item difficulty and item discrimination indices further verified item stability and validity of the CKAT. A knowledge instrument specifically designed for an adult CR population was systematically developed and tested in a large representative patient population, satisfying psychometric parameters, including validity and reliability.

Developing a tool to measure satisfaction among health professionals in sub-Saharan Africa

PubMed Central

2013-01-01

Background In sub-Saharan Africa, lack of motivation and job dissatisfaction have been cited as causes of poor healthcare quality and outcomes. Measurement of health workers’ satisfaction adapted to sub-Saharan African working conditions and cultures is a challenge. The objective of this study was to develop a valid and reliable instrument to measure satisfaction among health professionals in the sub-Saharan African context. Methods A survey was conducted in Senegal and Mali in 2011 among 962 care providers (doctors, midwives, nurses and technicians) practicing in 46 hospitals (capital, regional and district). The participation rate was very high: 97% (937/962). After exploratory factor analysis (EFA), construct validity was assessed through confirmatory factor analysis (CFA). The discriminant validity of our subscales was evaluated by comparing the average variance extracted (AVE) for each of the constructs with the squared interconstruct correlation (SIC), and finally for criterion validity, each subscale was tested with two hypotheses. Two dimensions of reliability were assessed: internal consistency with Cronbach’s alpha subscales and stability over time using a test-retest process. Results Eight dimensions of satisfaction encompassing 24 items were identified and validated using a process that combined psychometric analyses and expert opinions: continuing education, salary and benefits, management style, tasks, work environment, workload, moral satisfaction and job stability. All eight dimensions demonstrated significant discriminant validity. The final model showed good performance, with a root mean square error of approximation (RMSEA) of 0.0508 (90% CI: 0.0448 to 0.0569) and a comparative fit index (CFI) of 0.9415. The concurrent criterion validity of the eight dimensions was good. Reliability was assessed based on internal consistency, which was good for all dimensions but one (moral satisfaction < 0.70). Test-retest showed satisfactory temporal stability (intra class coefficient range: 0.60 to 0.91). Conclusions Job satisfaction is a complex construct; this study provides a multidimensional instrument whose content, construct and criterion validities were verified to ensure its suitability for the sub-Saharan African context. When using these subscales in further studies, the variability of the reliability of the subscales should be taken in to account for calculating the sample sizes. The instrument will be useful in evaluative studies which will help guide interventions aimed at improving both the quality of care and its effectiveness. PMID:23826720

[Design and study of parallel computing environment of Monte Carlo simulation for particle therapy planning using a public cloud-computing infrastructure].

PubMed

Yokohama, Noriya

2013-07-01

This report was aimed at structuring the design of architectures and studying performance measurement of a parallel computing environment using a Monte Carlo simulation for particle therapy using a high performance computing (HPC) instance within a public cloud-computing infrastructure. Performance measurements showed an approximately 28 times faster speed than seen with single-thread architecture, combined with improved stability. A study of methods of optimizing the system operations also indicated lower cost.

Validation of highly sensitive simultaneous targeted and untargeted analysis of keto-steroids by Girard P derivatization and stable isotope dilution-liquid chromatography-high resolution mass spectrometry.

PubMed

Frey, Alexander J; Wang, Qingqing; Busch, Christine; Feldman, Daniel; Bottalico, Lisa; Mesaros, Clementina A; Blair, Ian A; Vachani, Anil; Snyder, Nathaniel W

2016-12-01

A multiplexed quantitative method for the analysis of three major unconjugated steroids in human serum by stable isotope dilution liquid chromatography-high resolution mass spectrometry (LC-HRMS) was developed and validated on a Q Exactive Plus hybrid quadrupole/Orbitrap mass spectrometer. This quantification utilized isotope dilution and Girard P derivatization on the keto-groups of testosterone (T), androstenedione (AD) and dehydroepiandrosterone (DHEA) to improve ionization efficiency using electrospray ionization. Major isomeric compounds to T and DHEA; the inactive epimer of testosterone (epiT), and the metabolite of AD, 5α-androstanedione (5α-AD) were completely resolved on a biphenyl column within an 18min method. Inter- and intra-day method validation using LC-HRMS with qualifying product ions was performed and acceptable analytical performance was achieved. The method was further validated by comparing steroid levels from 100μL of serum from young vs older subjects. Since this approach provides high-dimensional HRMS data, untargeted analysis by age group was performed. DHEA and T were detected among the top analytes most significantly different across the two groups after untargeted LC-HRMS analysis, as well as a number of other still unknown metabolites, indicating the potential for combined targeted/untargeted analysis in steroid analysis. Copyright © 2016 Elsevier Inc. All rights reserved.

Chemical profiling and quantification of Dan-Deng-Tong-Nao-capsule using ultra high performance liquid chromatography coupled with high resolution hybrid quadruple-orbitrap mass spectrometry.

PubMed

Lv, Xiao-Jing; Sun, Zhi; Wang, Pei-Le; Yang, Jing; Xu, Tan-Ye; Jia, Qing-Quan; Li, Da-Wei; Su, Fang-Yi; Zhu, Zhen-Feng; Kang, Jian; Zhang, Xiao-Jian

2018-01-30

Dan-Deng-Tong-Nao capsule (DDTN) was a traditional Chinese medicine (TCM) formula, and has been widely used for the treatment of stroke clinically which caused by blood stasis. However, the bioactive substances and mechanism are unclear because of the complex compositions in DDTN. In this research, An ultra high-performance liquid chromatography (UHPLC) coupled with hybrid quadruple-orbitrap mass spectrometry (Q-Orbitrap MS) method was utilized to identify the chemical constituents of DDTN. In total, 102 compounds including diterpenes, lactones, flavonoids, and phenolic acids were identified by the accurate masses and fragmentation pathways, and 18 of them were unambiguously determined by comparison of reference standards. Besides, 12 representative compounds were simultaneously quantification analyzed and successfully applified for detecting in 9 batches of DDTN samples by UHPLC-Q-Orbitrap MS in parallel reaction monitoring (PRM) mode. The proposed approach was validated to be satisfied in terms of linearity (0.9954-0.9999), LOD (0.771ng/mL), LOQ (2.568ng/mL), intra-day precision ( <2.68%), inter-day precision ( <4.52%), repeatability ( <2.96%), stability ( <3.21%), and recovery (94.6-105.5%). The results indicate that the method of combining UHPLC with Q-Orbitrap MS is practical and efficient for the chemical clarification in DDTN, and has great potential for the integrating quality control of other traditional Chinese medicines. Copyright © 2017 Elsevier B.V. All rights reserved.

Liquid chromatography/tandem mass spectrometry method for simultaneous determination of cocaine and its metabolite (-)ecgonine methyl ester in human acidified stabilized plasma samples.

PubMed

Liu, Yongzhen; Zheng, Bo; Strafford, Stephanie; Orugunty, Ravi; Sullivan, Michael; Gus, Jeffrey; Heidbreder, Christian; Fudala, Paul J; Nasser, Azmi

2014-06-15

Two simple, sensitive and rapid liquid chromatography/electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) methods (low range and high range) were developed and validated for the quantification of cocaine and its metabolite (-)ecgonine methyl ester (EME) in human acidified stabilized plasma samples. In the low range assay, cocaine and the internal standard, cocaine-D3, were extracted using a single step liquid-liquid extraction from human acidified stabilized plasma. For the high range assay, human acidified stabilized plasma containing cocaine, EME, and the internal standards, cocaine-D3 and EME-D3, was mixed with acetonitrile, and the protein precipitate was separated by centrifugation. Both cocaine and EME extracted from both assays were separated on a HILIC column and detected in positive ion mode using multiple reaction monitoring (MRM). Both methods were validated and the specificity, linearity, lower limit of quantitation (LLOQ), precision, accuracy, recoveries and stability were determined. The linear range for the low range assay was 0.01-5ng/mL for cocaine; in the high range assay values were 5-1000ng/mL for cocaine and 1-200ng/mL for EME. The correlation coefficient (R(2)) values for both assays were 0.993 or greater. The precision and accuracy for intra-day and inter-day were better than 13.0%. The recovery was above 85% and matrix effects were low with the matrix factor ranging from 0.817 to 1.10 for both analytes in both assays. The validated methods were successfully used to quantify the plasma concentrations of cocaine and EME in clinical pharmacokinetic and pharmacodynamic studies. Copyright © 2014 Elsevier B.V. All rights reserved.

Stability-Indicating Liquid Chromatographic Methods with Photodiode Array Detection and Light Scattering Detection for Simultaneous Determination of Candesartan and Hydrochlorothiazide.

PubMed

de Diego, Marta; Godoy, Ricardo; Mennickent, Sigrid; Vergara, Carola; Miranda, Daniel; Navarro, Pía

2018-02-01

Development, validation and comparison of two stability-indicating LC methods, one with photodiode array detector (DAD) and the other with evaporative light scattering detector (ELSD), were performed for simultaneous determination of candesartan cilexetil (CANC) and hydrochlorothiazide (HCTZ), in pharmaceutical samples. A RP-18 column (125 mm × 4 mm, 5 μm) was used for separation of CANC, HCTZ and its major degradation products, using acetonitrile and phosphate buffer (pH 6.0) for DAD method and acetonitrile and water with acetic acid and triethylamine (pH 4.1) for ELSD method, as mobile phase in a gradient mode. The response with ELSD was fitted to a power function and the DAD response by a linear model over a range of 32-160 μg/mL for CANC and 25-125 μg/mL for HCTZ. The precision and accuracy of the methods were similar, with RSD below 3.0% and recovery between 98.1% and 103.9%. The drugs were subjected to stress conditions of hydrolysis, oxidation, photolysis, humidity and temperature. The degradation products were satisfactory separated from the main peaks and from each other. Both drugs mainly degrade by hydrolysis, showing the formation of one degradation product for HCTZ and two for CANC; its identification was conducted by LC/MS/MS. The methods were successfully applied to the analysis of CANC and HCTZ in combined commercial tablets. The performance of DAD and ELSD methods are comparable, therefore both methods are suitable for stability study and determination of CANC and HCTZ in pharmaceutical samples. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A composite stability index for dichotomous forecast of thunderstorms

NASA Astrophysics Data System (ADS)

Chaudhuri, Sutapa; Middey, Anirban

2012-12-01

Thunderstorms are the perennial feature of Kolkata (22° 32' N, 88° 20' E), India during the premonsoon season (April-May). Precise forecast of these thunderstorms is essential to mitigate the associated catastrophe due to lightning flashes, strong wind gusts, torrential rain, and occasional hail and tornadoes. The present research provides a composite stability index for forecasting thunderstorms. The forecast quality detection parameters are computed with the available indices during the period from 1997 to 2006 to select the most relevant indices with threshold ranges for the prevalence of such thunderstorms. The analyses reveal that the lifted index (LI) within the range of -5 to -12 °C, convective inhibition energy (CIN) within the range of 0-150 J/kg and convective available potential energy (CAPE) within the ranges of 2,000 to 7,000 J/kg are the most pertinent indices for the prevalence thunderstorms over Kolkata during the premonsoon season. A composite stability index, thunderstorm prediction index (TPI) is formulated with LI, CIN, and CAPE. The statistical skill score analyses show that the accuracy in forecasting such thunderstorms with TPI is 99.67 % with lead time less than 12 h during training the index whereas the accuracies are 89.64 % with LI, 60 % with CIN and 49.8 % with CAPE. The performance diagram supports that TPI has better forecast skill than its individual components. The forecast with TPI is validated with the observation of the India Meteorological Department during the period from 2007 to 2009. The real-time forecast of thunderstorms with TPI is provided for the year 2010.

A New Rapid and Sensitive Stability-Indicating UPLC Assay Method for Tolterodine Tartrate: Application in Pharmaceuticals, Human Plasma and Urine Samples.

PubMed

Yanamandra, Ramesh; Vadla, Chandra Sekhar; Puppala, Umamaheshwar; Patro, Balaram; Murthy, Yellajyosula L N; Ramaiah, Parimi Atchuta

2012-01-01

A new rapid, simple, sensitive, selective and accurate reversed-phase stability-indicating Ultra Performance Liquid Chromatography (RP-UPLC) technique was developed for the assay of Tolterodine Tartrate in pharmaceutical dosage form, human plasma and urine samples. The developed UPLC method is superior in technology to conventional HPLC with respect to speed, solvent consumption, resolution and cost of analysis. Chromatographic run time was 6 min in reversed-phase mode and ultraviolet detection was carried out at 220 nm for quantification. Efficient separation was achieved for all the degradants of Tolterodine Tartrate on BEH C18 sub-2-μm Acquity UPLC column using Trifluoroacetic acid and acetonitrile as organic solvent in a linear gradient program. The active pharmaceutical ingredient was extracted from tablet dosage form using a mixture of acetonitrile and water as diluent. The calibration graphs were linear and the method showed excellent recoveries for bulk and tablet dosage form. The test solution was found to be stable for 40 days when stored in the refrigerator between 2 and 8 °C. The developed UPLC method was validated and meets the requirements delineated by the International Conference on Harmonization (ICH) guidelines with respect to linearity, accuracy, precision, specificity and robustness. The intra-day and inter-day variation was found be less than 1%. The method was reproducible and selective for the estimation of Tolterodine Tartrate. Because the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating one.

A New Rapid and Sensitive Stability-Indicating UPLC Assay Method for Tolterodine Tartrate: Application in Pharmaceuticals, Human Plasma and Urine Samples

PubMed Central

Yanamandra, Ramesh; Vadla, Chandra Sekhar; Puppala, Umamaheshwar; Patro, Balaram; Murthy, Yellajyosula. L. N.; Ramaiah, Parimi Atchuta

2012-01-01

A new rapid, simple, sensitive, selective and accurate reversed-phase stability-indicating Ultra Performance Liquid Chromatography (RP-UPLC) technique was developed for the assay of Tolterodine Tartrate in pharmaceutical dosage form, human plasma and urine samples. The developed UPLC method is superior in technology to conventional HPLC with respect to speed, solvent consumption, resolution and cost of analysis. Chromatographic run time was 6 min in reversed-phase mode and ultraviolet detection was carried out at 220 nm for quantification. Efficient separation was achieved for all the degradants of Tolterodine Tartrate on BEH C18 sub-2-μm Acquity UPLC column using Trifluoroacetic acid and acetonitrile as organic solvent in a linear gradient program. The active pharmaceutical ingredient was extracted from tablet dosage form using a mixture of acetonitrile and water as diluent. The calibration graphs were linear and the method showed excellent recoveries for bulk and tablet dosage form. The test solution was found to be stable for 40 days when stored in the refrigerator between 2 and 8 °C. The developed UPLC method was validated and meets the requirements delineated by the International Conference on Harmonization (ICH) guidelines with respect to linearity, accuracy, precision, specificity and robustness. The intra-day and inter-day variation was found be less than 1%. The method was reproducible and selective for the estimation of Tolterodine Tartrate. Because the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating one. PMID:22396907

Lightweight ZERODUR: Validation of Mirror Performance and Mirror Modeling Predictions

NASA Technical Reports Server (NTRS)

Hull, Tony; Stahl, H. Philip; Westerhoff, Thomas; Valente, Martin; Brooks, Thomas; Eng, Ron

2017-01-01

Upcoming spaceborne missions, both moderate and large in scale, require extreme dimensional stability while relying both upon established lightweight mirror materials, and also upon accurate modeling methods to predict performance under varying boundary conditions. We describe tests, recently performed at NASA's XRCF chambers and laboratories in Huntsville Alabama, during which a 1.2 m diameter, f/1.2988% lightweighted SCHOTT lightweighted ZERODUR(TradeMark) mirror was tested for thermal stability under static loads in steps down to 230K. Test results are compared to model predictions, based upon recently published data on ZERODUR(TradeMark). In addition to monitoring the mirror surface for thermal perturbations in XRCF Thermal Vacuum tests, static load gravity deformations have been measured and compared to model predictions. Also the Modal Response(dynamic disturbance) was measured and compared to model. We will discuss the fabrication approach and optomechanical design of the ZERODUR(TradeMark) mirror substrate by SCHOTT, its optical preparation for test by Arizona Optical Systems (AOS). Summarize the outcome of NASA's XRCF tests and model validations

Lightweight ZERODUR®: Validation of mirror performance and mirror modeling predictions

NASA Astrophysics Data System (ADS)

Hull, Anthony B.; Stahl, H. Philip; Westerhoff, Thomas; Valente, Martin; Brooks, Thomas; Eng, Ron

2017-01-01

Upcoming spaceborne missions, both moderate and large in scale, require extreme dimensional stability while relying both upon established lightweight mirror materials, and also upon accurate modeling methods to predict performance under varying boundary conditions. We describe tests, recently performed at NASA’s XRCF chambers and laboratories in Huntsville Alabama, during which a 1.2m diameter, f/1.29 88% lightweighted SCHOTT lightweighted ZERODUR® mirror was tested for thermal stability under static loads in steps down to 230K. Test results are compared to model predictions, based upon recently published data on ZERODUR®. In addition to monitoring the mirror surface for thermal perturbations in XRCF Thermal Vacuum tests, static load gravity deformations have been measured and compared to model predictions. Also the Modal Response (dynamic disturbance) was measured and compared to model. We will discuss the fabrication approach and optomechanical design of the ZERODUR® mirror substrate by SCHOTT, its optical preparation for test by Arizona Optical Systems (AOS), and summarize the outcome of NASA’s XRCF tests and model validations.

The design of the Comet streamliner: An electric land speed record motorcycle

NASA Astrophysics Data System (ADS)

McMillan, Ethan Alexander

The development of the land speed record electric motorcycle streamliner, the Comet, is discussed herein. Its design process includes a detailed literary review of past and current motorcycle streamliners in an effort to highlight the main components of such a vehicle's design, while providing baseline data for performance comparisons. A new approach to balancing a streamliner at low speeds is also addressed, a system henceforth referred to as landing gear, which has proven an effective means for allowing the driver to control the low speed instabilities of the vehicle with relative ease compared to tradition designs. This is accompanied by a dynamic stability analysis conducted on a test chassis that was developed for the primary purpose of understanding the handling dynamics of streamliners, while also providing a test bed for the implementation of the landing gear system and a means to familiarize the driver to the operation and handling of such a vehicle. Data gathered through the use of GPS based velocity tracking, accelerometers, and a linear potentiometer provided a means to validate a dynamic stability analysis of the weave and wobble modes of the vehicle through linearization of a streamliner model developed in the BikeSIM software suite. Results indicate agreement between the experimental data and the simulation, indicating that the conventional recumbent design of a streamliner chassis is in fact highly stable throughout the performance envelope beyond extremely low speeds. A computational fluid dynamics study was also performed, utilized in the development of the body of the Comet to which a series of tests were conducted in order to develop a shape that was both practical to transport and highly efficient. By creating a hybrid airfoil from a NACA 0018 and NACA 66-018, a drag coefficient of 0.1 and frontal area of 0.44 m2 has been found for the final design. Utilizing a performance model based on the proposed vehicle's motor, its rolling resistance, and the body's aerodynamic drag, the top speed is predicted at 226 mph. Further design considerations are also addressed, including the development of the component level layout of the motorcycle, weighing factors such as safety and ease of fabrication with that of performance and accessibility. At the time of composition, the Comet had started the fabrication process, and it is the intent of the author that the finished product competes in the 2016 Bonneville Motorcycle Speed Trials to set the first world record for a single track electric motorcycle streamliner.

Assessment of performance validity in the Stroop Color and Word Test in mild traumatic brain injury patients: a criterion-groups validation design.

PubMed

Guise, Brian J; Thompson, Matthew D; Greve, Kevin W; Bianchini, Kevin J; West, Laura

2014-03-01

The current study assessed performance validity on the Stroop Color and Word Test (Stroop) in mild traumatic brain injury (TBI) using criterion-groups validation. The sample consisted of 77 patients with a reported history of mild TBI. Data from 42 moderate-severe TBI and 75 non-head-injured patients with other clinical diagnoses were also examined. TBI patients were categorized on the basis of Slick, Sherman, and Iverson (1999) criteria for malingered neurocognitive dysfunction (MND). Classification accuracy is reported for three indicators (Word, Color, and Color-Word residual raw scores) from the Stroop across a range of injury severities. With false-positive rates set at approximately 5%, sensitivity was as high as 29%. The clinical implications of these findings are discussed. © 2012 The British Psychological Society.

Fuzzy Logic Controller Stability Analysis Using a Satisfiability Modulo Theories Approach

NASA Technical Reports Server (NTRS)

Arnett, Timothy; Cook, Brandon; Clark, Matthew A.; Rattan, Kuldip

2017-01-01

While many widely accepted methods and techniques exist for validation and verification of traditional controllers, at this time no solutions have been accepted for Fuzzy Logic Controllers (FLCs). Due to the highly nonlinear nature of such systems, and the fact that developing a valid FLC does not require a mathematical model of the system, it is quite difficult to use conventional techniques to prove controller stability. Since safety-critical systems must be tested and verified to work as expected for all possible circumstances, the fact that FLC controllers cannot be tested to achieve such requirements poses limitations on the applications for such technology. Therefore, alternative methods for verification and validation of FLCs needs to be explored. In this study, a novel approach using formal verification methods to ensure the stability of a FLC is proposed. Main research challenges include specification of requirements for a complex system, conversion of a traditional FLC to a piecewise polynomial representation, and using a formal verification tool in a nonlinear solution space. Using the proposed architecture, the Fuzzy Logic Controller was found to always generate negative feedback, but inconclusive for Lyapunov stability.

Rapid and reliable quantitation of amino acids and myo-inositol in mouse brain by high performance liquid chromatography and tandem mass spectrometry.

PubMed

Bathena, Sai P; Huang, Jiangeng; Epstein, Adrian A; Gendelman, Howard E; Boska, Michael D; Alnouti, Yazen

2012-04-15

Amino acids and myo-inositol have long been proposed as putative biomarkers for neurodegenerative diseases. Accurate measures and stability have precluded their selective use. To this end, a sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method based on multiple reaction monitoring was developed to simultaneously quantify glutamine, glutamate, γ-aminobutyric acid (GABA), aspartic acid, N-acetyl aspartic acid, taurine, choline, creatine, phosphocholine and myo-inositol in mouse brain by methanol extractions. Chromatography was performed using a hydrophilic interaction chromatography silica column within in a total run time of 15 min. The validated method is selective, sensitive, accurate, and precise. The method has a limit of quantification ranging from 2.5 to 20 ng/ml for a range of analytes and a dynamic range from 2.5-20 to 500-4000 ng/ml. This LC-MS/MS method was validated for biomarker discovery in models of human neurological disorders. Copyright © 2012 Elsevier B.V. All rights reserved.

A study of the problem of designing airplanes with satisfactory inherent damping of the dutch roll oscillation

NASA Technical Reports Server (NTRS)

Campbell, John P; Mckinney, Marion O , Jr

1954-01-01

Considerable interest has recently been shown in means of obtaining satisfactory stability of the dutch roll oscillation for modern high-performance airplanes without resort to complicated artificial stabilizing devices. One approach to this problem is to lay out the airplane in the earliest stages of design so that it will have the greatest practicable inherent stability of the lateral oscillation. The present report presents some preliminary results of a theoretical analysis to determine the design features that appear most promising in providing adequate inherent stability. These preliminary results cover the case of fighter airplanes at subsonic speeds. The investigation indicated that it is possible to design fighter airplanes to have substantially better inherent stability than most current designs. Since the use of low-aspect-ratio swept-back wings is largely responsible for poor dutch roll stability, it is important to design the airplane with the maximum aspect ratio and minimum sweep that will permit attainment of the desired performance. The radius of gyration in roll should be kept as low as possible and the nose-up inclination of the principal longitudinal axis of inertia should be made as great as practicable. (author)

Robust interval-based regulation for anaerobic digestion processes.

PubMed

Alcaraz-González, V; Harmand, J; Rapaport, A; Steyer, J P; González-Alvarez, V; Pelayo-Ortiz, C

2005-01-01

A robust regulation law is applied to the stabilization of a class of biochemical reactors exhibiting partially known highly nonlinear dynamic behavior. An uncertain environment with the presence of unknown inputs is considered. Based on some structural and operational conditions, this regulation law is shown to exponentially stabilize the aforementioned bioreactors around a desired set-point. This approach is experimentally applied and validated on a pilot-scale (1 m3) anaerobic digestion process for the treatment of raw industrial wine distillery wastewater where the objective is the regulation of the chemical oxygen demand (COD) by using the dilution rate as the manipulated variable. Despite large disturbances on the input COD and state and parametric uncertainties, this regulation law gave excellent performances leading the output COD towards its set-point and keeping it inside a pre-specified interval.

Integrated electromagnetic methods for archaeological prospection and stability assessment of anthropogenic mounds: insights into the English Cemetery in Florence

NASA Astrophysics Data System (ADS)

Cappuccini, Luca; Pazzi, Veronica; Tapete, Deodato

2013-04-01

The archaeological interest in anthropogenic mounds as historical products of human occupation generally concerns the understanding of their stratigraphic sequence and the discovery of buried structures. Nevertheless, a further key element relies on the assessment of their stability. This is particularly crucial when the conservation history induced relevant alteration of the former configuration, and a potential collapse might cause damages to heritage and actual risk for public safety. To respond to such dual diagnostic need, we propose an integration approach based on Very Low Frequency Electromagnetic (VLF-EM) qualitative method and 2D-Electrical Resistivity Tomography (2D-ERT), to make the best out of these two techniques in light of their frequencies/bandwidth and methods of soil investigation (15-30 kHz and DC, respectively). We present here the results from the experiments performed on one of the test sites selected to validate the proposed methodology, i.e. the Protestant Cemetery (the so-called "English Cemetery") in Florence, Italy, which is a demonstrative example of a huge sample of anthropogenic mounds within urban and rural environments. Located on a topographic relief, the cemetery testifies a long history since Roman times, as proved by historical documentation and the ceramic findings still now discovered on the (sub-)surface. Converted into a cemetery in 1827, the mound appeared as an anomalous outcrop adjacent to the town walls, prior to the final arrangement and reshaping due to the urban renewal of Florence in 1877, which definitely transformed it into a raised graveyard surrounded by boulevards. A campaign of VLF-EM and ERT measurements was performed to ascertain the presence of a buried part of the ancient eastern wall and identify the key areas of concern for the stability. High values of resistivity were clearly detected and mapped by means of 2D-ERT along the AA' array intercepting the hypothesized location of the buried wall. This measure was cross-validated with the corresponding VLF-EM anomaly profiles, thereby retrieving reliable geophysical evidences suggesting the presence of buried remains. To correlate the effects of inner structures and soil properties with the stability condition of the mound, crack pattern survey was carried out over the wall containing the mound, jointly to an inspection of the cavities and the interspaces between the exterior masonry surfaces and the rear terrain. The spatial distribution of the opened cracks allowed the actual threat for the stability of the mound to be assessed also in relation to the current positions of the cypresses, periodically replanted for landscape reasons. Interesting insights were obtained by mapping the inclination and tilt direction of the gravestones and funerary monuments, as superficial indicators of ground subsidence and soil compaction/collapse at the top of the mound. The benefits achieved for site management and tombstones maintenance have encouraged the exportation of this approach (highly adaptable to include also GPR and seismic methods) to other case studies, and open to a sustainable implementation for the investigation of funerary mounds, such as the Etruscan burial mounds.

Analysis of a Precambrian Resonance-Stabilized Day Length

NASA Astrophysics Data System (ADS)

Bartlett, B. C.; Stevenson, D. J.

2014-12-01

Calculations indicate the average rate of decrease of Earth's angular momentum must have been less than its present value in the past; otherwise, the Earth should have a longer day length. Existing stromatolite data suggests the Earth's rotational frequency would have been near that of the atmospheric resonance frequency toward the end of the Precambrian era, approximately 600Ma. The semidiurnal atmospheric tidal torque would have reached a maximum near this day length of 21hr. At this point, the atmospheric torque would have been comparable in magnitude but opposite in direction to the lunar torque, creating a stabilizing effect which could preserve a constant day length while trapped in this resonant state, as suggested by Zahnle and Walker (1987). We examine the hypothesis that this resonant stability was encountered and sustained for a large amount of time during the Precambrian era and was broken by a large and relatively fast increase in global temperature, possibly in the deglaciation period following a snowball event. Computational simulations of this problem were performed, indicating that a persistent increase in temperature larger than around 10K over a period of time less than 107 years will break resonance (though these values vary with Q), but that the resonant stability is not easily broken by random high-amplitude high-frequency atmospheric temperature fluctuation or other forms of thermal noise. Further work also indicates it is possible to escape resonance simply by increasing the lunar tidal torque on the much longer timescale of plate tectonics, particularly for low atmospheric Q-factors, or that resonance could have never formed in the first place, had the lunar torque been very high or Q been very low when the Earth's rotational frequency was near the atmospheric resonance frequency. However, the need to explain the present day length given the current lunar torque favors the interpretation we offer, in which Earth's length of day was stabilized for hundreds of millions of years, escaping this stability in the aftermath of a sudden global temperature change.

Determination of molindone enantiomers in human plasma by high-performance liquid chromatography-tandem mass spectrometry using macrocyclic antibiotic chiral stationary phases.

PubMed

Jiang, Hongliang; Li, Yinghe; Pelzer, Mary; Cannon, Michelle J; Randlett, Christopher; Junga, Heiko; Jiang, Xiangyu; Ji, Qin C

2008-05-30

A sensitive and selective bioanalytical assay was developed and validated for the determination of enantiomeric molindone in human plasma using high-performance liquid chromatography-tandem mass spectrometry along with supported liquid extraction procedures. The chiral separation was evaluated and optimized on macrocyclic antibiotic type chiral stationary phases (CSPs) based on teicoplanin aglycone (Chirobiotic TAG) in polar organic, polar ionic, and reversed-phase mode chromatography, respectively. Complete baseline separation was achieved on a Chirobiotic TAG column under isocratic condition in reversed-phase chromatography. The method validation was conducted using a Chirobiotic TAG column (100 mm x 2.1 mm) over the curve range 0.100-100 ng/ml for each molindone enantiomer using 0.0500 ml of plasma sample. The flow rate was 0.8 ml/min and the total run time was 9 min. Supported liquid extraction in a 96-well plate format was used for sample preparation. Parameters including recovery, matrix effect, linearity, sensitivity, specificity, carryover, precision, accuracy, dilution integrity, and stability were evaluated. The intra- and inter-day precision and accuracy of the quality control samples at low, medium, and high concentration levels were RSD

One-year temporal stability and predictive and incremental validity of the body, eating, and exercise comparison orientation measure (BEECOM) among college women.

PubMed

Fitzsimmons-Craft, Ellen E; Bardone-Cone, Anna M

2014-01-01

This study examined the one-year temporal stability and the predictive and incremental validity of the Body, Eating, and Exercise Comparison Measure (BEECOM) in a sample of 237 college women who completed study measures at two time points about one year apart. One-year temporal stability was high for the BEECOM total and subscale (i.e., Body, Eating, and Exercise Comparison Orientation) scores. Additionally, the BEECOM exhibited predictive validity in that it accounted for variance in body dissatisfaction and eating disorder symptomatology one year later. These findings held even after controlling for body mass index and existing measures of social comparison orientation. However, results regarding the incremental validity of the BEECOM, or its ability to predict change in these constructs over time, were more mixed. Overall, this study demonstrated additional psychometric properties of the BEECOM among college women, further establishing the usefulness of this measure for more comprehensively assessing eating disorder-related social comparison. Copyright © 2013 Elsevier Ltd. All rights reserved.

Simultaneous quantification of acetaminophen and five acetaminophen metabolites in human plasma and urine by high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry: Method validation and application to a neonatal pharmacokinetic study.

PubMed

Cook, Sarah F; King, Amber D; van den Anker, John N; Wilkins, Diana G

2015-12-15

Drug metabolism plays a key role in acetaminophen (paracetamol)-induced hepatotoxicity, and quantification of acetaminophen metabolites provides critical information about factors influencing susceptibility to acetaminophen-induced hepatotoxicity in clinical and experimental settings. The aims of this study were to develop, validate, and apply high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) methods for simultaneous quantification of acetaminophen, acetaminophen-glucuronide, acetaminophen-sulfate, acetaminophen-glutathione, acetaminophen-cysteine, and acetaminophen-N-acetylcysteine in small volumes of human plasma and urine. In the reported procedures, acetaminophen-d4 and acetaminophen-d3-sulfate were utilized as internal standards (IS). Analytes and IS were recovered from human plasma (10μL) by protein precipitation with acetonitrile. Human urine (10μL) was prepared by fortification with IS followed only by sample dilution. Calibration concentration ranges were tailored to literature values for each analyte in each biological matrix. Prepared samples from plasma and urine were analyzed under the same HPLC-ESI-MS/MS conditions, and chromatographic separation was achieved through use of an Agilent Poroshell 120 EC-C18 column with a 20-min run time per injected sample. The analytes could be accurately and precisely quantified over 2.0-3.5 orders of magnitude. Across both matrices, mean intra- and inter-assay accuracies ranged from 85% to 112%, and intra- and inter-assay imprecision did not exceed 15%. Validation experiments included tests for specificity, recovery and ionization efficiency, inter-individual variability in matrix effects, stock solution stability, and sample stability under a variety of storage and handling conditions (room temperature, freezer, freeze-thaw, and post-preparative). The utility and suitability of the reported procedures were illustrated by analysis of pharmacokinetic samples collected from neonates receiving intravenous acetaminophen. Copyright © 2015 Elsevier B.V. All rights reserved.

Utilize Cementitious High Carbon Fly Ash (CHCFA) to Stabilize Cold In-Place Recycled (CIR) Asphalt Pavement as Base Coarse

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wen, Haifang; Li, Xiaojun; Edil, Tuncer

The purpose of this study was to evaluate the performance of cementitious high carbon fly ash (CHCFA) stabilized recycled asphalt pavement as a base course material in a real world setting. Three test road cells were built at MnROAD facility in Minnesota. These cells have the same asphalt surface layers, subbases, and subgrades, but three different base courses: conventional crushed aggregates, untreated recycled pavement materials (RPM), and CHCFA stabilized RPM materials. During and after the construction of the three cells, laboratory and field tests were carried out to characterize the material properties. The test results were used in the mechanistic-empiricalmore » pavement design guide (MEPDG) to predict the pavement performance. Based on the performance prediction, the life cycle analyses of cost, energy consumption, and greenhouse gasses were performed. The leaching impacts of these three types of base materials were compared. The laboratory and field tests showed that fly ash stabilized RPM had higher modulus than crushed aggregate and RPM did. Based on the MEPDG performance prediction, the service life of the Cell 79 containing fly ash stabilized RPM, is 23.5 years, which is about twice the service life (11 years) of the Cell 77 with RPM base, and about three times the service life (7.5 years) of the Cell 78 with crushed aggregate base. The life cycle analysis indicated that the usage of the fly ash stabilized RPM as the base of the flexible pavement can significantly reduce the life cycle cost, the energy consumption, the greenhouse gases emission. Concentrations of many trace elements, particularly those with relatively low water quality standards, diminish over time as water flows through the pavement profile. For many elements, concentrations below US water drinking water quality standards are attained at the bottom of the pavement profile within 2-4 pore volumes of flow.« less

Advanced stability indicating chemometric methods for quantitation of amlodipine and atorvastatin in their quinary mixture with acidic degradation products.

PubMed

Darwish, Hany W; Hassan, Said A; Salem, Maissa Y; El-Zeany, Badr A

2016-02-05

Two advanced, accurate and precise chemometric methods are developed for the simultaneous determination of amlodipine besylate (AML) and atorvastatin calcium (ATV) in the presence of their acidic degradation products in tablet dosage forms. The first method was Partial Least Squares (PLS-1) and the second was Artificial Neural Networks (ANN). PLS was compared to ANN models with and without variable selection procedure (genetic algorithm (GA)). For proper analysis, a 5-factor 5-level experimental design was established resulting in 25 mixtures containing different ratios of the interfering species. Fifteen mixtures were used as calibration set and the other ten mixtures were used as validation set to validate the prediction ability of the suggested models. The proposed methods were successfully applied to the analysis of pharmaceutical tablets containing AML and ATV. The methods indicated the ability of the mentioned models to solve the highly overlapped spectra of the quinary mixture, yet using inexpensive and easy to handle instruments like the UV-VIS spectrophotometer. Copyright © 2015 Elsevier B.V. All rights reserved.

Digitized Spiral Drawing: A Possible Biomarker for Early Parkinson's Disease.

PubMed

San Luciano, Marta; Wang, Cuiling; Ortega, Roberto A; Yu, Qiping; Boschung, Sarah; Soto-Valencia, Jeannie; Bressman, Susan B; Lipton, Richard B; Pullman, Seth; Saunders-Pullman, Rachel

2016-01-01

Pre-clinical markers of Parkinson's Disease (PD) are needed, and to be relevant in pre-clinical disease, they should be quantifiably abnormal in early disease as well. Handwriting is impaired early in PD and can be evaluated using computerized analysis of drawn spirals, capturing kinematic, dynamic, and spatial abnormalities and calculating indices that quantify motor performance and disability. Digitized spiral drawing correlates with motor scores and may be more sensitive in detecting early changes than subjective ratings. However, whether changes in spiral drawing are abnormal compared with controls and whether changes are detected in early PD are unknown. 138 PD subjects (50 with early PD) and 150 controls drew spirals on a digitizing tablet, generating x, y, z (pressure) data-coordinates and time. Derived indices corresponded to overall spiral execution (severity), shape and kinematic irregularity (second order smoothness, first order zero-crossing), tightness, mean speed and variability of spiral width. Linear mixed effect adjusted models comparing these indices and cross-validation were performed. Receiver operating characteristic analysis was applied to examine discriminative validity of combined indices. All indices were significantly different between PD cases and controls, except for zero-crossing. A model using all indices had high discriminative validity (sensitivity = 0.86, specificity = 0.81). Discriminative validity was maintained in patients with early PD. Spiral analysis accurately discriminates subjects with PD and early PD from controls supporting a role as a promising quantitative biomarker. Further assessment is needed to determine whether spiral changes are PD specific compared with other disorders and if present in pre-clinical PD.

Digitized Spiral Drawing: A Possible Biomarker for Early Parkinson’s Disease

PubMed Central

San Luciano, Marta; Wang, Cuiling; Ortega, Roberto A.; Yu, Qiping; Boschung, Sarah; Soto-Valencia, Jeannie; Bressman, Susan B.; Lipton, Richard B.; Pullman, Seth; Saunders-Pullman, Rachel

2016-01-01

Introduction Pre-clinical markers of Parkinson’s Disease (PD) are needed, and to be relevant in pre-clinical disease, they should be quantifiably abnormal in early disease as well. Handwriting is impaired early in PD and can be evaluated using computerized analysis of drawn spirals, capturing kinematic, dynamic, and spatial abnormalities and calculating indices that quantify motor performance and disability. Digitized spiral drawing correlates with motor scores and may be more sensitive in detecting early changes than subjective ratings. However, whether changes in spiral drawing are abnormal compared with controls and whether changes are detected in early PD are unknown. Methods 138 PD subjects (50 with early PD) and 150 controls drew spirals on a digitizing tablet, generating x, y, z (pressure) data-coordinates and time. Derived indices corresponded to overall spiral execution (severity), shape and kinematic irregularity (second order smoothness, first order zero-crossing), tightness, mean speed and variability of spiral width. Linear mixed effect adjusted models comparing these indices and cross-validation were performed. Receiver operating characteristic analysis was applied to examine discriminative validity of combined indices. Results All indices were significantly different between PD cases and controls, except for zero-crossing. A model using all indices had high discriminative validity (sensitivity = 0.86, specificity = 0.81). Discriminative validity was maintained in patients with early PD. Conclusion Spiral analysis accurately discriminates subjects with PD and early PD from controls supporting a role as a promising quantitative biomarker. Further assessment is needed to determine whether spiral changes are PD specific compared with other disorders and if present in pre-clinical PD. PMID:27732597

High-voltage leak detection of a parenteral proteinaceous solution product packaged in form-fill-seal plastic laminate bags. Part 1. Method development and validation.

PubMed

Damgaard, Rasmus; Rasmussen, Mats; Buus, Peter; Mulhall, Brian; Guazzo, Dana Morton

2013-01-01

In Part 1 of this three-part research series, a leak test performed using high-voltage leak detection (HVLD) technology, also referred to as an electrical conductivity and capacitance leak test, was developed and validated for container-closure integrity verification of a small-volume laminate plastic bag containing an aqueous solution for injection. The sterile parenteral product is the rapid-acting insulin analogue, insulin aspart (NovoRapid®/NovoLog®, by Novo Nordisk A/S, Bagsværd, Denmark). The aseptically filled and sealed package is designed to preserve product sterility through expiry. Method development and validation work incorporated positive control packages with a single hole laser-drilled through the laminate film of each bag. A unique HVLD method characterized by specific high-voltage and potentiometer set points was established for testing bags positioned in each of three possible orientations as they are conveyed through the instrument's test zone in each of two possible directions-resulting in a total of six different test method options. Validation study results successfully demonstrated the ability of all six methods to accurately and reliably detect those packages with laser-drilled holes from 2.5-11.2 μm in nominal diameter. Part 2 of this series will further explore HVLD test results as a function of package seal and product storage variables. The final Part 3 will report the impact of HVLD exposure on product physico-chemical stability. In this Part 1 of a three-part research series, a leak test method based on electrical conductivity and capacitance, called high voltage leak detection (HVLD), was used to find leaks in small plastic bags filled with an insulin pharmaceutical solution for human injection by Novo Nordisk A/S (Bagsværd, Denmark). To perform the test, the package is electrically grounded while being conveyed past an electrode linked to a high-voltage, low-amperage transformer. The instrument measures the current that passes from the transformer to the electrode, through the packaged product and along the package walls, to the ground. Plastic packages without defect are relatively nonconductive and yield a low voltage reading; a leaking package with electrically conductive solution located in or near the leak triggers a spike in voltage reading. Test methods were optimized and validated, enabling the detection of leaking packages with holes as small as 2.5 μm in diameter. Part 2 of this series will further explore HVLD test results as a function of package seal and product storage variables. The final Part 3 will report the impact of HVLD exposure on product stability.

The reliability and validity of the Complex Task Performance Assessment: A performance-based assessment of executive function.

PubMed

Wolf, Timothy J; Dahl, Abigail; Auen, Colleen; Doherty, Meghan

2017-07-01

The objective of this study was to evaluate the inter-rater reliability, test-retest reliability, concurrent validity, and discriminant validity of the Complex Task Performance Assessment (CTPA): an ecologically valid performance-based assessment of executive function. Community control participants (n = 20) and individuals with mild stroke (n = 14) participated in this study. All participants completed the CTPA and a battery of cognitive assessments at initial testing. The control participants completed the CTPA at two different times one week apart. The intra-class correlation coefficient (ICC) for inter-rater reliability for the total score on the CTPA was .991. The ICCs for all of the sub-scores of the CTPA were also high (.889-.977). The CTPA total score was significantly correlated to Condition 4 of the DKEFS Color-Word Interference Test (p = -.425), and the Wechsler Test of Adult Reading (p  = -.493). Finally, there were significant differences between control subjects and individuals with mild stroke on the total score of the CTPA (p = .007) and all sub-scores except interpretation failures and total items incorrect. These results are also consistent with other current executive function performance-based assessments and indicate that the CTPA is a reliable and valid performance-based measure of executive function.

Brief screening for mild cognitive impairment: validation of the Brazilian version of the Montreal cognitive assessment.

PubMed

Memória, Cláudia M; Yassuda, Mônica S; Nakano, Eduardo Y; Forlenza, Orestes V

2013-01-01

The Montreal Cognitive Assessment (MoCA) is a brief cognitive schedule that has been developed for the screening of patients with Mild Cognitive Impairment (MCI). MCI is recognized as a high-risk state for Alzheimer's disease. The aim of the present study is to examine the reliability and validity of the Brazilian version of the MoCA test (MoCA-BR) in a sample of older individuals with at least 4 years of education. The MoCA-BR was administered to 112 older adults who were classified into three diagnostic groups according to their cognitive state (Alzheimer's disease, n = 28; MCI, n = 43; normal controls, n = 41). This procedure was based on clinical and neuropsychological data. The performance in the MoCA-BR was compared with the Mini-mental state examination (MMSE) and the Cambridge Cognitive Examination. Diagnostic accuracy was examined with the receiver operating characteristic (ROC) curve analyses. Cronbach's alpha for the MoCA-BR was 0.75. Temporal stability (retesting after 3 months) using intraclass correlation coefficient was 0.75 (p < 0.001). The sensitivity and specificity of the MoCA-BR for MCI were 81% and 77%, respectively, with a cut-off score of 25 points. The area under the ROC curve for predicting MCI was 0.82 ± 0.06. The present results indicate that the MoCA-BR maintains its core diagnostic properties rendering it a valid and reliable tool for the screening of MCI among older individuals with at least 4 years of education. Copyright © 2012 John Wiley & Sons, Ltd.

Development and validation of a simple and sensitive method for quantification of levodopa and carbidopa in rat and monkey plasma using derivatization and UPLC-MS/MS.

PubMed

Junnotula, Venkatraman; Licea-Perez, Hermes

2013-05-01

A simple, selective, and sensitive quantitative method has been developed for the simultaneous determination of levodopa and carbidopa in rat and monkey plasma by protein precipitation using acetonitrile containing the derivatizing reagent, flourescamine. Derivatized products of levodopa and carbidopa were separated on a BEH C18 column (2.1 mm × 50 mm; 1.7 μm particle size) using ultra high performance liquid chromatography (UHPLC) without any further purification. Tandem mass spectrometry (MS/MS) was used for detection. The method was validated over the concentration range of 5-5000 ng/mL and 3-3000 ng/mL for levodopa and carbidopa, respectively in rat and monkey plasma. Due to the poor stability of the investigated analytes in biological matrices, a mixture of sodium metabisulfite and hydrazine dihydrochloride was used as a stabilizer. This method was successfully utilized to support pharmacokinetic studies in both species. The results from assay validations and incurred samples re-analysis show that the method is selective, sensitive and robust. To our knowledge, this is the first UHPLC-MS/MS based method that utilizes derivatization with fluorescamine and provides adequate sensitivity for both levodopa and carbidopa with 50 μL of sample and a run time of 3.5 min. Copyright © 2013 Elsevier B.V. All rights reserved.

Stability of cognitive performance in children with mild intellectual disability.

PubMed

Jenni, Oskar G; Fintelmann, Sylvia; Caflisch, Jon; Latal, Beatrice; Rousson, Valentin; Chaouch, Aziz

2015-05-01

Longitudinal studies that have examined cognitive performance in children with intellectual disability more than twice over the course of their development are scarce. We assessed population and individual stability of cognitive performance in a clinical sample of children with borderline to mild non-syndromic intellectual disability. Thirty-six children (28 males, eight females; age range 3-19y) with borderline to mild intellectual disability (Full-scale IQ [FSIQ] 50-85) of unknown origin were examined in a retrospective clinical case series using linear mixed models including at least three assessments with standardized intelligence tests. Average cognitive performance remained remarkably stable over time (high population stability, drop of only 0.38 IQ points per year, standard error=0.39, p=0.325) whereas individual stability was at best moderate (intraclass correlation of 0.58), indicating that about 60% of the residual variation in FSIQ scores can be attributed to between-child variability. Neither sex nor socio-economic status had a statistically significant impact on FSIQ. Although intellectual disability during childhood is a relatively stable phenomenon, individual stability of IQ is only moderate, likely to be caused by test-to-test reliability (e.g. level of child's cooperation, motivation, and attention). Therefore, clinical decisions and predictions should not rely on single IQ assessments, but should also consider adaptive functioning and previous developmental history. © 2014 Mac Keith Press.

The Effect of Blunt-Trailing-Edge Modifications on the High-Speed Stability and Control Characteristics of a Swept-Wing Fighter Airplane

NASA Technical Reports Server (NTRS)

Sadoff, Melvin; Matteson, Frederick H.; Van Dyke, Rudolph D., Jr.

1954-01-01

An investigation was conducted on a 35 deg swept-wing fighter airplane to determine the effects of several blunt-trailing-edge modifications to the wing and tail on the high-speed stability and control characteristics and tracking performance. The results indicated significant improvement in the pitch-up characteristics for the blunt-aileron configuration at Mach numbers around 0.90. As a result of increased effectiveness of the blunt-trailing-edge aileron, the roll-off, customarily experienced with the unmodified airplane in wings-level flight between Mach numbers of about 0.9 and 1.0 was eliminated, The results also indicated that the increased effectiveness of the blunt aileron more than offset the large associated aileron hinge moment, resulting in significant improvement in the rolling performance at Mach numbers between 0.85 and 1.0. It appeared from these results that the tracking performance with the blunt-aileron configuration in the pitch-up and buffeting flight region at high Mach numbers was considerably improved over that of the unmodified airplane; however, the tracking errors of 8 to 15 mils were definitely unsatisfactory. A drag increment of about O.OOl5 due to the blunt ailerons was noted at Mach numbers to about 0.85. The drag increment was 0 at Mach numbers above 0.90.

Development and Validation of New Discriminative Dissolution Method for Carvedilol Tablets

PubMed Central

Raju, V.; Murthy, K. V. R.

2011-01-01

The objective of the present study was to develop and validate a discriminative dissolution method for evaluation of carvedilol tablets. Different conditions such as type of dissolution medium, volume of dissolution medium and rotation speed of paddle were evaluated. The best in vitro dissolution profile was obtained using Apparatus II (paddle), 50 rpm, 900 ml of pH 6.8 phosphate buffer as dissolution medium. The drug release was evaluated by high-performance liquid chromatographic method. The dissolution method was validated according to current ICH and FDA guidelines using parameters such as the specificity, accuracy, precision and stability were evaluated and obtained results were within the acceptable range. The comparison of the obtained dissolution profiles of three different products were investigated using ANOVA-based, model-dependent and model-independent methods, results showed that there is significant difference between the products. The dissolution test developed and validated was adequate for its higher discriminative capacity in differentiating the release characteristics of the products tested and could be applied for development and quality control of carvedilol tablets. PMID:22923865

The Resilience Questionnaire for Bipolar Disorder: Development and validation.

PubMed

Echezarraga, Ainara; Las Hayas, Carlota; González-Pinto, Ana María; Jones, Steven

2017-08-01

The goal of this research project was to develop a new questionnaire to assess resilience in Bipolar Disorder (BD), the Resilience Questionnaire for Bipolar Disorder (RBD). To examine its psychometric properties, a sample of 125 patients diagnosed with BD and a comparison sample of 107 people completed the new RBD and established measures of generic resilience and health-related outcomes. Exploratory factor analysis for the RBD yielded a 23-item 5-factor solution, and confirmatory factor analysis indicated adequate fit indices. Internal consistency, stability, concurrent validation and known-groups' validity were also supported. The RBD obtained higher responsiveness (6-month follow-up) than the generic resilience scale (BD sample). The RBD is a robust measure to monitor resilience in BD. Copyright © 2017 Elsevier Inc. All rights reserved.

Laser source for dimensional metrology: investigation of an iodine stabilized system based on narrow linewidth 633 nm DBR diode

NASA Astrophysics Data System (ADS)

Rerucha, Simon; Yacoot, Andrew; Pham, Tuan M.; Cizek, Martin; Hucl, Vaclav; Lazar, Josef; Cip, Ondrej

2017-04-01

We demonstrated that an iodine stabilized distributed Bragg reflector (DBR) diode based laser system lasing at a wavelength in close proximity to λ =633 nm could be used as an alternative laser source to the helium-neon lasers in both scientific and industrial metrology. This yields additional advantages besides the optical frequency stability and coherence: inherent traceability, wider optical frequency tuning range, higher output power and high frequency modulation capability. We experimentally investigated the characteristics of the laser source in two major steps: first using a wavelength meter referenced to a frequency comb controlled with a hydrogen maser and then on an interferometric optical bench testbed where we compared the performance of the laser system with that of a traditional frequency stabilized He-Ne laser. The results indicate that DBR diode laser system provides a good laser source for applications in dimensional (nano)metrology, especially in conjunction with novel interferometric detection methods exploiting high frequency modulation or multiaxis measurement systems.

Psychometric properties of the Chinese version of the Life Attitude Schedule (LAS-C) in a sample of Taiwanese adolescents.

PubMed

Chang, Hsiu-Ju; Wu, Chiung-Jane; Chen, Tzen Wen; Cheng, Andrew Tai Ann; Lin, Kuan-Chia; Rong, Jiin-Ru; Lee, Hsin-Chien

2011-05-01

Although prior research has proposed that several risk factors are conceptually and positively related to suicidal behavior, researchers have also suggested that suicide may be multifaceted. The Life Attitude Schedule (LAS) measures a broad range of suicide-related behaviors, including life-enhancing and life-threatening behaviors. This study aimed to translate the LAS into Chinese and evaluate the psychometric properties of the new version (LAS-C). A cross-sectional and descriptive design was used. Data were collected from high schools in the city of Taipei in northern Taiwan. A convenience sample of 1492 high school students was recruited from five high schools in Taipei. We used the Multi-Health Systems (MHS) translation policy to guide the translation process. Reliability was evaluated by internal consistency (represented by Cronbach's α coefficients) and test-retest (represented by intraclass correlation). Validity was demonstrated by content, convergent, divergent, concurrent, and contrast group comparison. Confirmatory factor analysis was further used to examine the theoretical model and to support construct validity. The Cronbach's α coefficient for the whole scale of the LAS-C and its subscales ranged from 0.70 to 0.91. The Intraclass Correlation Coefficient (ICC) ranged from 0.76 to 0.89 on the whole scale and its subscales, and were all statistically significant, at least at the p<0.05 level, indicating good stability over a three-week period. Validity was supported by a Content Validity Index (CVI) of 0.99, convergent, divergent, current, and contrast group comparison validity. Confirmatory factor analysis supported the theoretical model, further providing solid evidence of construct validity. The LAS-C has proper psychometric properties. Future studies must be conducted to shorten the items to form a briefer version. Copyright © 2010 Elsevier Ltd. All rights reserved.

Does Poor Spelling Equate to Slow Reading? The Relationship between Reading, Spelling, and Orthographic Quality

ERIC Educational Resources Information Center

Martin-Chang, Sandra; Ouellette, Gene; Madden, Melanie

2014-01-01

High quality lexical representations in memory, characterized by accuracy and stability, are said to underpin fluent reading. Here, the relationship between orthographic quality and reading speed was examined by asking undergraduates (N = 74) to repeatedly read and spell words. Spelling performance over five trials indicated orthographic quality.…

Validated stability-indicating HPLC method for paricalcitol in pharmaceutical dosage form according to ICH guidelines: application to stability studies.

PubMed

Ortega, Raquel; Navas, Natalia; Salmerón, Antonio; Cabeza, José; Capitán-Vallvey, Luís F

2011-01-01

A stability-indicating HPLC method with diode array detection for the determination of paricalcitol, a synthetic vitamin D2 analog, was developed. Analytical parameters were studied according to International Conference on Harmonization guidelines. A C18 column (250 x 4.6 mm, 5 microm particle size) maintained at 25 degrees C was used as the stationary phase, and acetonitrile-water (70 + 30, v/v) as the mobile phase. Chromatograms were recorded at 250 nm. In forced degradation studies, the effects of acid, base, oxidation, temperature, and UV light were investigated and showed no interference with the drug peak. The method was found to be linear (r = 0.9989) at concentrations ranging from 0.6 to 10.0 mg/L paricalcitol, precise (repeatability and intermediate precision estimated as RSD less than 3.5%), accurate (recoveries higher than 95%), specific, and robust. The LOD and LOQ were 0.6 and 0.2 mg/L, respectively. The validated method was used for paricalcitol determination in a formal stability study of its pharmaceutical dosage form in preloaded syringes. The stability of a diluted solution of its pharmaceutical form in Viaflo bags was also tested. The results showed that paricalcitol was stable in preloaded syringes during a period of 30 days from preparation in the different storage conditions tested (room temperature without protection from daylight and 4.4 degrees C with protection from daylight). On the contrary, paricalcitol was quickly lost when stored in Viaflo bags by adsorption onto the walls of the container.

Psychometric properties of the Penn State Worry Questionnaire for children in a large clinical sample.

PubMed

Pestle, Sarah L; Chorpita, Bruce F; Schiffman, Jason

2008-04-01

The Penn State Worry Questionnaire for Children (PSWQ-C; Chorpita, Tracey, Brown, Collica, & Barlow, 1997) is a 14-item self-report measure of worry in children and adolescents. Although the PSWQ-C has demonstrated favorable psychometric properties in small clinical and large community samples, this study represents the first psychometric evaluation of the PSWQ-C in a large clinical sample (N = 491). Factor analysis indicated a two-factor structure, in contrast to all previously published findings on the measure. The PSWQ-C demonstrated favorable psychometric properties in this sample, including high internal consistency, high convergent validity with related constructs, and acceptable discriminative validity between diagnostic categories. The performance of the 3 reverse-scored items was closely examined, and results indicated retaining all 14 items.

Characterization of cementitiously stabilized subgrades for mechanistic-empirical pavement design

NASA Astrophysics Data System (ADS)

Solanki, Pranshoo

Pavements are vulnerable to subgrade layer performance because it acts as a foundation. Due to increase in the truck traffic, pavement engineers are challenged to build more strong and long-lasting pavements. To increase the load-bearing capacity of pavements, subgrade layer is often stabilized with cementitious additives. Thus, an overall characterization of stabilized subgrade layer is important for enhanced short- and long-term pavement performance. In this study, the effect of type and amount of additive on the short-term performance in terms of material properties recommended by the new Mechanistic-Empirical Pavement Design Guide (MEPDG) is examined. A total of four soils commonly encountered as subgrades in Oklahoma are utilized. Results show that the changes in the Mr, ME and UCS values stabilized specimens depend on the soil type and properties of additives. The long-term performance (or durability) of stabilized soil specimens is investigated by conducting freeze-thaw (F-T) cycling, vacuum saturation and tube suction tests on 7-day cured P-, K- and C-soil specimens stabilized with 6% lime, 10% CFA and 10% CKD. This study is motivated by the fact that during the service life of pavement stabilized layers are subjected to F-T cycles and moisture variations. It is found that that UCS value of all the stabilized specimens decreased with increase in the number of F-T cycles. A strong correlation was observed between UCS values retained after vacuum saturation and F-T cycles indicating that vacuum saturation could be used as a time-efficient and inexpensive method for evaluating durability of stabilized soils. In this study, short- and long-term observations from stabilization of sulfate bearing soil with locally available low (CFA), moderate (CKD) and high (lime) calcium-based stabilizers are determined to evaluate and compare the effect of additive type on the phenomenon of sulfate-induced heave. The impact of different factors on the development of the ettringite, responsible for sulfate-induced heaving, is also discussed. For Level 2 design of pavements, a total of four stress-based statistical models and two feed-forward-type artificial neural network (ANN) models, are evaluated for predicting resilient modulus of 28-day cured stabilized specimens. Specifically, one semi-log stress-based, three log-log stress-based, one Multi-Layer Perceptrons Network (MLPN), and one Radial Basis Function Network (RBFN) are developed. Overall, semi-log stress-based and MLPN neural network are found to show best acceptable performance for the present evaluation and validation datasets. Further, correlations are presented for stress-based models to correlate Mr with compacted specimen characteristics and soil/additive properties. Additionally, the effect of type of additive on indirect tensile and fatigue characteristics of selected stabilized P- and V-soil is evaluated. This study is based on the fact that stabilized layer is subjected to tensile stresses under wheel loading. Thus, the resilient modulus in tension (M rt), fatigue life and strength in tension (sigmat) or flexure (represented by modulus of rupture, MOR) becomes another important design parameter within the mechanistic framework. Cylindrical specimens are prepared, cured for 28 days and subjected to different stress sequences in indirect tension to study the Mrt. On the other hand, stabilized beam specimens are compacted using a Linear Kneading Compactor and subjected to repeated cycles of reloading-unloading after 28 days of curing in a four-point beam fatigue apparatus for evaluating fatigue life and flexural stiffness. It is found that all three additives improved the Mrt, sigmat and MOR values; however, degree of improvement varied with the type of additive and soil. This study encompasses the differences in the design of semi-rigid pavements developed using AASHTO 1993 and AASHTO 2002 MEPDG methodologies. Further, the design curves for fatigue performance prediction of stabilized layers are developed for different stabilized pavement sections. Knowledge gained from the parametric analysis of different sections using AASHTO 1993 and MEPDG is expected to be useful to pavement designers and others in implementation of the new MEPDG for future pavement design. (Abstract shortened by UMI.)

Validation of the Long-term Difficulties Inventory (LDI) and the List of Threatening Experiences (LTE) as measures of stress in epidemiological population-based cohort studies.

PubMed

Rosmalen, J G M; Bos, E H; de Jonge, P

2012-12-01

Stress questionnaires are included in many epidemiological cohort studies but the psychometric characteristics of these questionnaires are largely unknown. The aim of this study was to describe these characteristics for two short questionnaires measuring the lifetime and past year occurrence of stress: the List of Threatening Events (LTE) as a measure of acute stress and the Long-term Difficulties Inventory (LDI) as a measure of chronic stress. This study was performed in a general population cohort consisting of 588 females (53.7%) and 506 males (46.3%), with a mean age of 53.5 years (s.d.=11.3 years). Respondents completed the LTE and the LDI for the past year, and for the age categories of 0-12, 13-18, 19-39, 40-60, and >60 years. They also completed questionnaires on perceived stress, psychological distress (the General Health Questionnaire, GHQ-12), anxiety and depression (the Symptom Checklist, SCL-8) and neuroticism (the Eysenck Personality Questionnaire - Revised Short Scale, EPQ-RSS-N). Approximately 2 years later, 976 respondents (89%) completed these questionnaires for a second time. The stability of the retrospective reporting of long-term difficulties and life events was satisfactory: 0.7 for the lifetime LDI and 0.6 for the lifetime LTE scores. The construct validity of these lists is indicated by their positive associations with psychological distress, mental health problems and neuroticism. This study in a large population-based sample shows that the LDI and LTE have sufficient validity and stability to include them in major epidemiological cohort studies.

Integration and Test Flight Validation Plans for the Pulsed Plasma Thruster Experiment on EO- 1

NASA Technical Reports Server (NTRS)

Zakrzwski, Charles; Benson, Scott; Sanneman, Paul; Hoskins, Andy; Bauer, Frank H. (Technical Monitor)

2002-01-01

The Pulsed Plasma Thruster (PPT) Experiment on the Earth Observing One (EO-1) spacecraft has been designed to demonstrate the capability of a new generation PPT to perform spacecraft attitude control. The PPT is a small, self-contained pulsed electromagnetic propulsion system capable of delivering high specific impulse (900-1200 s), very small impulse bits (10-1000 uN-s) at low average power (less than 1 to 100 W). Teflon fuel is ablated and slightly ionized by means of a capacitative discharge. The discharge also generates electromagnetic fields that accelerate the plasma by means of the Lorentz Force. EO-1 has a single PPT that can produce thrust in either the positive or negative pitch direction. The flight validation has been designed to demonstrate of the ability of the PPT to provide precision pointing accuracy, response and stability, and confirmation of benign plume and EMI effects. This paper will document the success of the flight validation.

Novel 3D bio-macromolecular bilinear descriptors for protein science: Predicting protein structural classes.

PubMed

Marrero-Ponce, Yovani; Contreras-Torres, Ernesto; García-Jacas, César R; Barigye, Stephen J; Cubillán, Néstor; Alvarado, Ysaías J

2015-06-07

In the present study, we introduce novel 3D protein descriptors based on the bilinear algebraic form in the ℝ(n) space on the coulombic matrix. For the calculation of these descriptors, macromolecular vectors belonging to ℝ(n) space, whose components represent certain amino acid side-chain properties, were used as weighting schemes. Generalization approaches for the calculation of inter-amino acidic residue spatial distances based on Minkowski metrics are proposed. The simple- and double-stochastic schemes were defined as approaches to normalize the coulombic matrix. The local-fragment indices for both amino acid-types and amino acid-groups are presented in order to permit characterizing fragments of interest in proteins. On the other hand, with the objective of taking into account specific interactions among amino acids in global or local indices, geometric and topological cut-offs are defined. To assess the utility of global and local indices a classification model for the prediction of the major four protein structural classes, was built with the Linear Discriminant Analysis (LDA) technique. The developed LDA-model correctly classifies the 92.6% and 92.7% of the proteins on the training and test sets, respectively. The obtained model showed high values of the generalized square correlation coefficient (GC(2)) on both the training and test series. The statistical parameters derived from the internal and external validation procedures demonstrate the robustness, stability and the high predictive power of the proposed model. The performance of the LDA-model demonstrates the capability of the proposed indices not only to codify relevant biochemical information related to the structural classes of proteins, but also to yield suitable interpretability. It is anticipated that the current method will benefit the prediction of other protein attributes or functions. Copyright © 2015 Elsevier Ltd. All rights reserved.

A fast and validated method for the determination of malondialdehyde in fish liver using high-performance liquid chromatography with a photodiode array detector.

PubMed

Faizan, Mohammad; Esatbeyoglu, Tuba; Bayram, Banu; Rimbach, Gerald

2014-04-01

Malondialdehyde (MDA) is a biomarker of lipid peroxidation and is present in foods and biological samples such as plasma. A high-performance liquid chromatography (HPLC) method was applied to determine MDA in fish liver samples after derivatization with 2,4-dinitrophenylhydrazine (DNPH) using a ODS2 column (10 cm × 4.6 mm, 3 μm) and a photodiode array detector. The mobile phase consisted of 0.2% acetic acid (v/v) in distilled water and acetonitrile (42:58, v/v). The present method was validated in terms of linearity, lower limit of quantification, lower limit of detection, precision, accuracy, recovery, and stability of MDA according to U.S. Food and Drug Administration (FDA) guidelines. The limit of quantification of MDA was 0.39 μmol/L, which is comparable to other methods. The recovery of the spiked MDA liver samples was in the range of 92.4% to 104.2%. This newly modified HPLC method is specific, sensitive, and accurate and allows the analysis of MDA within 4 min in fish liver but also in other tissues and plasma. © 2014 Institute of Food Technologists®

Validation and Application of an Ultra High-Performance Liquid Chromatography Tandem Mass Spectrometry Method for Yuanhuacine Determination in Rat Plasma after Pulmonary Administration: Pharmacokinetic Evaluation of a New Drug Delivery System.

PubMed

Li, Man; Liu, Xiao; Cai, Hao; Shen, Zhichun; Xu, Liu; Li, Weidong; Wu, Li; Duan, Jinao; Chen, Zhipeng

2016-12-16

Yuanhuacine was found to have significant inhibitory activity against A-549 human lung cancer cells. However, there would be serious adverse toxicity effects after systemic administration of yuanhuacine, such as by oral and intravenous ways. In order to achieve better curative effect and to alleviate the adverse toxicity effects, we tried to deliver yuanhuacine directly into the lungs. Ultra high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) was used to detect the analyte and IS. After extraction (ether:dichloromethane = 8:1), the analyte and IS were separated on a Waters BEH-C 18 column (100 mm × 2.1 mm, 1.7 μm) under a 5 min gradient elution using a mixture of acetonitrile and 0.1% formic acid aqueous solution as mobile phase at a flow rate of 0.3 mL/min. ESI positive mode was chosen for detection. The method was fully validated for its selectivity, accuracy, precision, stability, matrix effect, and extraction recovery. This new method for yuanhuacine concentration determination in rat plasma was reliable and could be applied for its preclinical and clinical monitoring purpose.

Performance of ITER as a burning plasma experiment

NASA Astrophysics Data System (ADS)

Shimada, M.; Mukhovatov, V.; Federici, G.; Gribov, Y.; Kukushkin, A.; Murakami, Y.; Polevoi, A.; Pustovitov, V.; Sengoku, S.; Sugihara, M.

2004-02-01

Recent performance analysis has improved confidence in achieving Q (= fusion power/auxiliary heating power)geq 10 in inductive operation in ITER. Performance analysis based on empirical scalings shows the feasibility of achieving Q geq 10 in inductive operation, particularly with improved modelling of helium exhaust. Analysis has also indicated the possibility that ITER can potentially demonstrate Q ~ 50, enabling studies of self-heated plasmas. Theory-based core modelling indicates the need for a high pedestal temperature (3.2-5.3 keV) to achieve Q geq 10, which is in the range of projections with presently available pedestal scalings. Pellet injection from the high-field side would be useful in enhancing Q and reducing edge localized mode (ELM) heat load in high plasma current operation. If the ELM heat load is not acceptable, it could be made tolerable by further tilting the target plate. Steady state operation scenarios at Q = 5 have been developed with modest requirements on confinement improvement and beta (HH98(y,2) geq 1.3 and bgrN geq 2.6). Stabilization of the resistive wall modes (RWMs), required in such regimes, is feasible with the present saddle coils and power supplies with double-wall structures taken into account. Recent analysis shows a potential of high power steady state operation with a fusion power of 0.7 GW at Q ~ 8. Achievement of the required bgrN ~ 3.6 by RWM stabilization is a possibility. Further analysis is also needed on reduction of the divertor target heat load.

Numerical Simulation and Validation of a High Head Model Francis Turbine at Part Load Operating Condition

NASA Astrophysics Data System (ADS)

Goyal, Rahul; Trivedi, Chirag; Kumar Gandhi, Bhupendra; Cervantes, Michel J.

2017-07-01

Hydraulic turbines are operated over an extended operating range to meet the real time electricity demand. Turbines operated at part load have flow parameters not matching the designed ones. This results in unstable flow conditions in the runner and draft tube developing low frequency and high amplitude pressure pulsations. The unsteady pressure pulsations affect the dynamic stability of the turbine and cause additional fatigue. The work presented in this paper discusses the flow field investigation of a high head model Francis turbine at part load: 50% of the rated load. Numerical simulation of the complete turbine has been performed. Unsteady pressure pulsations in the vaneless space, runner, and draft tube are investigated and validated with available experimental data. Detailed analysis of the rotor stator interaction and draft tube flow field are performed and discussed. The analysis shows the presence of a rotating vortex rope in the draft tube at the frequency of 0.3 times of the runner rotational frequency. The frequency of the vortex rope precession, which causes severe fluctuations and vibrations in the draft tube, is predicted within 3.9% of the experimental measured value. The vortex rope results pressure pulsations propagating in the system whose frequency is also perceive in the runner and upstream the runner.

Identification, characterization, and high-performance liquid chromatography quantification of process-related impurities in vonoprazan fumarate.

PubMed

Liu, Lei; Cao, Na; Ma, Xingling; Xiong, Kaihe; Sun, Lili; Zou, Qiaogen

2016-04-01

High-performance liquid chromatography analysis of vonoprazan fumarate, a novel proton pump inhibitor drug revealed six impurities. These were identified by liquid chromatography with mass spectrometry. Further, the structures of the impurities were confirmed by synthesis followed by characterization by mass spectrometry, NMR spectroscopy, and infrared spectroscopy. On the basis of these data and knowledge of the synthetic scheme of vonoprazan fumarate, the previously unknown impurity was identified as 1-[5-(2-fluorophenyl)-1-(pyridin-3-ylsulfonyl)-1H-pyrrol-3-yl]-N-methyldimethylamine, which is a new compound. The possible mechanisms by which these impurities were formed were also discussed. A high-performance liquid chromatography method was optimized in order to separate, selectively detect, and quantify all process-related impurities of vonoprazan fumarate. The presented method has been validated in terms of linearity, limits of detection, and quantification, and response factors and, therefore, is highly suitable for routine analysis of vonoprazan fumarate related substances as well as stability studies. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Validity of a physical activity questionnaire in Shanghai.

PubMed

Peters, Tricia M; Shu, Xiao-Ou; Moore, Steven C; Xiang, Yong Bing; Yang, Gong; Ekelund, Ulf; Liu, Da-Ke; Tan, Yu-Ting; Ji, Bu-Tian; Schatzkin, Arthur S; Zheng, Wei; Chow, Wong Ho; Matthews, Charles E; Leitzmann, Michael F

2010-12-01

In large epidemiologic studies, physical activity (PA) is often assessed using PA questionnaires (PAQ). Because available PAQ may not capture the full range of PA in which urban Chinese adults engage, a PAQ was developed for this purpose. We examined the validity of this PAQ and the 1-yr stability of PA in 545 urban Shanghai adults. The PAQ was interview-administered twice, approximately 1 yr apart, and participants also wore an accelerometer and completed a PA-log for seven consecutive days every 3 months during the same year. The intraclass correlation coefficient (ICC) was used to evaluate the stability of PA across questionnaire administrations, and Spearman correlation coefficients (ρ) and mean differences and 95% limits of agreement were used to examine the validity of the questionnaire compared against accelerometry and the PA-log. When measured by accelerometry, estimates of time spent in moderate-to-vigorous PA were lower and estimates of time spent sedentary were higher than when self-reported on the PAQ (P < 0.001). Total PA (ICC = 0.65) and PA domains (ICC = 0.45-0.85) showed moderate to high stability across PAQ administrations. Total PA (ρ = 0.30), moderate-to-vigorous activity (ρ = 0.17), light activity (ρ = 0.36), and sedentary behavior (ρ = 0.16) assessed by PAQ and by accelerometry were significantly and positively correlated, and correlations of the PAQ with the PA-log (ρ = 0.36-0.85) were stronger than those observed with accelerometry. The PAQ significantly overestimated time spent in moderate-to-vigorous activity and underestimated time spent in light activity and sedentary behavior compared with accelerometry, but it performed well at ranking participants according to PA level.

Meshless collocation methods for the numerical solution of elliptic boundary valued problems the rotational shallow water equations on the sphere

NASA Astrophysics Data System (ADS)

Blakely, Christopher D.

This dissertation thesis has three main goals: (1) To explore the anatomy of meshless collocation approximation methods that have recently gained attention in the numerical analysis community; (2) Numerically demonstrate why the meshless collocation method should clearly become an attractive alternative to standard finite-element methods due to the simplicity of its implementation and its high-order convergence properties; (3) Propose a meshless collocation method for large scale computational geophysical fluid dynamics models. We provide numerical verification and validation of the meshless collocation scheme applied to the rotational shallow-water equations on the sphere and demonstrate computationally that the proposed model can compete with existing high performance methods for approximating the shallow-water equations such as the SEAM (spectral-element atmospheric model) developed at NCAR. A detailed analysis of the parallel implementation of the model, along with the introduction of parallel algorithmic routines for the high-performance simulation of the model will be given. We analyze the programming and computational aspects of the model using Fortran 90 and the message passing interface (mpi) library along with software and hardware specifications and performance tests. Details from many aspects of the implementation in regards to performance, optimization, and stabilization will be given. In order to verify the mathematical correctness of the algorithms presented and to validate the performance of the meshless collocation shallow-water model, we conclude the thesis with numerical experiments on some standardized test cases for the shallow-water equations on the sphere using the proposed method.

Performance status of the AIRS instrument thirteen years after launch

NASA Astrophysics Data System (ADS)

Elliott, Denis A.; Pagano, Thomas S.; Aumann, Hartmut H.; Broberg, Steven E.

2015-09-01

The Atmospheric Infrared Sounder (AIRS) is a hyperspectral infrared instrument on the EOS Aqua Spacecraft, launched on May 4, 2002. AIRS has 2378 infrared channels ranging from 3.7 μm to 15.4 μm and a 13.5 km footprint at nadir. AIRS is a "facility" instrument developed by NASA as an experimental demonstration of advanced technology for remote sensing and the benefits of high resolution infrared spectra to science investigations. AIRS, in conjunction with the Advanced Microwave Sounding Unit (AMSU), produces temperature profiles with 1K/km accuracy on a global scale, as well as water vapor profiles and trace gas amounts for CO2 , CO, SO2 , O3 and CH4. AIRS data are used for weather forecasting, climate process studies and validating climate models. The AIRS instrument has far exceeded its required design life of 5 years, with nearly 13 years of routine science operations that began on August 31, 2002. While the instrument has performed exceptionally well, with little sign of wear, the AIRS Project continues to monitor and maintain the health of AIRS, characterize its behavior and improve performance where possible. Radiometric stability has been monitored and trending shows better than 16 mK/year stability. Spectral calibration stability is better than 1 ppm/year. At this time we expect the AIRS to continue to perform well into the next decade. This paper contains updates to previous instrument status reports, with emphasis on the last three years.

A Note on the Incremental Validity of Aggregate Predictors.

ERIC Educational Resources Information Center

Day, H. D.; Marshall, David

Three computer simulations were conducted to show that very high aggregate predictive validity coefficients can occur when the across-case variability in absolute score stability occurring in both the predictor and criterion matrices is quite small. In light of the increase in internal consistency reliability achieved by the method of aggregation…

Advanced Li-Ion Hybrid Supercapacitors Based on 3D Graphene-Foam Composites.

PubMed

Liu, Wenwen; Li, Jingde; Feng, Kun; Sy, Abel; Liu, Yangshuai; Lim, Lucas; Lui, Gregory; Tjandra, Ricky; Rasenthiram, Lathankan; Chiu, Gordon; Yu, Aiping

2016-10-05

Li-ion hybrid supercapacitors (LIHSs) have recently attracted increasing attention as a new and promising energy storage device. However, it is still a great challenge to construct novel LIHSs with high-performance due to the majority of battery-type anodes retaining the sluggish kinetics of Li-ion storage and most capacitor-type cathodes with low specific capacitance. To solve this problem, 3D graphene-wrapped MoO 3 nanobelt foam with the unique porous network structure has been designed and prepared as anode material, which delivers high capacity, improved rate performance, and enhanced cycle stability. First-principles calculation reveals that the combination of graphene dramatically reduces the diffusion energy barrier of Li + adsorbed on the surface of MoO 3 nanobelt, thus improving its electrochemical performance. Furthermore, 3D graphene-wrapped polyaniline nanotube foam derived carbon is employed as a new type of capacitor-type cathode, demonstrating high specific capacitance, good rate performance, and long cycle stability. Benefiting from these two graphene foam-enhanced materials, the constructed LIHSs show a wide operating voltage range (3.8 V), a long stable cycle life (90% capacity retention after 3000 cycles), a high energy density (128.3 Wh·kg -1 ), and a high power density (13.5 kW·kg -1 ). These encouraging performances indicate that the obtained LIHSs may have promising prospect as next-generation energy-storage devices.

Developing and validating a scale to measure Food and Nutrition Literacy (FNLIT) in elementary school children in Iran.

PubMed

Doustmohammadian, Aazam; Omidvar, Nasrin; Keshavarz-Mohammadi, Nastaran; Abdollahi, Morteza; Amini, Maryam; Eini-Zinab, Hassan

2017-01-01

Food and nutrition literacy is an emerging term which is increasingly used in policy and research. Though research in this area is growing, progression is limited by the lack of an accepted method to measure food and nutrition literacy. The aim of this study is to develop a valid and reliable questionnaire to assess food and nutrition literacy in elementary school children in the city of Tehran. The study was conducted in three phases. To develop Food and Nutrition Literacy (FNLIT) questionnaire, a comprehensive literature review and a qualitative study were initially performed to identify food and nutrition literacy dimensions and its components. Content and face validity of the questionnaire were evaluated by an expert panel as well as students. In the second phase, construct validity of the scale was evaluated using Explanatory Factor Analyses (EFA) and Confirmatory Factor Analyses (CFA). In the last phase (confirmatory phase), the final version of the questionnaire was evaluated on 400 students. Findings show Content Validity Ratio (CVR) and Content Validity Index (CVI) of the 62-item questionnaire at acceptable levels of 0.87 and 0.92, respectively. EFA suggested a six-factor construct, namely, understanding food and nutrition information, knowledge, functional, interactive, food choice, and critical. The results of CFA indicated acceptable fit indices for the proposed models. All subscales demonstrated satisfactory internal consistency (Cronbach's alpha≥0.70), except for critical skill subscale (0.48). The intraclass correlation coefficient (ICC = 0.90, CI: 0.83-0.94) indicated that Food and Nutrition Literacy (FNLIT) scale had satisfactory stability. Each phase of development progressively improved the questionnaire, which resulted in a 46-item (42 likert-type items and 4 true-false items) Food and Nutrition Literacy (FNLIT) scale. The questionnaire measured two domains with 6 subscales, including: 1) cognitive domain: understanding and knowledge; 2) skill domain: functional, food choice, interactive, and critical skills. The developed food and nutrition literacy scale is a valid and reliable instrument to measure food and nutrition literacy in children. This measure lays a solid empirical and theoretical foundation for future research and tailored interventions to promote food and nutrition literacy in this age group.

Wide-Field Infrared Survey Telescope (WFIRST) Integrated Modeling

NASA Technical Reports Server (NTRS)

Liu, Kuo-Chia; Blaurock, Carl

2017-01-01

Contents: introduction to WFIRST (Wide-Field Infrared Survey Telescope) and integrated modeling; WFIRST stability requirement summary; instability mitigation strategies; dynamic jitter results; STOP (structural-thermal-optical performance) (thermal distortion) results; STOP and jitter capability limitations; model validation philosophy.

Development of Modal Analysis for the Study of Global Modes in High Speed Boundary Layer Flows

NASA Astrophysics Data System (ADS)

Brock, Joseph Michael

Boundary layer transition for compressible flows remains a challenging and unsolved problem. In the context of high-speed compressible flow, transitional and turbulent boundary-layers produce significantly higher surface heating caused by an increase in skin-friction. The higher heating associated with transitional and turbulent boundary layers drives thermal protection systems (TPS) and mission trajectory bounds. Proper understanding of the mechanisms that drive transition is crucial to the successful design and operation of the next generation spacecraft. Currently, prediction of boundary-layer transition is based on experimental efforts and computational stability analysis. Computational analysis, anchored by experimental correlations, offers an avenue to assess/predict stability at a reduced cost. Classical methods of Linearized Stability Theory (LST) and Parabolized Stability Equations (PSE) have proven to be very useful for simple geometries/base flows. Under certain conditions the assumptions that are inherent to classical methods become invalid and the use of LST/PSE is inaccurate. In these situations, a global approach must be considered. A TriGlobal stability analysis code, Global Mode Analysis in US3D (GMAUS3D), has been developed and implemented into the unstructured solver US3D. A discussion of the methodology and implementation will be presented. Two flow configurations are presented in an effort to validate/verify the approach. First, stability analysis for a subsonic cylinder wake is performed and results compared to literature. Second, a supersonic blunt cone is considered to directly compare LST/PSE analysis and results generated by GMAUS3D.

Stabilized TiN nanowire arrays for high-performance and flexible supercapacitors.

PubMed

Lu, Xihong; Wang, Gongming; Zhai, Teng; Yu, Minghao; Xie, Shilei; Ling, Yichuan; Liang, Chaolun; Tong, Yexiang; Li, Yat

2012-10-10

Metal nitrides have received increasing attention as electrode materials for high-performance supercapacitors (SCs). However, most of them are suffered from poor cycling stability. Here we use TiN as an example to elucidate the mechanism causing the capacitance loss. X-ray photoelectron spectroscopy analyses revealed that the instability is due to the irreversible electrochemical oxidation of TiN during the charging/discharging process. Significantly, we demonstrate for the first time that TiN can be stabilized without sacrificing its electrochemical performance by using poly(vinyl alcohol) (PVA)/KOH gel as the electrolyte. The polymer electrolyte suppresses the oxidation reaction on electrode surface. Electrochemical studies showed that the TiN solid-state SCs exhibit extraordinary stability up to 15,000 cycles and achieved a high volumetric energy density of 0.05 mWh/cm(3). The capability of effectively stabilizing nitride materials could open up new opportunities in developing high-performance and flexible SCs.

Identification and Validation of Novel Small Molecule Disruptors of HuR-mRNA Interaction

PubMed Central

Wu, Xiaoqing; Lan, Lan; Wilson, David Michael; Marquez, Rebecca T.; Tsao, Wei-chung; Gao, Philip; Roy, Anuradha; Turner, Benjamin Andrew; McDonald, Peter; Tunge, Jon A; Rogers, Steven A; Dixon, Dan A.; Aubé, Jeffrey; Xu, Liang

2015-01-01

HuR, an RNA binding protein, binds to adenine- and uridine-rich elements (ARE) in the 3′-untranslated region (UTR) of target mRNAs, regulating their stability and translation. HuR is highly abundant in many types of cancer, and it promotes tumorigenesis by interacting with cancer-associated mRNAs, which encode proteins that are implicated in different tumor processes including cell proliferation, cell survival, angiogenesis, invasion, and metastasis. Drugs that disrupt the stabilizing effect of HuR upon mRNA targets could have dramatic effects on inhibiting cancer growth and persistence. In order to identify small molecules that directly disrupt the HuR–ARE interaction, we established a fluorescence polarization (FP) assay optimized for high throughput screening (HTS) using HuR protein and an ARE oligo from Musashi RNA-binding protein 1 (Msi1) mRNA, a HuR target. Following the performance of an HTS of ~6000 compounds, we discovered a cluster of potential disruptors, which were then validated by AlphaLISA (Amplified Luminescent Proximity Homogeneous Assay), surface plasmon resonance (SPR), ribonucleoprotein immunoprecipitation (RNP IP) assay, and luciferase reporter functional studies. These compounds disrupted HuR–ARE interactions at the nanomolar level and blocked HuR function by competitive binding to HuR. These results support future studies toward chemical probes for a HuR function study and possibly a novel therapy for HuR-overexpressing cancers. PMID:25750985

Design conceptuel d'un avion blended wing body de 200 passagers

NASA Astrophysics Data System (ADS)

Ammar, Sami

The Blended Wing Body is built based on the flying wing concept and performance improvements compared to conventional aircraft. Contrariwise, most studies have focused on large aircraft and it is not sure whether the gains are the same for smaller aircraft. The main of objective is to perform the conceptual design of a BWB of 200 passengers and compare the performance obtained with a conventional aircraft equivalent in terms of payload and range. The design of the Blended Wing Body was carried out under the CEASIOM environment. This platform design suitable for conventional aircraft design has been modified and additional tools have been integrated in order to achieve the aerodynamic analysis, performance and stability of the aircraft fuselage built. A plane model is obtained in the geometric module AcBuilder CEASIOM from the design variables of a wing. Estimates of mass are made from semi- empirical formulas adapted to the geometry of the BWB and calculations centering and inertia are possible through BWB model developed in CATIA. Low fidelity methods, such as TORNADO and semi- empirical formulas are used to analyze the aerodynamic performance and stability of the aircraft. The aerodynamic results are validated using a high-fidelity analysis using FLUENT CFD software. An optimization process is implemented in order to obtain improved while maintaining a feasible design performance. It is an optimization of the plan form of the aircraft fuselage integrated with a number of passengers and equivalent to that of a A320.Les performance wing aircraft merged optimized maximum range are compared to A320 also optimized. Significant gains were observed. An analysis of the dynamics of longitudinal and lateral flight is carried out on the aircraft optimized BWB finesse and mass. This study identified the stable and unstable modes of the aircraft. Thus, this analysis has highlighted the stability problems associated with the oscillation of incidence and the Dutch roll for the absence of stabilizers.

Stability-indicating methods for the determination of piretanide in presence of the alkaline induced degradates.

PubMed

Youssef, Nadia F

2005-10-04

Stability-indicating high performance liquid chromatography (HPLC), thin-layer chromatography (TLC) and first-derivative of ratio spectra (1DD) methods are developed for the determination of piretanide in presence of its alkaline induced degradates. HPLC method depends on separation of piretanide from its degradates on mu-Bondapak C18 column using methanol:water:acetic acid (70:30:1, v/v/v) as a mobile phase at flow rate 1.0 ml/min and UV detector at 275 nm. TLC densitometic method is based on the difference in Rf-values between the intact drug and its degradates on thin-layer silica gel. Iso-propanol:ammonia 33% (8:2, v/v) was used as a developing mobile phase and the chromatogram was scanned at 275 nm. The derivative of ratio spectra method (1DD) depends on the measurement of the absorbance at 288 nm in the first-derivative of ratio spectra for the determination of the cited drug in the presence of its degradates. Calibration graphs of the three suggested methods are linear in the concentration ranges 0.02-0.3 microg/20 microl, 0.5-10 microg/spot and 5-50 microg/ml, with mean percentage recovery 99.27+/-0.52, 99,17+/-1.01 and 99.65+/-1.01%, respectively. The three proposed methods were successfully applied for the determination of piretanide in bulk powder, laboratory-prepared mixtures and pharmaceutical dosage form with good accuracy and precision. The results were statistically analyzed and compared with those obtained by the official method. Validation of the method was determined with favourable specificity, linearity, precision, and accuracy was assessed by applying the standard addition technique.

Maximizing and stabilizing luminescence from halide perovskites with potassium passivation

NASA Astrophysics Data System (ADS)

Abdi-Jalebi, Mojtaba; Andaji-Garmaroudi, Zahra; Cacovich, Stefania; Stavrakas, Camille; Philippe, Bertrand; Richter, Johannes M.; Alsari, Mejd; Booker, Edward P.; Hutter, Eline M.; Pearson, Andrew J.; Lilliu, Samuele; Savenije, Tom J.; Rensmo, Håkan; Divitini, Giorgio; Ducati, Caterina; Friend, Richard H.; Stranks, Samuel D.

2018-03-01

Metal halide perovskites are of great interest for various high-performance optoelectronic applications. The ability to tune the perovskite bandgap continuously by modifying the chemical composition opens up applications for perovskites as coloured emitters, in building-integrated photovoltaics, and as components of tandem photovoltaics to increase the power conversion efficiency. Nevertheless, performance is limited by non-radiative losses, with luminescence yields in state-of-the-art perovskite solar cells still far from 100 per cent under standard solar illumination conditions. Furthermore, in mixed halide perovskite systems designed for continuous bandgap tunability (bandgaps of approximately 1.7 to 1.9 electronvolts), photoinduced ion segregation leads to bandgap instabilities. Here we demonstrate substantial mitigation of both non-radiative losses and photoinduced ion migration in perovskite films and interfaces by decorating the surfaces and grain boundaries with passivating potassium halide layers. We demonstrate external photoluminescence quantum yields of 66 per cent, which translate to internal yields that exceed 95 per cent. The high luminescence yields are achieved while maintaining high mobilities of more than 40 square centimetres per volt per second, providing the elusive combination of both high luminescence and excellent charge transport. When interfaced with electrodes in a solar cell device stack, the external luminescence yield—a quantity that must be maximized to obtain high efficiency—remains as high as 15 per cent, indicating very clean interfaces. We also demonstrate the inhibition of transient photoinduced ion-migration processes across a wide range of mixed halide perovskite bandgaps in materials that exhibit bandgap instabilities when unpassivated. We validate these results in fully operating solar cells. Our work represents an important advance in the construction of tunable metal halide perovskite films and interfaces that can approach the efficiency limits in tandem solar cells, coloured-light-emitting diodes and other optoelectronic applications.

Maximizing and stabilizing luminescence from halide perovskites with potassium passivation.

PubMed

Abdi-Jalebi, Mojtaba; Andaji-Garmaroudi, Zahra; Cacovich, Stefania; Stavrakas, Camille; Philippe, Bertrand; Richter, Johannes M; Alsari, Mejd; Booker, Edward P; Hutter, Eline M; Pearson, Andrew J; Lilliu, Samuele; Savenije, Tom J; Rensmo, Håkan; Divitini, Giorgio; Ducati, Caterina; Friend, Richard H; Stranks, Samuel D

2018-03-21

Metal halide perovskites are of great interest for various high-performance optoelectronic applications. The ability to tune the perovskite bandgap continuously by modifying the chemical composition opens up applications for perovskites as coloured emitters, in building-integrated photovoltaics, and as components of tandem photovoltaics to increase the power conversion efficiency. Nevertheless, performance is limited by non-radiative losses, with luminescence yields in state-of-the-art perovskite solar cells still far from 100 per cent under standard solar illumination conditions. Furthermore, in mixed halide perovskite systems designed for continuous bandgap tunability (bandgaps of approximately 1.7 to 1.9 electronvolts), photoinduced ion segregation leads to bandgap instabilities. Here we demonstrate substantial mitigation of both non-radiative losses and photoinduced ion migration in perovskite films and interfaces by decorating the surfaces and grain boundaries with passivating potassium halide layers. We demonstrate external photoluminescence quantum yields of 66 per cent, which translate to internal yields that exceed 95 per cent. The high luminescence yields are achieved while maintaining high mobilities of more than 40 square centimetres per volt per second, providing the elusive combination of both high luminescence and excellent charge transport. When interfaced with electrodes in a solar cell device stack, the external luminescence yield-a quantity that must be maximized to obtain high efficiency-remains as high as 15 per cent, indicating very clean interfaces. We also demonstrate the inhibition of transient photoinduced ion-migration processes across a wide range of mixed halide perovskite bandgaps in materials that exhibit bandgap instabilities when unpassivated. We validate these results in fully operating solar cells. Our work represents an important advance in the construction of tunable metal halide perovskite films and interfaces that can approach the efficiency limits in tandem solar cells, coloured-light-emitting diodes and other optoelectronic applications.

Medium fidelity modelling of loads in wind farms under non-neutral ABL stability conditions - a full-scale validation study

NASA Astrophysics Data System (ADS)

Larsen, G. C.; Larsen, T. J.; Chougule, A.

2017-05-01

The aim of the present paper is to demonstrate the capability of medium fidelity modelling of wind turbine component fatigue loading, when the wind turbines are subjected to wake affected non-stationary flow fields under non-neutral atmospheric stability conditions. To accomplish this we combine the classical Dynamic Wake Meandering model with a fundamental conjecture stating: Atmospheric boundary layer stability affects primary wake meandering dynamics driven by large turbulent scales, whereas wake expansion in the meandering frame of reference is hardly affected. Inclusion of stability (i.e. buoyancy) in description of both large- and small scale atmospheric boundary layer turbulence is facilitated by a generalization of the classical Mann spectral tensor, which consistently includes buoyancy effects. With non-stationary wind turbine inflow fields modelled as described above, fatigue loads are obtained using the state-of-the art aeroelastic model HAWC2. The Lillgrund offshore wind farm (WF) constitute an interesting case study for wind farm model validation, because the WT interspacing is small, which in turn means that wake effects are significant. A huge data set, comprising 5 years of blade and tower load recordings, is available for model validation. For a multitude of wake situations this data set displays a considerable scatter, which to a large degree seems to be caused by atmospheric boundary layer stability effects. Notable is also that rotating wind turbine components predominantly experience high fatigue loading for stable stratification with significant shear, whereas high fatigue loading of non-rotating wind turbine components are associated with unstable atmospheric boundary layer stratification.

High mobility and high stability glassy metal-oxynitride materials and devices

NASA Astrophysics Data System (ADS)

Lee, Eunha; Kim, Taeho; Benayad, Anass; Hur, Jihyun; Park, Gyeong-Su; Jeon, Sanghun

2016-04-01

In thin film technology, future semiconductor and display products with high performance, high density, large area, and ultra high definition with three-dimensional functionalities require high performance thin film transistors (TFTs) with high stability. Zinc oxynitride, a composite of zinc oxide and zinc nitride, has been conceded as a strong substitute to conventional semiconductor film such as silicon and indium gallium zinc oxide due to high mobility value. However, zinc oxynitride has been suffered from poor reproducibility due to relatively low binding energy of nitrogen with zinc, resulting in the instability of composition and its device performance. Here we performed post argon plasma process on zinc oxynitride film, forming nano-crystalline structure in stable amorphous matrix which hampers the reaction of oxygen with zinc. Therefore, material properties and device performance of zinc oxynitride are greatly enhanced, exhibiting robust compositional stability even exposure to air, uniform phase, high electron mobility, negligible fast transient charging and low noise characteristics. Furthermore, We expect high mobility and high stability zinc oxynitride customized by plasma process to be applicable to a broad range of semiconductor and display devices.

School Improvement under Test-Driven Accountability: A Comparison of High- and Low-Performing Middle Schools in California. CSE Report 717

ERIC Educational Resources Information Center

Mintrop, Heinrich; Trujillo, Tina

2007-01-01

Based on in-depth data from nine demographically similar schools, the study asks five questions in regard to key aspects of the improvement process and that speak to the consequential validity of accountability indicators: Do schools that differ widely according to system performance criteria also differ on the quality of the educational…

Implementation of an adaptive controller for the startup and steady-state running of a biomethanation process operated in the CSTR mode.

PubMed

Renard, P; Van Breusegem, V; Nguyen, M T; Naveau, H; Nyns, E J

1991-10-20

An adaptive control algorithm has been implemented on a biomethanation process to maintain propionate concentration, a stable variable, at a given low value, by steering the dilution rate. It was thereby expected to ensure the stability of the process during the startup and during steady-state running with an acceptable performance. The methane pilot reactor was operated in the completely mixed, once-through mode and computer-controlled during 161 days. The results yielded the real-life validation of the adaptive control algorithm, and documented the stability and acceptable performance expected.

Preparation and characterization of titania-deposited silica composite hollow fiber membranes with high hydrothermal stability.

PubMed

Kwon, Young-Nam; Kim, In-Chul

2013-11-01

Hydrothermal stability of a porous nickel-supported silica membrane was successfully improved by deposition of titania multilayers on colloidal silica particles embedded in the porous nickel fiber support. Porous nickel-supported silica membranes were prepared by means of a dipping-freezing-fast drying (DFF) method. The titania layers were deposited on colloidal silica particles by repeating hydrolysis and condensation reactions of titanium isopropoxide on the silica particle surfaces. The deposition of thin titania layers on the nickel-supported silica membrane was verified by various analytical tools. The water flux and the solute rejection of the porous Ni fiber-supported silica membranes did not change after titania layer deposition, indicating that thickness of titania layers deposited on silica surface is enough thin not to affect the membrane performance. Moreover, improvement of the hydrothermal stability in the titania-deposited silica membranes was confirmed by stability tests, indicating that thin titania layers deposited on silica surface played an important role as a diffusion barrier against 90 degrees C water into silica particles.

High-beta steady-state research with integrated modeling in the JT-60 Upgrade

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ozeki, T.

2007-05-15

Improvement of high-beta performance and its long sustainment was obtained with ferritic steel tiles in the JT-60 Upgrade (JT-60U) [T. Fujita et al., Phys. Plasmas 50, 104 (2005)], which were installed inside the vacuum vessel to reduce fast ion loss by decreasing the toroidal field ripple. When a separation between the plasma surface and the wall was small, high-beta plasmas reached the ideal wall stability limit, i.e., the ideal magnetohydrodynamics stability limit with the wall stabilization. A small rotation velocity of 0.3% of the Alfven velocity was found to be effective for suppressing the resistive wall mode. Sustainment of themore » high normalized beta value of {beta}{sub N}=2.3 has been extended to 28.6 s ({approx}15 times the current diffusion time) by improvement of the confinement and increase in the net heating power. Based on the research in JT-60U experiments and first-principle simulations, integrated models of core, edge-pedestal, and scrape-off-layer (SOL) divertors were developed, and they clarified complex features of reactor-relevant plasmas. The integrated core plasma model indicated that the small amount of electron cyclotron (EC) current density of about half the bootstrap current density could effectively stabilize the neoclassical tearing mode by the localized EC current accurately aligned to the magnetic island center. The integrated edge-pedestal model clarified that the collisionality dependence of energy loss due to the edge-localized mode was caused by the change in the width of the unstable mode and the SOL transport. The integrated SOL-divertor model clarified the effect of the exhaust slot on the pumping efficiency and the cause of enhanced radiation near the X-point multifaceted asymmetric radiation from edge. Success in these consistent analyses using the integrated code indicates that it is an effective means to investigate complex plasmas and to control the integrated performance.« less

Quantitative determination of a chemically modified hammerhead ribozyme in blood plasma using 96-well solid-phase extraction coupled with high-performance liquid chromatography or capillary gel electrophoresis.

PubMed

Bellon, L; Maloney, L; Zinnen, S P; Sandberg, J A; Johnson, K E

2000-08-01

Versatile bioanalytical assays to detect chemically stabilized hammerhead ribozyme and putative ribozyme metabolites from plasma are described. The extraction protocols presented are based on serial solid-phase extractions performed on a 96-well plate format and are compatible with either IEX-HPLC or CGE back-end analysis. A validation of both assays confirmed that both the HPLC and the CGE methods possess the required linearity, accuracy, and precision to accurately measure concentrations of hammerhead ribozyme extracted from plasma. These methods should be of general use to detect and quantitate ribozymes from other biological fluids such as serum and urine. Copyright 2000 Academic Press.

Validity of a gambling scale for the addiction severity index.

PubMed

Petry, Nancy M

2003-06-01

This study assessed the validity of an adaptation of the Addiction Severity Index (ASI) for evaluating severity of gambling problems. Participants (N = 597) from four different populations (pathological gamblers enrolled in a treatment study, pathological gamblers initiating outpatient treatment at a community-based program, frequent gamblers recruited from advertisement, and substance abusers) completed the ASI, along with a supplemental gambling subscale (ASI-G). Internal consistency of the ASI-G was good (alpha =.90), and a principal components analysis indicated a single factor explained 73% of the variance in responses. ASI-G scores demonstrated excellent convergent validity with other measures of gambling and convergent validity with external sources, including collateral informant and clinician-rated reports. ASI-G scores discriminated among the samples tested. Temporal stability of ASI-G scores was high during a 1-month period for patients with substance abuse disorder who were not seeking gambling treatment. For treatment-seeking gamblers, the number of treatment sessions attended was significantly associated with reductions in ASI-G scores. Together, these data suggest that the ASI-G subscale may be a useful tool for assessing severity of gambling problems in a variety of populations.

High-performance flexible all-solid-state supercapacitors based on densely-packed graphene/polypyrrole nanoparticle papers

NASA Astrophysics Data System (ADS)

Yang, Chao; Zhang, Liling; Hu, Nantao; Yang, Zhi; Wei, Hao; Wang, Yanyan; Zhang, Yafei

2016-11-01

Graphene-based all-solid-state supercapacitors (ASSSCs) have received increasing attention. It's a great challenge to fabricate high-performance flexible solid-state supercapacitors with high areal and volumetric energy storage capability, superior electron and ion conductivity, robust mechanical flexibility, as well as long term stability. Herein, we report a facile method to fabricate flexible ASSSCs based on densely-packed reduced graphene oxide (rGO)/polypyrrole nanoparticle (PPy NP) hybrid papers with a sandwich framework, which consists of well-separated and continuously-aligned rGO sheets. The incorporation of PPy NPs not only provides pseudocapacitance but also facilitates the infiltration of gel electrolyte. The assembled ASSSCs possess maximum areal and volumetric specific capacitances of 477 mF/cm2 and 94.9 F/cm3 at 0.5 mA/cm2. They also exhibit little capacitance deviation under different bending states, excellent cycling stability, small leakage current and low self-discharge characteristics. Additionally, the maximum areal and volumetric energy densities of 132.5 μWh/cm2 and 26.4 mWh/cm3 are achieved, which indicate that this hybrid paper is a promising candidate for high-performance flexible energy storage devices.

Validation of an HPLC method for the quantification of ambroxol hydrochloride and benzoic acid in a syrup as pharmaceutical form stress test for stability evaluation.

PubMed

Heinänen, M; Barbas, C

2001-03-01

A method is described for ambroxol, trans-4-(2-amino-3,5-dibromobenzylamino) cyclohexanol hydrochloride, and benzoic acid separation by HPLC with UV detection at 247 nm in a syrup as pharmaceutical presentation. Optimal conditions were: Column Symmetry Shield RPC8, 5 microm 250 x 4.6 mm, and methanol/(H(3)PO(4) 8.5 mM/triethylamine pH=2.8) 40:60 v/v. Validation was performed using standards and the pharmaceutical preparation which contains the compounds described above. Results from both standards and samples show suitable validation parameters. The pharmaceutical grade substances were tested by factors that could influence the chemical stability. These reaction mixtures were analysed to evaluate the capability of the method to separate degradation products. Degradation products did not interfere with the determination of the substances tested by the assay.

High-order fractional partial differential equation transform for molecular surface construction.

PubMed

Hu, Langhua; Chen, Duan; Wei, Guo-Wei

2013-01-01

Fractional derivative or fractional calculus plays a significant role in theoretical modeling of scientific and engineering problems. However, only relatively low order fractional derivatives are used at present. In general, it is not obvious what role a high fractional derivative can play and how to make use of arbitrarily high-order fractional derivatives. This work introduces arbitrarily high-order fractional partial differential equations (PDEs) to describe fractional hyperdiffusions. The fractional PDEs are constructed via fractional variational principle. A fast fractional Fourier transform (FFFT) is proposed to numerically integrate the high-order fractional PDEs so as to avoid stringent stability constraints in solving high-order evolution PDEs. The proposed high-order fractional PDEs are applied to the surface generation of proteins. We first validate the proposed method with a variety of test examples in two and three-dimensional settings. The impact of high-order fractional derivatives to surface analysis is examined. We also construct fractional PDE transform based on arbitrarily high-order fractional PDEs. We demonstrate that the use of arbitrarily high-order derivatives gives rise to time-frequency localization, the control of the spectral distribution, and the regulation of the spatial resolution in the fractional PDE transform. Consequently, the fractional PDE transform enables the mode decomposition of images, signals, and surfaces. The effect of the propagation time on the quality of resulting molecular surfaces is also studied. Computational efficiency of the present surface generation method is compared with the MSMS approach in Cartesian representation. We further validate the present method by examining some benchmark indicators of macromolecular surfaces, i.e., surface area, surface enclosed volume, surface electrostatic potential and solvation free energy. Extensive numerical experiments and comparison with an established surface model indicate that the proposed high-order fractional PDEs are robust, stable and efficient for biomolecular surface generation.

[Reliability and validity of depression scales of Chinese version: a systematic review].

PubMed

Sun, X Y; Li, Y X; Yu, C Q; Li, L M

2017-01-10

Objective: Through systematically reviewing the reliability and validity of depression scales of Chinese version in adults in China to evaluate the psychometric properties of depression scales for different groups. Methods: Eligible studies published before 6 May 2016 were retrieved from the following database: CNKI, Wanfang, PubMed and Embase. The HSROC model of the diagnostic test accuracy (DTA) for Meta-analysis was used to calculate the pooled sensitivity and specificity of the PHQ-9. Results: A total of 44 papers evaluating the performance of depression scales were included. Results showed that the reliability and validity of the common depression scales were eligible, including the Beck depression inventory (BDI), the Hamilton depression scale (HAMD), the center epidemiological studies depression scale (CES-D), the patient health questionnaire (PHQ) and the Geriatric depression scale (GDS). The Cronbach' s coefficient of most tools were larger than 0.8, while the test-retest reliability and split-half reliability were larger than 0.7, indicating good internal consistency and stability. The criterion validity, convergent validity, discrimination validity and screening validity were acceptable though different cut-off points were recommended by different studies. The pooled sensitivity of the 11 studies evaluating PHQ-9 was 0.88 (95 %CI : 0.85-0.91) while the pooled specificity was 0.89 (95 %CI : 0.82-0.94), which demonstrated the applicability of PHQ-9 in screening depression. Conclusion: The reliability and validity of different depression scales of Chinese version are acceptable. The characteristics of different tools and study population should be taken into consideration when choosing a specific scale.

Dopaminergic modulation of multi-muscle synergies in postural tasks performed by patients with Parkinson’s disease

PubMed Central

Falaki, Ali; Huang, Xuemei; Lewis, Mechelle M.; Latash, Mark L.

2017-01-01

Background Postural instability is one of most disabling motor symptoms in Parkinson’s disease. Indices of multi-muscle synergies are new measurements of postural stability. Objectives We explored the effects of dopamine-replacement drugs on multi-muscle synergies stabilizing center of pressure coordinate and their adjustments prior to a self-triggered perturbation in patients with Parkinson’s disease. We hypothesized that both synergy indices and synergy adjustments would be improved on dopaminergic drugs. Methods Patients at Hoehn-Yahr stages II and III performed whole-body tasks both off- and on-drugs while standing. Muscle modes were identified as factors in the muscle activation space. Synergy indices stabilizing center of pressure in the anterior-posterior direction were quantified in the muscle mode space during a load-release task. Results Dopamine-replacement drugs led to more consistent organization of muscles in stable groups (muscle modes). On-drugs patients showed larger indices of synergies and anticipatory synergy adjustments. In contrast, no medication effects were seen on anticipatory postural adjustments or other performance indices. Conclusions Dopamine-replacement drugs lead to significant changes in characteristics of multi-muscle synergies in Parkinson’s disease. Studies of synergies may provide a biomarker sensitive to problems with postural stability and agility and to efficacy of dopamine-replacement therapy. PMID:28110044

Transonic airfoil analysis and design in nonuniform flow

NASA Technical Reports Server (NTRS)

Chang, J. F.; Lan, C. E.

1986-01-01

A nonuniform transonic airfoil code is developed for applications in analysis, inverse design and direct optimization involving an airfoil immersed in propfan slipstream. Problems concerning the numerical stability, convergence, divergence and solution oscillations are discussed. The code is validated by comparing with some known results in incompressible flow. A parametric investigation indicates that the airfoil lift-drag ratio can be increased by decreasing the thickness ratio. A better performance can be achieved if the airfoil is located below the slipstream center. Airfoil characteristics designed by the inverse method and a direct optimization are compared. The airfoil designed with the method of direct optimization exhibits better characteristics and achieves a gain of 22 percent in lift-drag ratio with a reduction of 4 percent in thickness.

Validation and Reliability of the Portuguese Version of the Michigan Neuropathy Screening Instrument.

PubMed

Barbosa, Margarida; Saavedra, Ana; Severo, Milton; Maier, Christoph; Carvalho, Davide

2017-04-01

Diabetic peripheral neuropathy is very common in the diabetic population. Early screening for foot pathology is of the utmost importance. The Michigan Neuropathy Screening Instrument (MNSI) is an easy, brief, and noninvasive screening tool. The aim of this study was to validate the semantics and characteristics of both sections of the Portuguese translation of the MNSI for Portuguese diabetic patients. A cross-sectional study was performed on 87 type 1 and 2 diabetic patients at our outpatient endocrinology department. The final sample was composed of 76 patients. Nerve conduction studies were requested, but only a subsample of 42 patients agreed to participate in them. The scale was internally consistent (Cronbach's alpha > 0.70 in section A, or a clinical history questionnaire and a physical examination [section B]), and the scores of both sections were positively correlated (r = 0.70; P < 0.001). With regard to stability, MNSI scores between test/retest showed high stability (intraclass correlation coefficient = 0.91). The receiver-operating characteristic (ROC) demonstrated its validity, with ROC curve values for section A, section B, and sections A + B of 0.913, 0.798, and 0.906 respectively. Considering a cut off of ≥ 3 in section A and of ≥ 2 in section B, we obtained a sensitivity of 100% and 86%; a specificity of 64% and 61%; a positive predictive value of 80% and 73%; and a negative predictive value of 100% and 79%, respectively. The Portuguese MNSI is a reliable and valid tool for screening diabetic neuropathy. © 2016 World Institute of Pain.

Validation of the Combined Comorbidity Index of Charlson and Elixhauser to Predict 30-Day Mortality Across ICD-9 and ICD-10.

PubMed

Simard, Marc; Sirois, Caroline; Candas, Bernard

2018-05-01

To validate and compare performance of an International Classification of Diseases, tenth revision (ICD-10) version of a combined comorbidity index merging conditions of Charlson and Elixhauser measures against individual measures in the prediction of 30-day mortality. To select a weight derivation method providing optimal performance across ICD-9 and ICD-10 coding systems. Using 2 adult population-based cohorts of patients with hospital admissions in ICD-9 (2005, n=337,367) and ICD-10 (2011, n=348,820), we validated a combined comorbidity index by predicting 30-day mortality with logistic regression. To appreciate performance of the Combined index and both individual measures, factors impacting indices performance such as population characteristics and weight derivation methods were accounted for. We applied 3 scoring methods (Van Walraven, Schneeweiss, and Charlson) and determined which provides best predictive values. Combined index [c-statistics: 0.853 (95% confidence interval: CI, 0.848-0.856)] performed better than original Charlson [0.841 (95% CI, 0.835-0.844)] or Elixhauser [0.841 (95% CI, 0.837-0.844)] measures on ICD-10 cohort. All weight derivation methods provided close high discrimination results for the Combined index (Van Walraven: 0.852, Schneeweiss: 0.851, Charlson: 0.849). Results were consistent across both coding systems. The Combined index remains valid with both ICD-9 and ICD-10 coding systems and the 3 weight derivation methods evaluated provided consistent high performance across those coding systems.

Validation of the Persian version of the Daily Spiritual Experiences Scale (DSES) in Pregnant Women: A Proper Tool to Assess Spirituality Related to Mental Health.

PubMed

Saffari, Mohsen; Amini, Hossein; Sheykh-Oliya, Zarindokht; Pakpour, Amir H; Koenig, Harold G

2017-12-01

Assessing spirituality in healthy pregnant women may lead to supportive interventions that will improve their care. A psychometrically valid measure such as the Daily Spiritual Experiences Scale (DSES) may be helpful in this regard. The current study sought to adapt a Persian version of DSES for use in pregnancy. A total of 377 pregnant women were recruited from three general hospitals located in Tehran, Iran. Administered scales were the DSES, Duke University Religion Index, Santa Clara Strength of Religious Faith scale, and Depression Anxiety Stress Scale, as well as demographic measures. Reliability of the DSES was tested using Cronbach's alpha for internal consistency and the intraclass correlation coefficient (ICC) for test-retest stability. Scale validity was assessed by criterion-related tests, known-groups comparison, and exploratory factor analysis. Participant's mean age was 27.7 (4.1), and most were nulliparous (70%). The correlation coefficient between individual items on the scale and the total score was greater than 0.30 in most cases. Cronbach's alpha for the scale was 0.90. The ICC for 2-week test-retest reliability was high (0.86). Relationships between similar and dissimilar scales indicated acceptable convergent and divergent validity. The factor structure of the scale indicated a single factor that explained 59% of the variance. The DSES was found to be a reliable and valid measure of spirituality in pregnant Iranian women. This scale may be used to examine the relationship between spirituality and health outcomes, research that may lead to supportive interventions in this population.

Radiation Attenuation and Stability of ClearView Radiation Shielding TM-A Transparent Liquid High Radiation Shield.

PubMed

Bakshi, Jayeesh

2018-04-01

Radiation exposure is a limiting factor to work in sensitive environments seen in nuclear power and test reactors, medical isotope production facilities, spent fuel handling, etc. The established choice for high radiation shielding is lead (Pb), which is toxic, heavy, and abidance by RoHS. Concrete, leaded (Pb) bricks are used as construction materials in nuclear facilities, vaults, and hot cells for radioisotope production. Existing transparent shielding such as leaded glass provides minimal shielding attenuation in radiotherapy procedures, which in some cases is not sufficient. To make working in radioactive environments more practicable while resolving the lead (Pb) issue, a transparent, lightweight, liquid, and lead-free high radiation shield-ClearView Radiation Shielding-(Radium Incorporated, 463 Dinwiddie Ave, Waynesboro, VA). was developed. This paper presents the motivation for developing ClearView, characterization of certain aspects of its use and performance, and its specific attenuation testing. Gamma attenuation testing was done using a 1.11 × 10 Bq Co source and ANSI/HPS-N 13.11 standard. Transparency with increasing thickness, time stability of liquid state, measurements of physical properties, and performance in freezing temperatures are reported. This paper also presents a comparison of ClearView with existing radiation shields. Excerpts from LaSalle nuclear power plant are included, giving additional validation. Results demonstrated and strengthened the expected performance of ClearView as a radiation shield. Due to the proprietary nature of the work, some information is withheld.

Calculated performance, stability and maneuverability of high-speed tilting-prop-rotor aircraft

NASA Technical Reports Server (NTRS)

Johnson, Wayne; Lau, Benton H.; Bowles, Jeffrey V.

1986-01-01

The feasibility of operating tilting-prop-rotor aircraft at high speeds is examined by calculating the performance, stability, and maneuverability of representative configurations. The rotor performance is examined in high-speed cruise and in hover. The whirl-flutter stability of the coupled-wing and rotor motion is calculated in the cruise mode. Maneuverability is examined in terms of the rotor-thrust limit during turns in helicopter configuration. Rotor airfoils, rotor-hub configuration, wing airfoil, and airframe structural weights representing demonstrated advance technology are discussed. Key rotor and airframe parameters are optimized for high-speed performance and stability. The basic aircraft-design parameters are optimized for minimum gross weight. To provide a focus for the calculations, two high-speed tilt-rotor aircraft are considered: a 46-passenger, civil transport and an air-combat/escort fighter, both with design speeds of about 400 knots. It is concluded that such high-speed tilt-rotor aircraft are quite practical.

Ketamine and norketamine stability in whole blood at ambient and 4°C conditions.

PubMed

Tran, Benjamin Duy; Moorthy, Ganesh S; Zuppa, Athena F

2018-03-01

A study was implemented to describe the pharmacokinetics (PK) of ketamine (K) and its metabolite norketamine (NK) in critically ill adults. Conducting studies in these subjects is hindered by the immediate need to process and freeze samples obtained in a busy intensive care setting. The ability to store unprocessed samples at room temperature for an extended time period would overcome this barrier. Stability and blood to plasma partitioning of K and NK were investigated in whole blood for up to 120 h at room temperature and 4°C. Whole blood was spiked with K and NK (1000 ng/mL each). Blood samples were aliquoted at different time points (0-120 h), extracted and analyzed using a validated high-performance liquid chromatography tandem mass spectrometry assay. The study demonstrated the stability of both K and NK in whole blood up to 120 h. These in vitro studies suggest that the concentrations of K and NK measured in the PK samples are reliable. The established stability results were successfully employed to investigate K and NK pharmacology studies in critically ill adults. Copyright © 2017 John Wiley & Sons, Ltd.

Integrated Resilient Aircraft Control Project Full Scale Flight Validation

NASA Technical Reports Server (NTRS)

Bosworth, John T.

2009-01-01

Objective: Provide validation of adaptive control law concepts through full scale flight evaluation. Technical Approach: a) Engage failure mode - destabilizing or frozen surface. b) Perform formation flight and air-to-air tracking tasks. Evaluate adaptive algorithm: a) Stability metrics. b) Model following metrics. Full scale flight testing provides an ability to validate different adaptive flight control approaches. Full scale flight testing adds credence to NASA's research efforts. A sustained research effort is required to remove the road blocks and provide adaptive control as a viable design solution for increased aircraft resilience.

The stability and validity of automated vocal analysis in preverbal preschoolers with autism spectrum disorder.

PubMed

Woynaroski, Tiffany; Oller, D Kimbrough; Keceli-Kaysili, Bahar; Xu, Dongxin; Richards, Jeffrey A; Gilkerson, Jill; Gray, Sharmistha; Yoder, Paul

2017-03-01

Theory and research suggest that vocal development predicts "useful speech" in preschoolers with autism spectrum disorder (ASD), but conventional methods for measurement of vocal development are costly and time consuming. This longitudinal correlational study examines the reliability and validity of several automated indices of vocalization development relative to an index derived from human coded, conventional communication samples in a sample of preverbal preschoolers with ASD. Automated indices of vocal development were derived using software that is presently "in development" and/or only available for research purposes and using commercially available Language ENvironment Analysis (LENA) software. Indices of vocal development that could be derived using the software available for research purposes: (a) were highly stable with a single day-long audio recording, (b) predicted future spoken vocabulary to a degree that was nonsignificantly different from the index derived from conventional communication samples, and (c) continued to predict future spoken vocabulary even after controlling for concurrent vocabulary in our sample. The score derived from standard LENA software was similarly stable, but was not significantly correlated with future spoken vocabulary. Findings suggest that automated vocal analysis is a valid and reliable alternative to time intensive and expensive conventional communication samples for measurement of vocal development of preverbal preschoolers with ASD in research and clinical practice. Autism Res 2017, 10: 508-519. © 2016 International Society for Autism Research, Wiley Periodicals, Inc. © 2016 International Society for Autism Research, Wiley Periodicals, Inc.

Stability of extemporaneously compounded dexamethasone in glass and plastic bottles and plastic syringes.

PubMed

Ensom, Mary H H; Décarie, Diane

2014-07-01

Dexamethasone is widely used to treat rheumatic and endocrine disorders and chemotherapy-induced nausea and vomiting. A palatable, alcohol-free liquid formulation, with a suitable concentration to allow reasonable administration volume, is available only via extemporaneous compounding. To evaluate the stability of dexamethasone suspensions in commercially available vehicles (Oral Mix and Oral Mix SF) in various types of containers after storage at 25°C and 4°C for up to 91 days. Dexamethasone suspensions (1 mg/mL) were prepared in Oral Mix and Oral Mix SF and then transferred to amber glass and plastic prescription bottles and plastic oral syringes. Suspensions in all 3 types of containers were stored at 25°C; suspensions in glass and plastic bottles were also stored at 4°C. Samples were collected weekly from each container up to 28 days and then every 2 weeks up to 91 days. The samples were analyzed by a validated, stability-indicating high-performance liquid chromatography - ultraviolet detection method. A suspension was considered stable if it maintained at least 90% of its initial dexamethasone concentration. Changes in colour, taste, odour, precipitation (and ease of resuspension), and pH were used to assess physical compatibility. All suspensions maintained at least 96% of the original concentration for up to 91 days with storage at 25°C or at 4°C. No notable changes in colour, taste, odour, precipitation, or pH were observed over the 91-day period. Dexamethasone suspensions (1 mg/mL) in Oral Mix and Oral Mix SF, stored in amber glass or plastic bottles or plastic syringes at 25°C or in amber glass or plastic bottles at 4°C can be expected to remain stable for up to 91 days.

Long-Term Stability of Tramadol and Ketamine Solutions for Patient-Controlled Analgesia Delivery

PubMed Central

Gu, Junfeng; Qin, Wengang; Chen, Fuchao; Xia, Zhongyuan

2015-01-01

Background Subanesthetic doses of ketamine as an adjuvant to tramadol in patient-controlled analgesia (PCA) for postoperative pain have been shown to improve the quality of analgesia. However, there are no such commercially available drug mixtures, and the stability of the combination has rarely been assessed. Material/Methods Admixtures were assessed for periods of up to 14 days at 4°C and 25°C. Three different mixtures of tramadol and ketamine (tramadol 5.0 mg/mL + ketamine 0.5 mg/mL, tramadol 5.0 mg/mL + ketamine 1.0 mg/mL, and tramadol 5.0 mg/mL + ketamine 2.0 mg/mL) were prepared in polyolefin bags by combining these 2 drugs with 0.9% sodium chloride (normal saline [NS]). The chemical stability of the admixtures was evaluated by a validated high-performance liquid chromatography (HPLC) method and by measurement of pH values. Solution appearance and color were assessed by observing the samples against black and white backgrounds. Solutions were considered stable if they maintained 90% of the initial concentration of each drug. Results The percentages of initial concentration of tramadol and ketamine in the various solutions remained above 98% when stored at 4°C or 25°C over the testing period. No changes in color or turbidity were observed in any of the prepared solutions. Throughout this period, pH values remained stable. Conclusions The results indicate that the drug mixtures of tramadol with ketamine in NS for PCA delivery systems were stable for 14 days when stored in polyolefin bags at 4°C or 25°C. PMID:26306476

Performance, Stability, and Plume Characterization of the HERMeS Thruster with Boron Nitride Silica Composite Discharge Channel

NASA Technical Reports Server (NTRS)

Kamhawi, Hani; Huang, Wensheng; Gilland, James H.; Haag, Thomas W.; Mackey, Jonathan; Yim, John; Pinero, Luis; Williams, George; Peterson, Peter; Herman, Daniel

2017-01-01

NASA's Hall Effect Rocket with Magnetic Shielding (HERMeS) 12.5kW Technology Demonstration Unit-3 (TDU-3) has been the subject of extensive technology maturation in preparation for flight system development. Detailed performance, stability, and plume characterization tests of the thruster were performed at NASA GRC's Vacuum Facility 5 (VF-5). The TDU-3 thruster implements a magnetic topology that is identical to TDU-1. The TDU-3 boron nitride silica composite discharge channel material is different than the TDU-1 heritage boron nitride discharge channel material. Performance and stability characterization of the TDU-3 thruster was performed at discharge voltages between 300V and 600V and at discharge currents between 5A and 21.8A. The thruster performance and stability were assessed for varying magnetic field strength, cathode flow fractions between 5% and 9%, varying harness inductance, and for reverse magnet polarity. Performance characterization test results indicate that the TDU-3 thruster performance is in family with the TDU-1 levels. TDU-3's thrust efficiency of 65% and specific impulse of 2,800sec at 600V and 12.5kW exceed performance levels of SOA Hall thrusters. Thruster stability regimes were characterized with respect to the thruster discharge current oscillations (discharge current peak-to-peak and root mean square magnitudes), discharge current waveform power spectral density analysis, and maps of the current-voltage-magnetic field. Stability characterization test results indicate a stability profile similar to TDU-1. Finally, comparison of the TDU-1 and TDU-3 plume profiles found that there were negligible differences in the plasma plume characteristics between the TDU with heritage boron nitride versus the boron nitride silica composite discharge channel.

Validation of a new modal performance measure for flexible controllers design

DOE Office of Scientific and Technical Information (OSTI.GOV)

Simo, J.B.; Tahan, S.A.; Kamwa, I.

1996-05-01

A new modal performance measure for power system stabilizer (PSS) optimization is proposed in this paper. The new method is based on modifying the square envelopes of oscillating modes, in order to take into account their damping ratios while minimizing the performance index. This criteria is applied to flexible controllers optimal design, on a multi-input-multi-output (MIMO) reduced-order model of a prototype power system. The multivariable model includes four generators, each having one input and one output. Linear time-response simulation and transient stability analysis with a nonlinear package confirm the superiority of the proposed criteria and illustrate its effectiveness in decentralizedmore » control.« less

AOAC Official MethodSM Matrix Extension Validation Study of Assurance GDSTM for the Detection of Salmonella in Selected Spices.

PubMed

Feldsine, Philip; Kaur, Mandeep; Shah, Khyati; Immerman, Amy; Jucker, Markus; Lienau, Andrew

2015-01-01

Assurance GDSTM for Salmonella Tq has been validated according to the AOAC INTERNATIONAL Methods Committee Guidelines for Validation of Microbiological Methods for Food and Environmental Surfaces for the detection of selected foods and environmental surfaces (Official Method of AnalysisSM 2009.03, Performance Tested MethodSM No. 050602). The method also completed AFNOR validation (following the ISO 16140 standard) compared to the reference method EN ISO 6579. For AFNOR, GDS was given a scope covering all human food, animal feed stuff, and environmental surfaces (Certificate No. TRA02/12-01/09). Results showed that Assurance GDS for Salmonella (GDS) has high sensitivity and is equivalent to the reference culture methods for the detection of motile and non-motile Salmonella. As part of the aforementioned validations, inclusivity and exclusivity studies, stability, and ruggedness studies were also conducted. Assurance GDS has 100% inclusivity and exclusivity among the 100 Salmonella serovars and 35 non-Salmonella organisms analyzed. To add to the scope of the Assurance GDS for Salmonella method, a matrix extension study was conducted, following the AOAC guidelines, to validate the application of the method for selected spices, specifically curry powder, cumin powder, and chili powder, for the detection of Salmonella.

An appraisal of the enzyme stability-activity trade-off.

PubMed

Miller, Scott R

2017-07-01

A longstanding idea in evolutionary physiology is that an enzyme cannot jointly optimize performance at both high and low temperatures due to a trade-off between stability and activity. Although a stability-activity trade-off has been observed for well-characterized examples, such a trade-off is not imposed by any physical chemical constraint. To better understand the pervasiveness of this trade-off, I investigated the stability-activity relationship for comparative biochemical studies of purified orthologous enzymes identified by a literature search. The nature of this relationship varied greatly among studies. Notably, studies of enzymes with low mean synonymous nucleotide sequence divergence were less likely to exhibit the predicted negative correlation between stability and activity. Similarly, a survey of directed evolution investigations of the stability-activity relationship indicated that these traits are often uncoupled among nearly identical yet phenotypically divergent enzymes. This suggests that the presumptive trade-off often reported for investigations of enzymes with high mean sequence divergence may in some cases instead be a consequence of the degeneration over time of enzyme function in unselected environments, rather than a direct effect of thermal adaptation. The results caution against the general assertion of a stability-activity trade-off during enzyme adaptation. © 2017 The Author(s). Evolution © 2017 The Society for the Study of Evolution.

Atmospheric turbulence affects wind turbine nacelle transferfunctions

DOE Office of Scientific and Technical Information (OSTI.GOV)

St. Martin, Clara M.; Lundquist, Julie K.; Clifton, Andrew

Despite their potential as a valuable source of individual turbine power performance and turbine array energy production optimization information, nacelle-mounted anemometers have often been neglected because complex flows around the blades and nacelle interfere with their measurements. This work quantitatively explores the accuracy of and potential corrections to nacelle anemometer measurements to determine the degree to which they may be useful when corrected for these complex flows, particularly for calculating annual energy production (AEP) in the absence of other meteorological data. Using upwind meteorological tower measurements along with nacelle-based measurements from a General Electric (GE) 1.5sle model, we calculate empiricalmore » nacelle transfer functions (NTFs) and explore how they are impacted by different atmospheric and turbulence parameters. This work provides guidelines for the use of NTFs for deriving useful wind measurements from nacelle-mounted anemometers. Corrections to the nacelle anemometer wind speed measurements can be made with NTFs and used to calculate an AEP that comes within 1 % of an AEP calculated with upwind measurements. We also calculate unique NTFs for different atmospheric conditions defined by temperature stratification as well as turbulence intensity, turbulence kinetic energy, and wind shear. During periods of low stability as defined by the Bulk Richardson number ( RB), the nacelle-mounted anemometer underestimates the upwind wind speed more than during periods of high stability at some wind speed bins below rated speed, leading to a more steep NTF during periods of low stability. Similarly, during periods of high turbulence, the nacelle-mounted anemometer underestimates the upwind wind speed more than during periods of low turbulence at most wind bins between cut-in and rated wind speed. Based on these results, we suggest different NTFs be calculated for different regimes of atmospheric stability and turbulence for power performance validation purposes.« less

Atmospheric turbulence affects wind turbine nacelle transferfunctions

DOE PAGES

St. Martin, Clara M.; Lundquist, Julie K.; Clifton, Andrew; ...

2017-06-02

Despite their potential as a valuable source of individual turbine power performance and turbine array energy production optimization information, nacelle-mounted anemometers have often been neglected because complex flows around the blades and nacelle interfere with their measurements. This work quantitatively explores the accuracy of and potential corrections to nacelle anemometer measurements to determine the degree to which they may be useful when corrected for these complex flows, particularly for calculating annual energy production (AEP) in the absence of other meteorological data. Using upwind meteorological tower measurements along with nacelle-based measurements from a General Electric (GE) 1.5sle model, we calculate empiricalmore » nacelle transfer functions (NTFs) and explore how they are impacted by different atmospheric and turbulence parameters. This work provides guidelines for the use of NTFs for deriving useful wind measurements from nacelle-mounted anemometers. Corrections to the nacelle anemometer wind speed measurements can be made with NTFs and used to calculate an AEP that comes within 1 % of an AEP calculated with upwind measurements. We also calculate unique NTFs for different atmospheric conditions defined by temperature stratification as well as turbulence intensity, turbulence kinetic energy, and wind shear. During periods of low stability as defined by the Bulk Richardson number ( RB), the nacelle-mounted anemometer underestimates the upwind wind speed more than during periods of high stability at some wind speed bins below rated speed, leading to a more steep NTF during periods of low stability. Similarly, during periods of high turbulence, the nacelle-mounted anemometer underestimates the upwind wind speed more than during periods of low turbulence at most wind bins between cut-in and rated wind speed. Based on these results, we suggest different NTFs be calculated for different regimes of atmospheric stability and turbulence for power performance validation purposes.« less

Continuous Calibration Improvement in Solar Reflective Bands: Landsat 5 Through Landsat 8

NASA Technical Reports Server (NTRS)

Mishra, Nischal; Helder, Dennis; Barsi, Julia; Markham, Brian

2016-01-01

Launched in February 2013, the Operational Land Imager (OLI) on-board Landsat 8 continues to perform exceedingly well and provides high science quality data globally. Several design enhancements have been made in the OLI instrument relative to prior Landsat instruments: pushbroom imaging which provides substantially improved Signal-to-Noise Ratio (SNR), spectral bandpasses refinement to avoid atmospheric absorption features, 12 bit data resolution to provide a larger dynamic range that limits the saturation level, a set of well-designed onboard calibrators to monitor the stability of the sensor. Some of these changes such as refinements in spectral bandpasses compared to earlier Landsats and well-designed on-board calibrator have a direct impact on the improved radiometric calibration performance of the instrument from both the stability of the response and the ability to track the changes. The on-board calibrator lamps and diffusers indicate that the instrument drift is generally less than 0.1% per year across the bands. The refined bandpasses of the OLI indicate that temporal uncertainty of better than 0.5% is possible when the instrument is trended over vicarious targets such as Pseudo Invariant Calibration Sites (PICS), a level of precision that was never achieved with the earlier Landsat instruments. The stability measurements indicated by on-board calibrators and PICS agree much better compared to the earlier Landsats, which is very encouraging and bodes well for the future Landsat missions too.

CONTINUOUS CALIBRATION IMPROVEMENT: LANDSAT 5 THROUGH LANDSAT 8

PubMed Central

Mishra, Nischal; Helder, Dennis; Barsi, Julia; Markham, Brian

2018-01-01

Launched in February 2013, the Operational Land Imager (OLI) on-board Landsat 8 continues to perform exceedingly well and provides high science quality data globally. Several design enhancements have been made in the OLI instrument relative to prior Landsat instruments: pushbroom imaging which provides substantially improved Signal-to-Noise Ratio (SNR), spectral bandpasses refinement to avoid atmospheric absorption features, 12 bit data resolution to provide a larger dynamic range that limits the saturation level, a set of well-designed onboard calibrators to monitor the stability of the sensor. Some of these changes such as refinements in spectral bandpasses compared to earlier Landsats and well-designed on-board calibrator have a direct impact on the improved radiometric calibration performance of the instrument from both the stability of the response and the ability to track the changes. The on-board calibrator lamps and diffusers indicate that the instrument drift is generally less than 0.1% per year across the bands. The refined bandpasses of the OLI indicate that temporal uncertainty of better than 0.5% is possible when the instrument is trended over vicarious targets such as Pseudo Invariant Calibration Sites (PICS), a level of precision that was never achieved with the earlier Landsat instruments. The stability measurements indicated by on-board calibrators and PICS agree much better compared to the earlier Landsats, which is very encouraging and bodes well for the future Landsat missions too. PMID:29449747

Intra-session test-retest reliability of magnitude and structure of center of pressure from the Nintendo Wii Balance Board™ for a visually impaired and normally sighted population

PubMed Central

Jeter, Pamela E.; Wang, Jiangxia; Gu, Jialiang; Barry, Michael P.; Roach, Crystal; Corson, Marilyn; Yang, Liancheng; Dagnelie, Gislin

2014-01-01

Individuals with visual impairment (VI) have irreparable damage to one of the input streams contributing to postural stability. Here, we evaluated the intra-session test-retest reliability of the Wii Balance Board (WBB) for measuring Center of Pressure (COP) magnitude and structure, i.e. approximate entropy (ApEn) in fourteen legally blind participants and 21 participants with corrected-to-normal vision. Participants completed a validated balance protocol which included four sensory conditions: double-leg standing on a firm surface with eyes open (EO-firm); a firm surface with eyes closed (EC-firm); a foam surface with EO (EO-foam); and a foam surface with EC (EC-foam). Participants performed the full balance protocol twice during the session, separated by a period of 15 minutes, to determine the intraclass correlation coefficient (ICC). Absolute reliability was determined by the standard of measurement (SEM). The minimal difference (MD) was estimated to determine clinical significance for future studies. COP measures were derived from data sent by the WBB to a laptop via Bluetooth. COP scores increased with the difficulty of sensory condition indicating WBB sensitivity (all p < 0.01). ICCs in the VI group ranged from 0.73 to 0.95, indicating high to very high correlations, and the normal group showed moderate to very high ICCs (0.62–0.94). The SEM was comparable between groups regardless of between-subject variability. The reliability of the WBB makes it practical to screen for balance impairment among VI persons. PMID:25555361

Life Testing of Yb14MnSb11 for High Performance Thermoelectric Couples

NASA Technical Reports Server (NTRS)

Paik, Jong-Ah; Brandon, Erik; Caillat, Thierry; Ewell, Richard; Fleurial, Jean-Pierre

2011-01-01

The goal of this study is to verify the long term stability of Yb14MnSb11 for high performance thermoelectric (TE) couples. Three main requirements need to be satisfied to ensure the long term stability of thermoelectric couples: 1) stable thermoelectric properties, 2) stable bonding interfaces, and 3) adequate sublimation suppression. The efficiency of the couple is primarily based on the thermoelectric properties of the materials selected for the couple. Therefore, these TE properties should exhibit minimal degradation during the operating period of the thermoelectric couples. The stability of the bonding is quantified by low contact resistances of the couple interfaces. In order to ensure high efficiency, the contact resistances of the bonding interfaces should be negligible. Sublimation suppression is important because the majority of thermoelectric materials used for power generation have peak figures of merit at temperatures where sublimation rates are high. Controlling sublimation is also essential to preserve the efficiency of the couple. During the course of this research, three different life tests were performed with Yb14MnSb11 coupons. TE properties of Yb14MnSb11 exhibited no degradation after 6 months of aging at 1273K, and the electrical contact resistance between a thin metallization layer and the Yb14MnSb11 remained negligible after 1500hr aging at 1273K. A sublimation suppression layer for Yb14MnSb11 was developed and demonstrated for more than 18 months with coupon testing at 1273K. These life test data indicate that thermoelectric elements based on Yb14MnSb11 are a promising technology for use in future high performance thermoelectric power generating couples.

Modeling of autocatalytic hydrolysis of adefovir dipivoxil in solid formulations.

PubMed

Dong, Ying; Zhang, Yan; Xiang, Bingren; Deng, Haishan; Wu, Jingfang

2011-04-01

The stability and hydrolysis kinetics of a phosphate prodrug, adefovir dipivoxil, in solid formulations were studied. The stability relationship between five solid formulations was explored. An autocatalytic mechanism for hydrolysis could be proposed according to the kinetic behavior which fits the Prout-Tompkins model well. For the classical kinetic models could hardly describe and predict the hydrolysis kinetics of adefovir dipivoxil in solid formulations accurately when the temperature is high, a feedforward multilayer perceptron (MLP) neural network was constructed to model the hydrolysis kinetics. The build-in approaches in Weka, such as lazy classifiers and rule-based learners (IBk, KStar, DecisionTable and M5Rules), were used to verify the performance of MLP. The predictability of the models was evaluated by 10-fold cross-validation and an external test set. It reveals that MLP should be of general applicability proposing an alternative efficient way to model and predict autocatalytic hydrolysis kinetics for phosphate prodrugs.