Sample records for validated stability-indicating high-performance

  1. Stability-indicating assay of repaglinide in bulk and optimized nanoemulsion by validated high performance thin layer chromatography technique.

    PubMed

    Akhtar, Juber; Fareed, Sheeba; Aqil, Mohd

    2013-07-01

    A sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for analysis of repaglinide both as a bulk drug and in nanoemulsion formulation was developed and validated. The method employed TLC aluminum plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of chloroform/methanol/ammonia/glacial acetic acid (7.5:1.5:0.9:0.1, v/v/v/v). This system was found to give compact spots for repaglinide (R f value of 0.38 ± 0.02). Repaglinide was subjected to acid and alkali hydrolysis, oxidation, photodegradation and dry heat treatment. Also, the degraded products were well separated from the pure drug. Densitometric analysis of repaglinide was carried out in the absorbance mode at 240 nm. The linear regression data for the calibration plots showed good linear relationship with r (2)= 0.998 ± 0.032 in the concentration range of 50-800 ng. The method was validated for precision, accuracy as recovery, robustness and specificity. The limits of detection and quantitation were 0.023 and 0.069 ng per spot, respectively. The drug undergoes degradation under acidic and basic conditions, oxidation and dry heat treatment. All the peaks of the degraded product were resolved from the standard drug with significantly different R f values. Statistical analysis proves that the method is reproducible and selective for the estimation of the said drug. As the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating one. Moreover, the proposed HPTLC method was utilized to investigate the degradation kinetics in 1M NaOH.

  2. 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

  3. Development and validation of stability indicating method for the quantitative determination of venlafaxine hydrochloride in extended release formulation using high performance liquid chromatography

    PubMed Central

    Kaur, Jaspreet; Srinivasan, K. K.; Joseph, Alex; Gupta, Abhishek; Singh, Yogendra; Srinivas, Kona S.; Jain, Garima

    2010-01-01

    Objective: Venlafaxine,hydrochloride is a structurally novel phenethyl bicyclic antidepressant, and is usually categorized as a serotonin–norepinephrine reuptake inhibitor (SNRI) but it has been referred to as a serotonin–norepinephrine–dopamine reuptake inhibitor. It inhibits the reuptake of dopamine. Venlafaxine HCL is widely prescribed in the form of sustained release formulations. In the current article we are reporting the development and validation of a fast and simple stability indicating, isocratic high performance liquid chromatographic (HPLC) method for the determination of venlafaxine hydrochloride in sustained release formulations. Materials and Methods: The quantitative determination of venlafaxine hydrochloride was performed on a Kromasil C18 analytical column (250 × 4.6 mm i.d., 5 μm particle size) with 0.01 M phosphate buffer (pH 4.5): methanol (40: 60) as a mobile phase, at a flow rate of 1.0 ml/min. For HPLC methods, UV detection was made at 225 nm. Results: During method validation, parameters such as precision, linearity, accuracy, stability, limit of quantification and detection and specificity were evaluated, which remained within acceptable limits. Conclusions: The method has been successfully applied for the quantification and dissolution profiling of Venlafaxine HCL in sustained release formulation. The method presents a simple and reliable solution for the routine quantitative analysis of Venlafaxine HCL. PMID:21814426

  4. 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.

  5. Development and validation of stability-indicating high performance liquid chromatography method to analyze gatifloxacin in bulk drug and pharmaceutical preparations.

    PubMed

    Aljuffali, Ibrahim A; Kalam, Mohd Abul; Sultana, Yasmin; Imran, Ahamad; Alshamsan, Aws

    2015-01-01

    Quantitative determination of gatifloxacin in tablets, solid lipid nanoparticles (SLNs) and eye-drops using a very simple and rapid chromatographic technique was validated and developed. Formulations were analyzed using a reverse phase SUPELCO® 516 C-18-DB, 50306-U, HPLC column (250 mm × 4.6 mm, 5 μm) and a mobile phase consisting of disodium hydrogen phosphate buffer:acetonitrile (75:25, v/v) and with orthophosphoric acid pH was adjusted to 3.3 The flow rate was 1.0 mL/min and analyte concentrations were measured using a UV-detector at 293 nm. The analyses were performed at room temperature (25 ± 2 °C). Gatifloxacin was separated in all the formulations within 2.767 min. There were linear calibration curves over a concentration range of 4.0-40 μg.mL(-1) and correlation coefficients of 0.9998 with an average recovery above 99.91%. Detection of analyte from different dosage forms at the same Rt indicates the specificity and stability of the developed method.

  6. 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.

  7. 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.

  8. Stability indicating high performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in combined dosage form

    PubMed Central

    Bageshwar, Deepak; Khanvilkar, Vineeta; Kadam, Vilasrao

    2011-01-01

    A specific, precise and stability indicating high-performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in pharmaceutical formulations was developed and validated. The method employed TLC aluminium plates precoated with silica gel 60F254 as the stationary phase. The solvent system consisted of methanol:water:ammonium acetate; 4.0:1.0:0.5 (v/v/v). This system was found to give compact and dense spots for both itopride hydrochloride (Rf value of 0.55±0.02) and pantoprazole sodium (Rf value of 0.85±0.04). Densitometric analysis of both drugs was carried out in the reflectance–absorbance mode at 289 nm. The linear regression analysis data for the calibration plots showed a good linear relationship with R2=0.9988±0.0012 in the concentration range of 100–400 ng for pantoprazole sodium. Also, the linear regression analysis data for the calibration plots showed a good linear relationship with R2=0.9990±0.0008 in the concentration range of 200–1200 ng for itopride hydrochloride. The method was validated for specificity, precision, robustness and recovery. Statistical analysis proves that the method is repeatable and selective for the estimation of both the said drugs. As the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating method. PMID:29403710

  9. Stability indicating high performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in combined dosage form.

    PubMed

    Bageshwar, Deepak; Khanvilkar, Vineeta; Kadam, Vilasrao

    2011-11-01

    A specific, precise and stability indicating high-performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in pharmaceutical formulations was developed and validated. The method employed TLC aluminium plates precoated with silica gel 60F 254 as the stationary phase. The solvent system consisted of methanol:water:ammonium acetate; 4.0:1.0:0.5 (v/v/v). This system was found to give compact and dense spots for both itopride hydrochloride ( R f value of 0.55±0.02) and pantoprazole sodium ( R f value of 0.85±0.04). Densitometric analysis of both drugs was carried out in the reflectance-absorbance mode at 289 nm. The linear regression analysis data for the calibration plots showed a good linear relationship with R 2 =0.9988±0.0012 in the concentration range of 100-400 ng for pantoprazole sodium. Also, the linear regression analysis data for the calibration plots showed a good linear relationship with R 2 =0.9990±0.0008 in the concentration range of 200-1200 ng for itopride hydrochloride. The method was validated for specificity, precision, robustness and recovery. Statistical analysis proves that the method is repeatable and selective for the estimation of both the said drugs. As the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating method.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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%).

  16. A Stability-Indicating HPLC-DAD Method for Determination of Stiripentol: Development, Validation, Kinetics, Structure Elucidation and Application to Commercial Dosage Form

    PubMed Central

    Darwish, Hany W.; Abdelhameed, Ali S.; Bakheit, Ahmed H.; Khalil, Nasr Y.; Al-Majed, Abdulrahman A.

    2014-01-01

    A rapid, simple, sensitive, and accurate isocratic reversed-phase stability-indicating high performance liquid chromatography method has been developed and validated for the determination of stiripentol and its degradation product in its bulk form and pharmaceutical dosage form. Chromatographic separation was achieved on a Symmetry C18 column and quantification was achieved using photodiode array detector (DAD). The method was validated in accordance with the ICH requirements showing specificity, linearity (r 2 = 0.9996, range of 1–25 μg/mL), precision (relative standard deviation lower than 2%), accuracy (mean recovery 100.08 ± 1.73), limits of detection and quantitation (LOD = 0.024 and LOQ = 0.081 μg/mL), and robustness. Stiripentol was subjected to various stress conditions and it has shown marked stability under alkaline hydrolytic stress conditions, thermal, oxidative, and photolytic conditions. Stiripentol degraded only under acidic conditions, forming a single degradation product which was well resolved from the pure drug with significantly different retention time values. This degradation product was characterized by 1H-NMR and 13C-NMR spectroscopy as well as ion trap mass spectrometry. The results demonstrated that the method would have a great value when applied in quality control and stability studies for stiripentol. PMID:25371844

  17. 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.

  18. Nifedipine-loaded polymeric nanocapsules: validation of a stability-indicating HPLC method to evaluate the drug entrapment efficiency and in vitro release profiles.

    PubMed

    Granada, Andréa; Tagliari, Monika Piazzon; Soldi, Valdir; Silva, Marcos António Segatto; Zanetti-Ramos, Betina Ghiel; Fernandes, Daniel; Stulzer, Hellen Karine

    2013-01-01

    A simple stability-indicating analytical method was developed and validated to quantify nifedipine in polymeric nanocapsule suspensions; an in vitro drug release study was then carried out. The analysis was performed using an RP C18 column, UV-Vis detection at 262 nm, and methanol-water (70 + 30, v/v) mobile phase at a flow rate of 1.2 mL/min. The method was validated in terms of specificity, linearity and range, LOQ, accuracy, precision, and robustness. The results obtained were within the acceptable ranges. The nanocapsules, made of poly(epsilon-caprolactone), were prepared by the solvent displacement technique and showed high entrapment efficiency. The entrapment efficiency was 97.6 and 98.2% for the nifedipine-loaded polymeric nanocapsules prepared from polyvinyl alcohol (PVA) and Pluronic F68 (PF68), respectively. The particle size and zeta potential of nanocapsules were found to be influenced by the nature of the stabilizer used. The mean diameter and zeta potential for nanocapsules with PVA and PF68 were 290.9 and 179.9 nm, and -17.7 mV and -32.7 mV, respectively. The two formulations prepared showed a drug release of up to 70% over 4 days. This behavior indicates the viability of this drug delivery system for use as a controlled-release system.

  19. 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.

  20. 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.

  1. 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).

  2. Reliability and validity of the closed kinetic chain upper extremity stability test.

    PubMed

    Lee, Dong-Rour; Kim, Laurentius Jongsoon

    2015-04-01

    [Purpose] The purpose of this study was to examine the reliability and validity of the Closed Kinetic Chain Upper Extremity Stability (CKCUES) test. [Subjects and Methods] A sample of 40 subjects (20 males, 20 females) with and without pain in the upper limbs was recruited. The subjects were tested twice, three days apart to assess the reliability of the CKCUES test. The CKCUES test was performed four times, and the average was calculated using the data of the last 3 tests. In order to test the validity of the CKCUES test, peak torque of internal/external shoulder rotation was measured using an isokinetic dynamometer, and maximum grip strength was measured using a hand dynamometer, and their Pearson correlation coefficients with the average values of the CKCUES test were calculated. [Results] The reliability of the CKCUES test was very high (ICC=0.97). The correlations between the CKCUES test and maximum grip strength (r=0.78-0.79), and the peak torque of internal/external shoulder rotation (r=0.87-0.94) were high indicating its validity. [Conclusion] The reliability and validity of the CKCUES test were high. The CKCUES test is expected to be used for clinical tests on upper limb stability at low price.

  3. 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%.

  4. Reaction time as an indicator of insufficient effort: Development and validation of an embedded performance validity parameter.

    PubMed

    Stevens, Andreas; Bahlo, Simone; Licha, Christina; Liske, Benjamin; Vossler-Thies, Elisabeth

    2016-11-30

    Subnormal performance in attention tasks may result from various sources including lack of effort. In this report, the derivation and validation of a performance validity parameter for reaction time is described, using a set of malingering-indices ("Slick-criteria"), and 3 independent samples of participants (total n =893). The Slick-criteria yield an estimate of the probability of malingering based on the presence of an external incentive, evidence from neuropsychological testing, from self-report and clinical data. In study (1) a validity parameter is derived using reaction time data of a sample, composed of inpatients with recent severe brain lesions not involved in litigation and of litigants with and without brain lesion. In study (2) the validity parameter is tested in an independent sample of litigants. In study (3) the parameter is applied to an independent sample comprising cooperative and non-cooperative testees. Logistic regression analysis led to a derived validity parameter based on median reaction time and standard deviation. It performed satisfactorily in studies (2) and (3) (study 2 sensitivity=0.94, specificity=1.00; study 3 sensitivity=0.79, specificity=0.87). The findings suggest that median reaction time and standard deviation may be used as indicators of negative response bias. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

  5. Relative performance of three stream bed stability indices as indicators of stream health.

    PubMed

    Kusnierz, Paul C; Holbrook, Christopher M

    2017-10-16

    Bed stability is an important stream habitat attribute because it affects geomorphology and biotic communities. Natural resource managers desire indices of bed stability that can be used under a wide range of geomorphic conditions, are biologically meaningful, and are easily incorporated into sampling protocols. To eliminate potential bias due to presence of instream wood and increase precision of stability values, we modified a stream bed instability index (ISI) to include measurements of bankfull depth (d bf ) and median particle diameter (D 50 ) only in riffles and increased the pebble count to decrease variability (i.e., increase precision) in D 50 . The new riffle-based instability index (RISI) was compared to two established indices: ISI and the riffle stability index (RSI). RISI and ISI were strongly associated with each other but neither was closely associated with RSI. RISI and ISI were closely associated with both a diatom- and two macrovertebrate-based stream health indices, but RSI was only weakly associated with the macroinvertebrate indices. Unexpectedly, precision of D 50 did not differ between RISI and ISI. Results suggest that RISI is a viable alternative to both ISI and RSI for evaluating bed stability in multiple stream types. With few data requirements and a simple protocol, RISI may also better conform to riffle-based sampling methods used by some water quality practitioners.

  6. Relative performance of three stream bed stability indices as indicators of stream health

    USGS Publications Warehouse

    Kusnierz, Paul C; Holbrook, Christopher

    2017-01-01

    Bed stability is an important stream habitat attribute because it affects geomorphology and biotic communities. Natural resource managers desire indices of bed stability that can be used under a wide range of geomorphic conditions, are biologically meaningful, and are easily incorporated into sampling protocols. To eliminate potential bias due to presence of instream wood and increase precision of stability values, we modified a stream bed instability index (ISI) to include measurements of bankfull depth (dbf) and median particle diameter (D50) only in riffles and increased the pebble count to decrease variability (i.e., increase precision) in D50.The new riffle-based instability index (RISI) was compared to two established indices: ISI and the riffle stability index (RSI). RISI and ISI were strongly associated with each other but neither was closely associated with RSI. RISI and ISI were closely associated with both a diatom- and two macrovertebrate-based stream health indices, but RSI was only weakly associated with the macroinvertebrate indices. Unexpectedly, precision of D50 did not differ between RISI and ISI. Results suggest that RISI is a viable alternative to both ISI and RSI for evaluating bed stability in multiple stream types. With few data requirements and a simple protocol, RISI may also better conform to riffle-based sampling methods used by some water quality practitioners.

  7. Development and validation of a novel stability-indicating HPLC method for the simultaneous assay of betamethasone-17-valerate, fusidic acid, potassium sorbate, methylparaben and propylparaben in a topical cream preparation.

    PubMed

    Byrne, Jonathan; Velasco-Torrijos, Trinidad; Reinhardt, Robert

    2014-08-05

    A novel stability-indicating reversed phase high performance liquid chromatographic (RP-HPLC) method for the simultaneous assay of betamethasone-17-valerate, fusidic acid and potassium sorbate as well as methyl- and propylparaben in a topical cream preparation has been developed. A 100mm×3.0mm ID. Ascentis Express C18 column maintained at 30°C and UV detection at 240nm were used. A gradient programme was employed at a flow-rate of 0.75ml/min. Mobile phase A comprised of an 83:17 (v/v) mixture of acetonitrile and methanol and mobile phase B of a 10g/l solution of 85% phosphoric acid in purified water. The method has been validated according to current International Conference on Harmonisation (ICH) guidelines and applied during formulation development and stability studies. The procedure has been shown to be stability-indicating for the topical cream. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. 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).

  9. 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

  10. 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.

  11. Nonlinear stability and control study of highly maneuverable high performance aircraft

    NASA Technical Reports Server (NTRS)

    Mohler, R. R.

    1993-01-01

    This project is intended to research and develop new nonlinear methodologies for the control and stability analysis of high-performance, high angle-of-attack aircraft such as HARV (F18). Past research (reported in our Phase 1, 2, and 3 progress reports) is summarized and more details of final Phase 3 research is provided. While research emphasis is on nonlinear control, other tasks such as associated model development, system identification, stability analysis, and simulation are performed in some detail as well. An overview of various models that were investigated for different purposes such as an approximate model reference for control adaptation, as well as another model for accurate rigid-body longitudinal motion is provided. Only a very cursory analysis was made relative to type 8 (flexible body dynamics). Standard nonlinear longitudinal airframe dynamics (type 7) with the available modified F18 stability derivatives, thrust vectoring, actuator dynamics, and control constraints are utilized for simulated flight evaluation of derived controller performance in all cases studied.

  12. 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.

  13. 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

  14. 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.

  15. 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

  16. 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

  17. 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

  18. 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.

  19. 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).

  20. Rotordynamic Instability Problems in High-Performance Turbomachinery

    NASA Technical Reports Server (NTRS)

    1984-01-01

    Rotordynamics and predictions on the stability of characteristics of high performance turbomachinery were discussed. Resolutions of problems on experimental validation of the forces that influence rotordynamics were emphasized. The programs to predict or measure forces and force coefficients in high-performance turbomachinery are illustrated. Data to design new machines with enhanced stability characteristics or upgrading existing machines are presented.

  1. 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.

  2. QbD-Based Development and Validation of a Stability-Indicating HPLC Method for Estimating Ketoprofen in Bulk Drug and Proniosomal Vesicular System.

    PubMed

    Yadav, Nand K; Raghuvanshi, Ashish; Sharma, Gajanand; Beg, Sarwar; Katare, Om P; Nanda, Sanju

    2016-03-01

    The current studies entail systematic quality by design (QbD)-based development of simple, precise, cost-effective and stability-indicating high-performance liquid chromatography method for estimation of ketoprofen. Analytical target profile was defined and critical analytical attributes (CAAs) were selected. Chromatographic separation was accomplished with an isocratic, reversed-phase chromatography using C-18 column, pH 6.8, phosphate buffer-methanol (50 : 50v/v) as a mobile phase at a flow rate of 1.0 mL/min and UV detection at 258 nm. Systematic optimization of chromatographic method was performed using central composite design by evaluating theoretical plates and peak tailing as the CAAs. The method was validated as per International Conference on Harmonization guidelines with parameters such as high sensitivity, specificity of the method with linearity ranging between 0.05 and 250 µg/mL, detection limit of 0.025 µg/mL and quantification limit of 0.05 µg/mL. Precision was demonstrated using relative standard deviation of 1.21%. Stress degradation studies performed using acid, base, peroxide, thermal and photolytic methods helped in identifying the degradation products in the proniosome delivery systems. The results successfully demonstrated the utility of QbD for optimizing the chromatographic conditions for developing highly sensitive liquid chromatographic method for ketoprofen. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. Stability at high performance in the MAST spherical tokamak

    NASA Astrophysics Data System (ADS)

    Buttery, R. J.; Akers, R.; Arends, E.; Conway, N. J.; Counsell, G. F.; Cunningham, G.; Gimblett, C. G.; Gryaznevich, M.; Hastie, R. J.; Hole, M. J.; Lehane, I.; Martin, R.; Patel, A.; Pinfold, T.; Sauter, O.; Taylor, D.; Turri, G.; Valovic, M.; Walsh, M. J.; Wilson, H. R.; MAST Team

    2004-09-01

    The development of reliable H-modes on MAST, together with advances in heating power and a range of high spatial resolution diagnostics, has provided a platform to enable MAST to address some of the most important issues of tokamak stability. In particular the high bgr potential of the spherical tokamak is highlighted with stable operation at bgrN ~ 5-6, bgrT ~ 16% and bgrp up to ~2. Magnetic diagnostic evaluation of the global bgr parameters is independently confirmed by kinetic profile data. Calculations indicate that the bgrN values are in the vicinity of no-wall stability limits. Studies of neoclassical tearing modes (NTMs) have been extended to explore their effects and develop avoidance strategies. Experiments have demonstrated that sawteeth play a strong role in triggering NTMs—by avoiding large sawteeth a much higher bgrN value has been reached. The significance of NTMs is confirmed, with large islands observed using the 300 point Thomson scattering diagnostic, and locking of large n = 1 modes frequently leading to disruptions, which become more rapid at low q95. The role of error fields has been explored. H-mode plasmas are also limited by edge localized modes (ELMs), with confinement degraded as the ELM frequency rises. However, in contrast to the conventional tokamak, the ELMs in high performing regimes on MAST (HIPB98Y2 ~ 1) appear to be type III in nature. Modelling using the ELITE code, which incorporates finite n corrections, identifies instability to peeling modes, consistent with a type III interpretation. It also shows considerable scope to raise pressure gradients before ballooning type modes (perhaps associated with type I ELMs) occur. The calculations show that narrow pedestals can support much stronger pressure gradients than might be expected from simple n = infin ballooning calculations. Finally sawteeth are shown to degrade confinement by ~10-15% in particular cases examined. They are observed not to remove the q = 1 surface in the cases

  10. 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.

  11. 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.

  12. 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

  13. 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

  14. 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.

  15. Validation of a French version of the Sleep Condition Indicator: a clinical screening tool for insomnia disorder according to DSM-5 criteria.

    PubMed

    Bayard, Sophie; Lebrun, Cindy; Maudarbocus, Khaalid Hassan; Schellaert, Vanessa; Joffre, Alicia; Ferrante, Esther; Le Louedec, Marie; Cournoulat, Alice; Gely-Nargeot, Marie-Christine; Luik, Annemarie I

    2017-12-01

    Insomnia disorder is frequent in the population, yet there is no French screening instrument available that is based on the updated DSM-5 criteria. We evaluated the validity and reliability of the French version of an insomnia screening instrument based on DSM-5 criteria, the Sleep Condition Indicator, in a population-based sample of adults. A total of 366 community-dwelling participants completed a face-to-face clinical interview to determine insomnia disorder against DSM-5 criteria and several questionnaires including the French Sleep Condition Indicator version. Three-hundred and twenty-nine participants completed the Sleep Condition Indicator again after 1 month. Statistical analyses were performed to determine the reliability, construct validity, divergent validity and temporal stability of the French translation of the Sleep Condition Indicator. In addition, an explanatory factor analysis was performed to assess the underlying structure. The internal consistency (α = 0.87) and temporal stability (r = 0.86, P < 0.001) of the French Sleep Condition Indicator were high. When using the previously defined cut-off value of ≤ 16, the area under the receiver operating characteristic curve was 0.93 with a sensitivity of 95% and a specificity of 75%. Additionally, good construct and divergent validity were demonstrated. The factor analyses showed a two-factor structure with a focus on sleep and daytime effects. The French version of the Sleep Condition Indicator demonstrates satisfactory psychometric properties while being a useful instrument in detecting cases of insomnia disorder, consistent with features of DSM-5, in the general population. © 2017 European Sleep Research Society.

  16. 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.

  17. 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

  18. 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.

  19. Stability Indicating Reverse Phase HPLC Method for Estimation of Rifampicin and Piperine in Pharmaceutical Dosage Form.

    PubMed

    Shah, Umang; Patel, Shraddha; Raval, Manan

    2018-01-01

    High performance liquid chromatography is an integral analytical tool in assessing drug product stability. HPLC methods should be able to separate, detect, and quantify the various drug-related degradants that can form on storage or manufacturing, plus detect any drug-related impurities that may be introduced during synthesis. A simple, economic, selective, precise, and stability-indicating HPLC method has been developed and validated for analysis of Rifampicin (RIFA) and Piperine (PIPE) in bulk drug and in the formulation. Reversed-phase chromatography was performed on a C18 column with Buffer (Potassium Dihydrogen Orthophosphate) pH 6.5 and Acetonitrile, 30:70), (%, v/v), as mobile phase at a flow rate of 1 mL min-1. The detection was performed at 341 nm and sharp peaks were obtained for RIFA and PIPE at retention time of 3.3 ± 0.01 min and 5.9 ± 0.01 min, respectively. The detection limits were found to be 2.385 ng/ml and 0.107 ng/ml and quantification limits were found to be 7.228ng/ml and 0.325ng/ml for RIFA and PIPE, respectively. The method was validated for accuracy, precision, reproducibility, specificity, robustness, and detection and quantification limits, in accordance with ICH guidelines. Stress study was performed on RIFA and PIPE and it was found that these degraded sufficiently in all applied chemical and physical conditions. Thus, the developed RP-HPLC method was found to be suitable for the determination of both the drugs in bulk as well as stability samples of capsule containing various excipients. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  20. Validation of a Stability-Indicating Method for Methylseleno-l-Cysteine (l-SeMC)

    PubMed Central

    Canady, Kristin; Cobb, Johnathan; Deardorff, Peter; Larson, Jami; White, Jonathan M.; Boring, Dan

    2016-01-01

    Methylseleno-l-cysteine (l-SeMC) is a naturally occurring amino acid analogue used as a general dietary supplement and is being explored as a chemopreventive agent. As a known dietary supplement, l-SeMC is not regulated as a pharmaceutical and there is a paucity of analytical methods available. To address the lack of methodology, a stability-indicating method was developed and validated to evaluate l-SeMC as both the bulk drug and formulated drug product (400 µg Se/capsule). The analytical approach presented is a simple, nonderivatization method that utilizes HPLC with ultraviolet detection at 220 nm. A C18 column with a volatile ion-pair agent and methanol mobile phase was used for the separation. The method accuracy was 99–100% from 0.05 to 0.15 mg/mL l-SeMC for the bulk drug, and 98–99% from 0.075 to 0.15 mg/mL l-SeMC for the drug product. Method precision was <1% for the bulk drug and was 3% for the drug product. The LOQ was 0.1 µg/mL l-SeMC or 0.002 µg l-SeMC on column. PMID:26199341

  1. 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.

  2. 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.

  3. 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

  4. 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

  5. Validation and application of a stability-indicating HPLC method for the in vitro determination of gastric and intestinal stability of venlafaxine.

    PubMed

    Asafu-Adjaye, Ebenezer B; Faustino, Patrick J; Tawakkul, Mobin A; Anderson, Lawrence W; Yu, Lawrence X; Kwon, Hyojong; Volpe, Donna A

    2007-04-11

    Gastrointestinal stability of venlafaxine was evaluated in vitro in simulated gastric (SGF) and intestinal (SIF) fluids using a stability indicating HPLC method. The method was validated using a 5 microm Ascentis C18 column (150 mm x 4.6 mm) and mobile phase consisting of 30% acetonitrile in 20 mM potassium phosphate buffer (pH 6.5) delivered isocratically at a flow rate of 1 mL/min with UV detection at 228 nm. Venlafaxine in USP simulated gastric and intestinal fluids (0.4 mg/mL) was incubated at 37 degrees C in a shaking water bath. The gastric stability study samples were assayed at 0, 15, 30 and 60 min intervals while sampling for the intestinal stability study was at 0, 1, 2 and 3 h. System suitability determinations gave R.S.D.s of 0.68, 0.5 and 3.9% for retention factor (k'), peak area and tailing factor, respectively. The method was shown to be accurate, precise, specific, and linear over the analytical range. Intra- and inter-day precision was <5.3%. Forced degradation studies of drug substance in basic media at 70 degrees C as well as in H2O2 for 1 h and ultra-violet photostability studies at 255 and 365 nm for 24 h did not produce any detectable degradation products. Forced degradation studies of drug substance in acidic media at 70 degrees C for 1 h produced the dehydro-venlafaxine degradant. Venlafaxine was stable in SGF (pH approximately 1.2) for the 1-h incubation period and in SIF (pH 6.8) up to 3 h with <1.5% relative difference (RD) between the amount of drug added and that found for all time points. This stability experiment in simulated gastric and intestinal fluids suggests that drug loss in the gastrointestinal tract takes place by membrane permeation rather than a degradation process.

  6. Stress Degradation Studies on Varenicline Tartrate and Development of a Validated Stability-Indicating HPLC Method

    PubMed Central

    Pujeri, Sudhakar S.; Khader, Addagadde M. A.; Seetharamappa, Jaldappagari

    2012-01-01

    A simple, rapid and stability-indicating reversed-phase liquid chromatographic method was developed for the assay of varenicline tartrate (VRT) in the presence of its degradation products generated from forced decomposition studies. The HPLC separation was achieved on a C18 Inertsil column (250 mm × 4.6 mm i.d. particle size is 5 μm) employing a mobile phase consisting of ammonium acetate buffer containing trifluoroacetic acid (0.02M; pH 4) and acetonitrile in gradient program mode with a flow rate of 1.0 mL min−1. The UV detector was operated at 237 nm while column temperature was maintained at 40 °C. The developed method was validated as per ICH guidelines with respect to specificity, linearity, precision, accuracy, robustness and limit of quantification. The method was found to be simple, specific, precise and accurate. Selectivity of the proposed method was validated by subjecting the stock solution of VRT to acidic, basic, photolysis, oxidative and thermal degradation. The calibration curve was found to be linear in the concentration range of 0.1–192 μg mL−1 (R2 = 0.9994). The peaks of degradation products did not interfere with that of pure VRT. The utility of the developed method was examined by analyzing the tablets containing VRT. The results of analysis were subjected to statistical analysis. PMID:22396908

  7. Validation of a Stability-Indicating Method for Methylseleno-L-Cysteine (L-SeMC).

    PubMed

    Canady, Kristin; Cobb, Johnathan; Deardorff, Peter; Larson, Jami; White, Jonathan M; Boring, Dan

    2016-01-01

    Methylseleno-L-cysteine (L-SeMC) is a naturally occurring amino acid analogue used as a general dietary supplement and is being explored as a chemopreventive agent. As a known dietary supplement, L-SeMC is not regulated as a pharmaceutical and there is a paucity of analytical methods available. To address the lack of methodology, a stability-indicating method was developed and validated to evaluate L-SeMC as both the bulk drug and formulated drug product (400 µg Se/capsule). The analytical approach presented is a simple, nonderivatization method that utilizes HPLC with ultraviolet detection at 220 nm. A C18 column with a volatile ion-pair agent and methanol mobile phase was used for the separation. The method accuracy was 99-100% from 0.05 to 0.15 mg/mL L-SeMC for the bulk drug, and 98-99% from 0.075 to 0.15 mg/mL L-SeMC for the drug product. Method precision was <1% for the bulk drug and was 3% for the drug product. The LOQ was 0.1 µg/mL L-SeMC or 0.002 µg L-SeMC on column. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  8. Determination of aliskiren in tablet dosage forms by a validated stability-indicating RP-LC method.

    PubMed

    Wrasse-Sangoi, M; Sangoi, M S; Oliveira, P R; Secretti, L T; Rolim, C M B

    2011-02-01

    A reversed-phase liquid chromatography (RP-LC) method is validated for the determination of aliskiren in tablet dosage form. The LC method is carried out on a Waters XBridge C(18) column (150 × 4.6 mm i.d.), maintained at 25°C. The mobile phase consisted of acetonitrile:water (95:5, v/v)/phosphoric acid (25 mM, pH 3.0) (40:60, v/v), run at a flow rate of 1.0 mL/min, with photodiode array detector set at 229 nm. The chromatographic separation is obtained with aliskiren retention time of 3.68 min, and it is linear in the range of 10-300 μg/mL (r = 0.9999). The limits of detection and quantitation are 2.38 and 7.93 μg/mL, respectively. The specificity and stability-indicating capability of the method are proven through degradation studies, which also showed that there is no interference of the formulation excipients, showing that peak is free from any coeluting peak. The method showed adequate precision, with a relative standard deviation (RSD) values lower than 0.92%. Good values of accuracy were also obtained, with a mean value of 99.55%. Experimental design is used during validation to calculate method robustness. The proposed method is applied for the analysis of the tablet dosage forms, contributing to improve the quality control and to assure the therapeutic efficacy.

  9. Stability of High-Performance Pt-Based Catalysts for Oxygen Reduction Reactions.

    PubMed

    Lin, Rui; Cai, Xin; Zeng, Hao; Yu, Zhuoping

    2018-04-01

    Due to their environmental sustainability and high efficiency, proton-exchange-membrane fuel cells (PEMFCs) are expected to be an essential type of energy source for electric vehicles, energy generation, and the space industry in the coming decades. Here, the recent developments regarding shape-controlled nanostructure catalysts are reviewed, with a focus on the stability of high-performance Pt-based catalysts and related mechanisms. The catalysts, which possess great activity, are still far from meeting the requirements of their applications, due to stability issues, especially in membrane electrode assemblies (MEAs). Thus, solutions toward the comprehensive performance of Pt-based catalysts are discussed here. The research trends and related theories that can promote the application of Pt-based catalysts are also provided. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Stability of DIII-D high-performance, negative central shear discharges

    DOE PAGES

    Hanson, Jeremy M.; Berkery, John W.; Bialek, James M.; ...

    2017-03-20

    Tokamak plasma experiments on the DIII-D device demonstrate high-performance, negative central shear (NCS) equilibria with enhanced stability when the minimum safety factor q min exceeds 2, qualitatively confirming theoretical predictions of favorable stability in the NCS regime. The discharges exhibit good confinement with an L-mode enhancement factor H 89 = 2.5, and are ultimately limited by the ideal-wall external kink stability boundary as predicted by ideal MHD theory, as long as tearing mode (TM) locking events, resistive wall modes (RWMs), and internal kink modes are properly avoided or controlled. Although the discharges exhibit rotating TMs, locking events are avoided asmore » long as a threshold minimum safety factor value q min > 2 is maintained. Fast timescale magnetic feedback control ameliorates RWM activity, expanding the stable operating space and allowing access to β N values approaching the ideal-wall limit. Quickly growing and rotating instabilities consistent with internal kink mode dynamics are encountered when the ideal-wall limit is reached. The RWM events largely occur between the no- and ideal-wall pressure limits predicted by ideal MHD. However, evaluating kinetic contributions to the RWM dispersion relation results in a prediction of passive stability in this regime due to high plasma rotation. In addition, the ideal MHD stability analysis predicts that the ideal-wall limit can be further increased to β N > 4 by broadening the current profile. Furthermore, this path toward improved stability has the potential advantage of being compatible with the bootstrap-dominated equilibria envisioned for advanced tokamak (AT) fusion reactors.« less

  11. Stability of DIII-D high-performance, negative central shear discharges

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

    Hanson, Jeremy M.; Berkery, John W.; Bialek, James M.

    Tokamak plasma experiments on the DIII-D device demonstrate high-performance, negative central shear (NCS) equilibria with enhanced stability when the minimum safety factor q min exceeds 2, qualitatively confirming theoretical predictions of favorable stability in the NCS regime. The discharges exhibit good confinement with an L-mode enhancement factor H 89 = 2.5, and are ultimately limited by the ideal-wall external kink stability boundary as predicted by ideal MHD theory, as long as tearing mode (TM) locking events, resistive wall modes (RWMs), and internal kink modes are properly avoided or controlled. Although the discharges exhibit rotating TMs, locking events are avoided asmore » long as a threshold minimum safety factor value q min > 2 is maintained. Fast timescale magnetic feedback control ameliorates RWM activity, expanding the stable operating space and allowing access to β N values approaching the ideal-wall limit. Quickly growing and rotating instabilities consistent with internal kink mode dynamics are encountered when the ideal-wall limit is reached. The RWM events largely occur between the no- and ideal-wall pressure limits predicted by ideal MHD. However, evaluating kinetic contributions to the RWM dispersion relation results in a prediction of passive stability in this regime due to high plasma rotation. In addition, the ideal MHD stability analysis predicts that the ideal-wall limit can be further increased to β N > 4 by broadening the current profile. Furthermore, this path toward improved stability has the potential advantage of being compatible with the bootstrap-dominated equilibria envisioned for advanced tokamak (AT) fusion reactors.« less

  12. 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.

  13. 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.

  14. 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.

  15. 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 p

  16. Silicene Flowers: A Dual Stabilized Silicon Building Block for High-Performance Lithium Battery Anodes.

    PubMed

    Zhang, Xinghao; Qiu, Xiongying; Kong, Debin; Zhou, Lu; Li, Zihao; Li, Xianglong; Zhi, Linjie

    2017-07-25

    Nanostructuring is a transformative way to improve the structure stability of high capacity silicon for lithium batteries. Yet, the interface instability issue remains and even propagates in the existing nanostructured silicon building blocks. Here we demonstrate an intrinsically dual stabilized silicon building block, namely silicene flowers, to simultaneously address the structure and interface stability issues. These original Si building blocks as lithium battery anodes exhibit extraordinary combined performance including high gravimetric capacity (2000 mAh g -1 at 800 mA g -1 ), high volumetric capacity (1799 mAh cm -3 ), remarkable rate capability (950 mAh g -1 at 8 A g -1 ), and excellent cycling stability (1100 mA h g -1 at 2000 mA g -1 over 600 cycles). Paired with a conventional cathode, the fabricated full cells deliver extraordinarily high specific energy and energy density (543 Wh kg ca -1 and 1257 Wh L ca -1 , respectively) based on the cathode and anode, which are 152% and 239% of their commercial counterparts using graphite anodes. Coupled with a simple, cost-effective, scalable synthesis approach, this silicon building block offers a horizon for the development of high-performance batteries.

  17. Stability of DIII-D high-performance, negative central shear discharges

    NASA Astrophysics Data System (ADS)

    Hanson, J. M.; Berkery, J. W.; Bialek, J.; Clement, M.; Ferron, J. R.; Garofalo, A. M.; Holcomb, C. T.; La Haye, R. J.; Lanctot, M. J.; Luce, T. C.; Navratil, G. A.; Olofsson, K. E. J.; Strait, E. J.; Turco, F.; Turnbull, A. D.

    2017-05-01

    Tokamak plasma experiments on the DIII-D device (Luxon et al 2005 Fusion Sci. Tech. 48 807) demonstrate high-performance, negative central shear (NCS) equilibria with enhanced stability when the minimum safety factor {{q}\\text{min}} exceeds 2, qualitatively confirming theoretical predictions of favorable stability in the NCS regime. The discharges exhibit good confinement with an L-mode enhancement factor H 89  =  2.5, and are ultimately limited by the ideal-wall external kink stability boundary as predicted by ideal MHD theory, as long as tearing mode (TM) locking events, resistive wall modes (RWMs), and internal kink modes are properly avoided or controlled. Although the discharges exhibit rotating TMs, locking events are avoided as long as a threshold minimum safety factor value {{q}\\text{min}}>2 is maintained. Fast timescale magnetic feedback control ameliorates RWM activity, expanding the stable operating space and allowing access to {β\\text{N}} values approaching the ideal-wall limit. Quickly growing and rotating instabilities consistent with internal kink mode dynamics are encountered when the ideal-wall limit is reached. The RWM events largely occur between the no- and ideal-wall pressure limits predicted by ideal MHD. However, evaluating kinetic contributions to the RWM dispersion relation results in a prediction of passive stability in this regime due to high plasma rotation. In addition, the ideal MHD stability analysis predicts that the ideal-wall limit can be further increased to {β\\text{N}}>4 by broadening the current profile. This path toward improved stability has the potential advantage of being compatible with the bootstrap-dominated equilibria envisioned for advanced tokamak (AT) fusion reactors.

  18. 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.

  19. 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.

  20. 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

  1. 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.

  2. 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.

  3. Development of a Stability-Indicating Stereoselective Method for Quantification of the Enantiomer in the Drug Substance and Pharmaceutical Dosage Form of Rosuvastatin Calcium by an Enhanced Approach

    PubMed Central

    Rajendra Reddy, Gangireddy; Ravindra Reddy, Papammagari; Siva Jyothi, Polisetty

    2015-01-01

    A novel, simple, precise, and stability-indicating stereoselective method was developed and validated for the accurate quantification of the enantiomer in the drug substance and pharmaceutical dosage forms of Rosuvastatin Calcium. The method is capable of quantifying the enantiomer in the presence of other related substances. The chromatographic separation was achieved with an immobilized cellulose stationary phase (Chiralpak IB) 250 mm x 4.6 mm x 5.0 μm particle size column with a mobile phase containing a mixture of n-hexane, dichloromethane, 2-propanol, and trifluoroacetic acid in the ratio 82:10:8:0.2 (v/v/v/v). The eluted compounds were monitored at 243 nm and the run time was 18 min. Multivariate analysis and statistical tools were used to develop this highly robust method in a short span of time. The stability-indicating power of the method was established by subjecting Rosuvastatin Calcium to the stress conditions (forced degradation) of acid, base, oxidative, thermal, humidity, and photolytic degradation. Major degradation products were identified and found to be well-resolved from the enantiomer peak, 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, limit of detection and limit of quantification, precision, linearity, accuracy, and robustness. The method exhibited consistent, high-quality recoveries (100 ± 10%) with a high precision for the enantiomer. Linear regression analysis revealed an excellent correlation between the peak responses and concentrations (r2 value of 0.9977) for the enantiomer. The method is sensitive enough to quantify the enantiomer above 0.04% and detect the enantiomer above 0.015% in Rosuvastatin Calcium. The stability tests were also performed on the drug substances as per ICH norms. PMID:26839815

  4. 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.

  5. 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

  6. 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.

  7. 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…

  8. Effort, symptom validity testing, performance validity testing and traumatic brain injury.

    PubMed

    Bigler, Erin D

    2014-01-01

    To understand the neurocognitive effects of brain injury, valid neuropsychological test findings are paramount. This review examines the research on what has been referred to a symptom validity testing (SVT). Above a designated cut-score signifies a 'passing' SVT performance which is likely the best indicator of valid neuropsychological test findings. Likewise, substantially below cut-point performance that nears chance or is at chance signifies invalid test performance. Significantly below chance is the sine qua non neuropsychological indicator for malingering. However, the interpretative problems with SVT performance below the cut-point yet far above chance are substantial, as pointed out in this review. This intermediate, border-zone performance on SVT measures is where substantial interpretative challenges exist. Case studies are used to highlight the many areas where additional research is needed. Historical perspectives are reviewed along with the neurobiology of effort. Reasons why performance validity testing (PVT) may be better than the SVT term are reviewed. Advances in neuroimaging techniques may be key in better understanding the meaning of border zone SVT failure. The review demonstrates the problems with rigidity in interpretation with established cut-scores. A better understanding of how certain types of neurological, neuropsychiatric and/or even test conditions may affect SVT performance is needed.

  9. A passive microfluidic hydrogen-air fuel cell with exceptional stability and high performance.

    PubMed

    Mitrovski, Svetlana M; Nuzzo, Ralph G

    2006-03-01

    We describe an advanced microfluidic hydrogen-air fuel cell (FC) that exhibits exceptional durability and high performance, most notably yielding stable output power (>100 days) without the use of an anode-cathode separator membrane. This FC embraces an entirely passive device architecture and, unlike conventional microfluidic designs that exploit laminar hydrodynamics, no external pumps are used to sustain or localize the reagent flow fields. The devices incorporate high surface area/porous metal and metal alloy electrodes that are embedded and fully immersed in liquid electrolyte confined in the channels of a poly(dimethylsiloxane) (PDMS)-based microfluidic network. The polymeric network also serves as a self-supporting membrane through which oxygen and hydrogen are supplied to the cathode and alloy anode, respectively, by permeation. The operational stability of the device and its performance is strongly dependent on the nature of the electrolyte used (5 M H2SO4 or 2.5 M NaOH) and composition of the anode material. The latter choice is optimized to decrease the sensitivity of the system to oxygen cross-over while still maintaining high activity towards the hydrogen oxidation reaction (HOR). Three types of high surface area anodes were tested in this work. These include: high-surface area electrodeposited Pt (Pt); high-surface area electrodeposited Pd (Pd); and thin palladium adlayers supported on a "porous" Pt electrode (Pd/Pt). The FCs display their best performance in 5 M H2SO4 using the Pd/Pt anode. This exceptional stability and performance was ascribed to several factors, namely: the high permeabilities of O2, H2, and CO2 in PDMS; the inhibition of the formation of insoluble carbonate species due to the presence of a highly acidic electrolyte; and the selectivity of the Pd/Pt anode toward the HOR. The stability of the device for long-term operation was modeled using a stack of three FCs as a power supply for a portable display that otherwise uses a 3 V

  10. High-Performance AC Power Source by Applying Robust Stability Control Technology for Precision Material Machining

    NASA Astrophysics Data System (ADS)

    Chang, En-Chih

    2018-02-01

    This paper presents a high-performance AC power source by applying robust stability control technology for precision material machining (PMM). The proposed technology associates the benefits of finite-time convergent sliding function (FTCSF) and firefly optimization algorithm (FOA). The FTCSF maintains the robustness of conventional sliding mode, and simultaneously speeds up the convergence speed of the system state. Unfortunately, when a highly nonlinear loading is applied, the chatter will occur. The chatter results in high total harmonic distortion (THD) output voltage of AC power source, and even deteriorates the stability of PMM. The FOA is therefore used to remove the chatter, and the FTCSF still preserves finite system-state convergence time. By combining FTCSF with FOA, the AC power source of PMM can yield good steady-state and transient performance. Experimental results are performed in support of the proposed technology.

  11. 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).

  12. A validated stability-indicating LC method for the separation of enantiomer and potential impurities of Linezolid using polar organic mode.

    PubMed

    Satyanarayana Raju, T; Vishweshwari Kutty, O; Ganesh, V; Yadagiri Swamy, P

    2012-08-01

    Although a number of methods are available for evaluating Linezolid and its possible impurities, a common method for separation if its potential impurities, degradants and enantiomer in a single method with good efficiency remain unavailable. With the objective of developing an advanced method with shorter runtimes, a simple, precise, accurate stability-indicating LC method was developed for the determination of purity of Linezolid drug substance and drug products in bulk samples and pharmaceutical dosage forms in the presence of its impurities and degradation products. This method is capable of separating all the related substances of Linezolid along with the chiral impurity. This method can also be used for the estimation of assay of Linezolid in drug substance as well as in drug product. The method was developed using Chiralpak IA (250 mm×4.6 mm, 5 μm) column. A mixture of acetonitrile, ethanol, n-butyl amine and trifluoro acetic acid in 96:4:0.10:0.16 (v/v/v/v) ratio was used as a mobile phase. The eluted compounds were monitored at 254 nm. Linezolid was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. 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, limit of detection, limit of quantification, precision, linearity, accuracy, robustness and system suitability.

  13. 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.

  14. Performance and stability of a liquid anode high-temperature metal-air battery

    NASA Astrophysics Data System (ADS)

    Otaegui, L.; Rodriguez-Martinez, L. M.; Wang, L.; Laresgoiti, A.; Tsukamoto, H.; Han, M. H.; Tsai, C.-L.; Laresgoiti, I.; López, C. M.; Rojo, T.

    2014-02-01

    A High-Temperature Metal-Air Battery (HTMAB) that operates based on a simple redox reaction between molten metal and atmospheric oxygen at 600-1000 °C is presented. This innovative HTMAB concept combines the technology of conventional metal-air batteries with that of solid oxide fuel cells to provide a high energy density system for many applications. Electrochemical reversibility is demonstrated with 95% coulomb efficiency. Cell sealing has been identified as a key issue in order to determine the end-of-charge voltage, enhance coulomb efficiency and ensure long term stability. In this work, molten Sn is selected as anode material. Low utilization of the stored material due to precipitation of the SnO2 on the electrochemically active area limits the expected capacity, which should theoretically approach 903 mAh g-1. Nevertheless, more than 1000 charge/discharge cycles are performed during more than 1000 h at 800 °C, showing highly promising results of stability, reversibility and cyclability.

  15. 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.

  16. ESI-MSn and LC-ESI-MS studies to characterize forced degradation products of bosentan and a validated stability-indicating LC-UV method.

    PubMed

    Bansal, Gulshan; Singh, Ranjit; Saini, Balraj; Bansal, Yogita

    2013-01-01

    The present study reports the characterization of forced degradation products of bosentan and a validated stability-indicating HPLC method for the stability testing of bosentan tablets. The forced degradation was carried out under the conditions of hydrolysis, oxidation, dry heat and photolysis. The drug was found unstable in acid, alkali and oxidative media whereas stable to the hydrolysis in water, to dry heat and to photolysis. In total, six degradation products were formed in all conditions which were resolved in a single run on a C-18 column with gradient elution using ammonium acetate buffer (pH 4.5, 5.0mM), methanol and acetonitrile. Structures of all the degradation products were characterized through +ESI-MS(n) and LC-ESI-MS spectral data of bosentan as well as LC-ESI-MS spectral data of the products. The products II-VI were characterized as 6-amino-[2,2']bipyrimidinyl-4,5-diol, 6-amino-5-(2-methoxyphenoxy)-[2,2']-bipyrimidinyl-4-ol, 2-[6-amino-5-(2-methoxyphenoxy)-[2,2']-bipyrimidinyl-4-yloxy]-ethanol, 4-tert-butyl-N-[6-(1-methoxyethoxy)-5-(2-methoxyphenoxy)-[2,2']-bipyrimidinyl-4-yl]-benzenesulfonamide and 4-tert-butyl-N-[6-hydroxy-5-(2-methoxyphenoxy)-[2,2']bipyrimidinyl-4-yl]-benzenesulfonamide, respectively. The peak of the product I was found to be due to two secondary degradation products which co-eluted and were characterized as β-hydroxyethyl p-tert-butylphenylsulfonate (Ia) and 2-[2-(2-hydroxyethoxy)-phenoxy]-ethanol (Ib). These products were formed due to hydrolysis of sulfonamide and alkylaryl ether and the diaryl ether linkages as well as dehydration of the primary alcohol group. The most probable degradation mechanisms were proposed. The HPLC method was found to be stability-indicating, linear (2-100 μg ml(-1)), accurate, precise, sensitive, specific, rugged and robust for quantitation of the drug. The method was applied to the stability testing of the commercially available bosentan tablets successfully. Copyright © 2012 Elsevier B.V. All

  17. 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…

  18. Stability of extemporaneous oral ribavirin liquid preparation.

    PubMed

    Chan, John P; Tong, Henry H Y; Chow, Albert H L

    2004-01-01

    Ribavirin is an antiviral agent commonly used in Hong Kong for the treatment of severe acute respiratory syndrome. The choice of oral ribavirin therapeutic products available in the local market is currently limited to capsules. The present study investigated the chemical stability of an oral ribavirin suspension (200 mg/5mL) prepared extemporaneously from oral capsules using a sugar-free suspension formula. The suspension was subjected to stability testing at 4 deg C for up to 28 days. Employing a validated stability-indicating high-performance liquid chromatographic method, the ribavirin content of the extemporaneous preparation has been demonstrated to exhibit negligible changes throughout the storage period. No degradation product was observable in all high-peroformance liquid chromatograms, suggesting that the suspension remained chermically stable under the stated conditions.

  19. 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.

  20. Polyacrylonitrile Separator for High-Performance Aluminum Batteries with Improved Interface Stability.

    PubMed

    Elia, Giuseppe Antonio; Ducros, Jean-Baptiste; Sotta, Dane; Delhorbe, Virginie; Brun, Agnès; Marquardt, Krystan; Hahn, Robert

    2017-11-08

    Herein we report, for the first time, an overall evaluation of commercially available battery separators to be used for aluminum batteries, revealing that most of them are not stable in the highly reactive 1-ethyl-3-methylimidazolium chloride:aluminum trichloride (EMIMCl:AlCl 3 ) electrolyte conventionally employed in rechargeable aluminum batteries. Subsequently, a novel highly stable polyacrylonitrile (PAN) separator obtained by the electrospinning technique for application in high-performance aluminum batteries has been prepared. The developed PAN separator has been fully characterized in terms of morphology, thermal stability, and air permeability, revealing its suitability as a separator for battery applications. Furthermore, extremely good compatibility and improved aluminum interface stability in the highly reactive EMIMCl:AlCl 3 electrolyte were discovered. The use of the PAN separator strongly affects the aluminum dissolution/deposition process, leading to a quite homogeneous deposition compared to that of a glass fiber separator. Finally, the applicability of the PAN separator has been demonstrated in aluminum/graphite cells. The electrochemical tests evidence the full compatibility of the PAN separator in aluminum cells. Furthermore, the aluminum/graphite cells employing the PAN separator are characterized by a slightly higher delivered capacity compared to those employing glass fiber separators, confirming the superior characteristics of the PAN separator as a more reliable separator for the emerging aluminum battery technology.

  1. 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.

  2. Single-Shot Scalar-Triplet Measurements in High-Pressure Swirl-Stabilized Flames for Combustion Code Validation

    NASA Technical Reports Server (NTRS)

    Kojima, Jun; Nguyen, Quang-Viet

    2007-01-01

    In support of NASA ARMD's code validation project, we have made significant progress by providing the first quantitative single-shot multi-scalar data from a turbulent elevated-pressure (5 atm), swirl-stabilized, lean direct injection (LDI) type research burner operating on CH4-air using a spatially-resolved pulsed-laser spontaneous Raman diagnostic technique. The Raman diagnostics apparatus and data analysis that we present here were developed over the past 6 years at Glenn Research Center. From the Raman scattering data, we produce spatially-mapped probability density functions (PDFs) of the instantaneous temperature, determined using a newly developed low-resolution effective rotational bandwidth (ERB) technique. The measured 3-scalar (triplet) correlations, between temperature, CH4, and O2 concentrations, as well as their PDF s, also provide a high-level of detail into the nature and extent of the turbulent mixing process and its impact on chemical reactions in a realistic gas turbine injector flame at elevated pressures. The multi-scalar triplet data set presented here provides a good validation case for CFD combustion codes to simulate by providing both average and statistical values for the 3 measured scalars.

  3. Temporal and voltage stress stability of high performance indium-zinc-oxide thin film transistors

    NASA Astrophysics Data System (ADS)

    Song, Yang; Katsman, Alexander; Butcher, Amy L.; Paine, David C.; Zaslavsky, Alexander

    2017-10-01

    Thin film transistors (TFTs) based on transparent oxide semiconductors, such as indium zinc oxide (IZO), are of interest due to their improved characteristics compared to traditional a-Si TFTs. Previously, we reported on top-gated IZO TFTs with an in-situ formed HfO2 gate insulator and IZO active channel, showing high performance: on/off ratio of ∼107, threshold voltage VT near zero, extracted low-field mobility μ0 = 95 cm2/V·s, and near-perfect subthreshold slope at 62 mV/decade. Since device stability is essential for technological applications, in this paper we report on the temporal and voltage stress stability of IZO TFTs. Our devices exhibit a small negative VT shift as they age, consistent with an increasing carrier density resulting from an increasing oxygen vacancy concentration in the channel. Under gate bias stress, freshly annealed TFTs show a negative VT shift during negative VG gate bias stress, while aged (>1 week) TFTs show a positive VT shift during negative VG stress. This indicates two competing mechanisms, which we identify as the field-enhanced generation of oxygen vacancies and the field-assisted migration of oxygen vacancies, respectively. A simplified kinetic model of the vacancy concentration evolution in the IZO channel under electrical stress is provided.

  4. 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.

  5. 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.

  6. Development and validation of a stability-indicating RP-HPLC method for determination of atomoxetine hydrochloride in tablets.

    PubMed

    Patel, Sejal K; Patel, Natvarlal J

    2010-01-01

    This paper describes the development of a stability-indicating RP-HPLC method for the determination of atomoxetine hydrochloride (ATX) in the presence of its degradation products generated from forced decomposition studies. The drug substance was subjected to stress conditions of acid, base, oxidation, wet heat, dry heat, and photodegradation. In stability tests, the drug was susceptible to acid, base, oxidation, and dry and wet heat degradation. It was found to be stable under the photolytic conditions tested. The drug was successfully separated from the degradation products formed under stress conditions on a Phenomenex C18 column (250 x 4.6 mm id, 5 microm particle size) by using acetonitrile-methanol-0.032 M ammonium acetate (55 + 05 + 40, v/v/v) as the mobile phase at 1.0 mL/min and 40 degrees C. Photodiode array detection at 275 nm was used for quantitation after RP-HPLC over the concentration range of 0.5-5 microg/mL with a mean recovery of 100.8 +/- 0.4% for ATX. Statistical analysis demonstrated that the method is repeatable, specific, and accurate for the estimation of ATX. Because the method effectively separates the drug from its degradation products, it can be used as a stability-indicating method.

  7. Optimum design of high speed prop rotors including the coupling of performance, aeroelastic stability and structures

    NASA Technical Reports Server (NTRS)

    Chattopadhyay, Aditi; Mccarthy, Thomas R.; Madden, John F., III

    1992-01-01

    An optimization procedure is developed for the design of high speed prop-rotors to be used in civil tiltrotor applications. The goal is to couple aerodynamic performance, aeroelastic stability, and structural design requirements inside a closed-loop optimization procedure. The objective is to minimize the gross weight and maximize the propulsive efficiency in high speed cruise. Constraints are imposed on the rotor aeroelastic stability in both hover and cruise and rotor figure of merit in hover. Both structural and aerodynamic design variables are used.

  8. 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…

  9. Evaluation of a high-moisture stabilization strategy for harvested microalgae blended with herbaceous biomass: Part I—Storage performance

    DOE PAGES

    Wendt, Lynn M.; Wahlen, Bradley D.; Li, Chenlin; ...

    2017-06-01

    Here, algal biomass is becoming increasingly attractive as a feedstock for biofuel production. However, the swing in algal biomass production between summer and winter months poses a challenge for delivering predictable, constant feedstock supply to a conversion facility. Drying is one approach for stabilizing algal biomass produced in excess during high productivity summer months for utilization during low productivity months, yet drying is energy intensive and thus costly. Wet, anaerobic storage, or ensiling, is a low-cost approach that is commonly used to preserve high moisture herbaceous feedstock. The potential for microalgae stabilization without the need for drying was investigated inmore » this study by simulating ensiling, in which oxygen limitation drives anaerobic fermentation of soluble sugars to organic acids, dropping the pH and thereby stabilizing the material. Algal biomass, Scenedesmus obliquus, was blended with corn stover and stored in acidic, anaerobic conditions at 60% moisture (wet basis) to simulate wet storage by means of ensiling. Results demonstrate that algae and corn stover blends were successfully preserved in anaerobic, acidic conditions for 30 days with < 2% dry matter loss occurring during storage compared to 21% loss in aerobic, non-acidified conditions. Likewise, Scenedesmus obliquus stored alone at 80% moisture (wet basis) in acidified, anaerobic conditions for 30 days, resulted in dry matter losses of 6–14%, compared to 44% loss in neutral pH, anaerobic storage and 37% loss in a neutral pH, aerobically stored condition. Additional experiments were performed at a larger scale in which an algae and corn stover blend was subject to mechanical oxygen exclusion and a Lactobacillus acidophilus inoculum, resulting in 8% loss over 35 days and further indicating that acidic, anaerobic conditions can stabilize microalgae biomass. In summary, the stabilization of harvested algae can be achieved through anaerobic storage, securing a

  10. Evaluation of a high-moisture stabilization strategy for harvested microalgae blended with herbaceous biomass: Part I—Storage performance

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

    Wendt, Lynn M.; Wahlen, Bradley D.; Li, Chenlin

    Here, algal biomass is becoming increasingly attractive as a feedstock for biofuel production. However, the swing in algal biomass production between summer and winter months poses a challenge for delivering predictable, constant feedstock supply to a conversion facility. Drying is one approach for stabilizing algal biomass produced in excess during high productivity summer months for utilization during low productivity months, yet drying is energy intensive and thus costly. Wet, anaerobic storage, or ensiling, is a low-cost approach that is commonly used to preserve high moisture herbaceous feedstock. The potential for microalgae stabilization without the need for drying was investigated inmore » this study by simulating ensiling, in which oxygen limitation drives anaerobic fermentation of soluble sugars to organic acids, dropping the pH and thereby stabilizing the material. Algal biomass, Scenedesmus obliquus, was blended with corn stover and stored in acidic, anaerobic conditions at 60% moisture (wet basis) to simulate wet storage by means of ensiling. Results demonstrate that algae and corn stover blends were successfully preserved in anaerobic, acidic conditions for 30 days with < 2% dry matter loss occurring during storage compared to 21% loss in aerobic, non-acidified conditions. Likewise, Scenedesmus obliquus stored alone at 80% moisture (wet basis) in acidified, anaerobic conditions for 30 days, resulted in dry matter losses of 6–14%, compared to 44% loss in neutral pH, anaerobic storage and 37% loss in a neutral pH, aerobically stored condition. Additional experiments were performed at a larger scale in which an algae and corn stover blend was subject to mechanical oxygen exclusion and a Lactobacillus acidophilus inoculum, resulting in 8% loss over 35 days and further indicating that acidic, anaerobic conditions can stabilize microalgae biomass. In summary, the stabilization of harvested algae can be achieved through anaerobic storage, securing a

  11. The Development of Performance Indicators for Prison Libraries.

    ERIC Educational Resources Information Center

    Lithgow, Susan D.

    This report describes a study to investigate the improved efficiency and effectiveness of prison library provision in England and Wales, through the development and validation of relevant performance indicators to be used as part of quality assurance programs. Prison libraries perform important educational, rehabilitative, and recreational…

  12. Sensitivity of stability indices to dealerting

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

    Canavan, G.H.

    1998-03-01

    It is reported that more than 100 former or current heads of state and civilian leaders from around the world, including ex-presidents Jimmy Carter and Mikhail Gorbachev, have signed a statement that calls for removing nuclear weapons from alert status and other measures aimed at the eventual elimination of atomic arsenals--reflecting mounting support for the cause of nuclear bolition. This note uses stability analysis derived from current US and Russian analyses to study the impact of such dealerting on stability, indicating that it could be negative. Dealerting forces removes them from first and second strikes for as long as theymore » are dealerted. If they are dealerted for periods long compared to those involved in the evaluation of first strike stability, dealerting has the same effect as permanent arms reductions, it subtracts them from first and second strikes. Thus, it is conceptually a way of implementing such reductions on an accelerated scale. Dealerting strategic forces has been posited as a stabilizing step towards their abolition. Previous reports have shown that planned START reductions will reduce stability indices by about a factor of two. Dealerting would hasten those reductions. They would also raise the possibility that one side could realert faster than the other. If so, the remobilized forces could be used to damage limit, which would reduce his first strike cost and stability index. The impact of complete demobilization of SSBNs would be an order of magnitude reduction in the overall stability index, to a level set by alert ICBMs. Generally, it would be preferable to maintain any existing strategic forces at the highest level of alert to minimize this effect and to concentrate instead on decreasing their total number.« less

  13. 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).

  14. 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.

  15. 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

  16. [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.

  17. Cognitive performance and electrophysiological indices of cognitive control: a validation study of conflict adaptation.

    PubMed

    Clayson, Peter E; Larson, Michael J

    2012-05-01

    Psychiatric and neurologic disorders are associated with deficits in the postconflict recruitment of cognitive control. The primary aim of this study was to validate the relationship between cognitive functioning and indices of conflict adaptation. Event-related potentials were obtained from 89 healthy individuals who completed an Eriksen flanker task. Neuropsychological domains tested included memory, verbal fluency, and attention/executive functioning. Behavioral measures and N2 amplitudes showed significant conflict adaptation (i.e., previous-trial congruencies influenced current-trial measures). Higher scores on the attention/executive functioning and verbal fluency domains were associated with larger incongruent-trial N2 conflict adaptation; measures of cognitive functioning were not related to behavioral indices. This study provides initial validation of N2 conflict adaptation effects as cognitive function-related aspects of cognitive control. Copyright © 2012 Society for Psychophysiological Research.

  18. 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.

  19. Performance Indicators: Information in Search of a Valid and Reliable Use.

    ERIC Educational Resources Information Center

    Carrigan, Sarah D.; Hackett, E. Raymond

    1998-01-01

    Examined the usefulness of performance indicators in campus decision making at 20 institutions with Carnegie Baccalaureate II classification using hypothesis testing and case-study approaches. Performance measures most commonly cited as measures of financial viability were of limited use for specific policy development, but were most useful within…

  20. 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.

  1. 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

  2. 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.

  3. Construct validity of the individual work performance questionnaire.

    PubMed

    Koopmans, Linda; Bernaards, Claire M; Hildebrandt, Vincent H; de Vet, Henrica C W; van der Beek, Allard J

    2014-03-01

    To examine the construct validity of the Individual Work Performance Questionnaire (IWPQ). A total of 1424 Dutch workers from three occupational sectors (blue, pink, and white collar) participated in the study. First, IWPQ scores were correlated with related constructs (convergent validity). Second, differences between known groups were tested (discriminative validity). First, IWPQ scores correlated weakly to moderately with absolute and relative presenteeism, and work engagement. Second, significant differences in IWPQ scores were observed for workers differing in job satisfaction, and workers differing in health. Overall, the results indicate acceptable construct validity of the IWPQ. Researchers are provided with a reliable and valid instrument to measure individual work performance comprehensively and generically, among workers from different occupational sectors, with and without health problems.

  4. 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.

  5. 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.

  6. Invalid before impaired: an emerging paradox of embedded validity indicators.

    PubMed

    Erdodi, Laszlo A; Lichtenstein, Jonathan D

    Embedded validity indicators (EVIs) are cost-effective psychometric tools to identify non-credible response sets during neuropsychological testing. As research on EVIs expands, assessors are faced with an emerging contradiction: the range of credible impairment disappears between the 'normal' and 'invalid' range of performance. We labeled this phenomenon as the invalid-before-impaired paradox. This study was designed to explore the origin of this psychometric anomaly, subject it to empirical investigation, and generate potential solutions. Archival data were analyzed from a mixed clinical sample of 312 (M Age  = 45.2; M Education  = 13.6) patients medically referred for neuropsychological assessment. The distribution of scores on eight subtests of the third and fourth editions of Wechsler Adult Intelligence Scale (WAIS) were examined in relation to the standard normal curve and two performance validity tests (PVTs). Although WAIS subtests varied in their sensitivity to non-credible responding, they were all significant predictors of performance validity. While subtests previously identified as EVIs (Digit Span, Coding, and Symbol Search) were comparably effective at differentiating credible and non-credible response sets, their classification accuracy was driven by their base rate of low scores, requiring different cutoffs to achieve comparable specificity. Invalid performance had a global effect on WAIS scores. Genuine impairment and non-credible performance can co-exist, are often intertwined, and may be psychometrically indistinguishable. A compromise between the alpha and beta bias on PVTs based on a balanced, objective evaluation of the evidence that requires concessions from both sides is needed to maintain/restore the credibility of performance validity assessment.

  7. Validated stability-indicating HPLC method for the determination of pridinol mesylate. Kinetics study of its degradation in acid medium.

    PubMed

    Bianchini, Romina M; Castellano, Patricia M; Kaufman, Teodoro S

    2008-12-01

    The stability of pridinol mesylate (PRI) was investigated under different stress conditions, including hydrolytic, oxidative, photolytic and thermal, as recommended by the ICH guidelines. Relevant degradation was found to take place under acidic (0.1N HCl) and photolytic (visible and long-wavelength UV-light) conditions, both yielding the product resulting from water elimination (ELI), while submission to an oxidizing environment gave the N-oxidation derivative (NOX). The standards of these degradation products were synthesized and characterized by IR, (1)H and (13)C NMR spectroscopy. A simple, sensitive and specific HPLC method was developed for the quantification of PRI, ELI and NOX in bulk drug, and the conditions were optimized by means of a statistical design strategy. The separation employs a C(18) column and a 51:9:40 (v/v/v) mixture of MeOH, 2-propanol and potassium phosphate solution (50mM, pH 6.0), as mobile phase, delivered at 1.0 ml min(-1); the analytes were detected and quantified at 220 nm. The method was validated, demonstrating to be accurate and precise (repeatability and intermediate precision levels) within the corresponding linear ranges of PRI (0.1-1.5 mg ml(-1); r=0.9983, n=18) and both impurities (0.1-1.3% relative to PRI, r=0.9996 and 0.9995 for ELI and NOX, respectively, n=18). Robustness against small modifications of pH and percentage of the aqueous mobile phase was ascertained and the limits of quantification of the analytes were also determined (0.4 and 0.5 microg ml(-1); 0.04% and 0.05% relative to PRI for ELI and NOX, respectively). Peak purity indices (>0.9997), obtained with the aid of diode-array detection, and satisfactory resolution (R(s)>2.0) between PRI and its impurities established the specificity of the determination, all these results proving the stability-indicating capability of the method. The kinetics of the degradation of PRI in acid medium was also studied, determining that this is a first-order process with regards

  8. Stability Indicating HPLC Determination of Risperidone in Bulk Drug and Pharmaceutical Formulations

    PubMed Central

    Dedania, Zarna R.; Dedania, Ronak R.; Sheth, Navin R.; Patel, Jigar B.; Patel, Bhavna

    2011-01-01

    The objective of the current study was to develop a validated stability-indicating assay method (SIAM) for risperidone after subjecting it to forced decomposition under hydrolysis, oxidation, photolysis, and thermal stress conditions. The liquid chromatographic separation was achieved isocratically on a symmetry C18 column (5 μm size, 250 mm × 4.6 mm i.d.) using a mobile phase containing methanol: acetonitrile (80 : 20, v/v) at a flow rate of 1 mL/min and UV detection at 280 nm. Retention time of risperidone was found to be 3.35 ± 0.01. The method was linear over the concentration range of 10–60 μg/mL(r 2 = 0.998) with a limit of detection and quantitation of 1.79 and 5.44 μg/mL, respectively. The method has the requisite accuracy, specificity, sensitivity, and precision to assay risperidone in bulk form and pharmaceutical dosage forms. Degradation products resulting from the stress studies did not interfere with the detection of Risperidone, and the assay is thus stability indicating. PMID:22007220

  9. 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

  10. Stabilized display of coronary x-ray image sequences

    NASA Astrophysics Data System (ADS)

    Close, Robert A.; Whiting, James S.; Da, Xiaolin; Eigler, Neal L.

    2004-05-01

    Display stabilization is a technique by which a feature of interest in a cine image sequence is tracked and then shifted to remain approximately stationary on the display device. Prior simulations indicate that display stabilization with high playback rates ( 30 f/s) can significantly improve detectability of low-contrast features in coronary angiograms. Display stabilization may also help to improve the accuracy of intra-coronary device placement. We validated our automated tracking algorithm by comparing the inter-frame difference (jitter) between manual and automated tracking of 150 coronary x-ray image sequences acquired on a digital cardiovascular X-ray imaging system with CsI/a-Si flat panel detector. We find that the median (50%) inter-frame jitter between manual and automatic tracking is 1.41 pixels or less, indicating a jump no further than an adjacent pixel. This small jitter implies that automated tracking and manual tracking should yield similar improvements in the performance of most visual tasks. We hypothesize that cardiologists would perceive a benefit in viewing the stabilized display as an addition to the standard playback of cine recordings. A benefit of display stabilization was identified in 87 of 101 sequences (86%). The most common tasks cited were evaluation of stenosis and determination of stent and balloon positions. We conclude that display stabilization offers perceptible improvements in the performance of visual tasks by cardiologists.

  11. Validating the Use of pPerformance Risk Indices for System-Level Risk and Maturity Assessments

    NASA Astrophysics Data System (ADS)

    Holloman, Sherrica S.

    With pressure on the U.S. Defense Acquisition System (DAS) to reduce cost overruns and schedule delays, system engineers' performance is only as good as their tools. Recent literature details a need for 1) objective, analytical risk quantification methodologies over traditional subjective qualitative methods -- such as, expert judgment, and 2) mathematically rigorous system-level maturity assessments. The Mahafza, Componation, and Tippett (2005) Technology Performance Risk Index (TPRI) ties the assessment of technical performance to the quantification of risk of unmet performance; however, it is structured for component- level data as input. This study's aim is to establish a modified TPRI with systems-level data as model input, and then validate the modified index with actual system-level data from the Department of Defense's (DoD) Major Defense Acquisition Programs (MDAPs). This work's contribution is the establishment and validation of the System-level Performance Risk Index (SPRI). With the introduction of the SPRI, system-level metrics are better aligned, allowing for better assessment, tradeoff and balance of time, performance and cost constraints. This will allow system engineers and program managers to ultimately make better-informed system-level technical decisions throughout the development phase.

  12. High-solids anaerobic co-digestion of sewage sludge and food waste in comparison with mono digestions: stability and performance.

    PubMed

    Dai, Xiaohu; Duan, Nina; Dong, Bin; Dai, Lingling

    2013-02-01

    System stability and performance of high-solids anaerobic co-digestion of dewatered sludge (DS) and food waste (FW) in comparison with mono digestions were investigated. System stability was improved in co-digestion systems with co-substrate acting as a diluting agent to toxic chemicals like ammonia or Na(+). For high-solids digestion of DS, the addition of FW not only improved system stability but also greatly enhanced volumetric biogas production. For high-solids digestion of FW, the addition of DS could reduce Na(+) concentration and help maintain satisfactory stability during the conversion of FW into biogas. System performances of co-digestion systems were mainly determined by the mixing ratios of DS and FW. Biogas production and volatile solids (VSs) reduction in digestion of the co-mixture of DS and FW increased linearly with higher ratios of FW. A kinetic model, which aimed to forecast the performance of co-digestion and to assist reactor design, was developed from long-term semi-continuous experiments. Maximum VS reduction for DS and FW was estimated to be 44.3% and 90.3%, respectively, and first order constant k was found to be 0.17d(-1) and 0.50 d(-1), respectively. Experimental data of co-digestion were in good conformity to the predictions of the model. Copyright © 2012 Elsevier Ltd. All rights reserved.

  13. 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.

  14. Conceptual framework for holistic dialysis management based on key performance indicators.

    PubMed

    Liu, Hu-Chen; Itoh, Kenji

    2013-10-01

    This paper develops a theoretical framework of holistic hospital management based on performance indicators that can be applied to dialysis hospitals, clinics or departments in Japan. Selection of a key indicator set and its validity tests were performed primarily by a questionnaire survey to dialysis experts as well as their statements obtained through interviews. The expert questionnaire asked respondents to rate the degree of "usefulness" for each of 66 indicators on a three-point scale (19 responses collected). Applying the theoretical framework, we selected a minimum set of key performance indicators for dialysis management that can be used in the Japanese context. The indicator set comprised 27 indicators and items that will be collected through three surveys: patient satisfaction, employee satisfaction, and safety culture. The indicators were confirmed by expert judgment from viewpoints of face, content and construct validity as well as their usefulness. This paper established a theoretical framework of performance measurement for holistic dialysis management from primary healthcare stakeholders' perspectives. In this framework, performance indicators were largely divided into healthcare outcomes and performance shaping factors. Indicators of the former type may be applied for the detection of operational problems or weaknesses in a dialysis hospital, clinic or department, while latent causes of each problem can be more effectively addressed by the latter type of indicators in terms of process, structure and culture/climate within the organization. © 2013 The Authors. Therapeutic Apheresis and Dialysis © 2013 International Society for Apheresis.

  15. Cross-cultural validity and measurement invariance of the Organizational Stressor Indicator for Sport Performers (OSI-SP) across three countries.

    PubMed

    Arnold, R; Ponnusamy, V; Zhang, C-Q; Gucciardi, D F

    2017-08-01

    Organizational stressors are a universal phenomenon which can be particularly prevalent and problematic for sport performers. In view of their global existence, it is surprising that no studies have examined cross-cultural differences in organizational stressors. One explanation for this is that the Organizational Stressor Indicator for Sport Performers (OSI-SP; Arnold, Fletcher, & Daniels, 2013), which can comprehensively measure the organizational pressures that sport performers have encountered, has not yet been translated from English into any other languages nor scrutinized cross-culturally. The first purpose of this study, therefore, was to examine the cross-cultural validity of the OSI-SP. In addition, the study aimed to test the equivalence of the OSI-SP's factor structure across cultures. British (n = 379), Chinese (n = 335), and Malaysian (n = 444) sport performers completed the OSI-SP. Confirmatory factor analyses confirmed the cross-cultural validity of the factorial model for the British and Malaysian samples; however, the overall model fit for the Chinese data did not meet all guideline values. Support was provided for the equality of factor loadings, variances, and covariances on the OSI-SP across the British and Malaysian cultures. These findings advance knowledge and understanding on the cross-cultural existence, conceptualization, and operationalization of organizational stressors. © 2016 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

  16. 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

  17. Stability of physical activity, fitness components and diet quality indices.

    PubMed

    Mertens, E; Clarys, P; Mullie, P; Lefevre, J; Charlier, R; Knaeps, S; Huybrechts, I; Deforche, B

    2017-04-01

    Regular physical activity (PA), a high level of fitness and a high diet quality are positively associated with health. However, information about stability of fitness components and diet quality indices is limited. This study aimed to evaluate stability of those parameters. This study includes 652 adults (men=57.56 (10.28) years; women=55.90 (8.34) years at follow-up) who participated in 2002-2004 and returned for follow-up at the Policy Research Centre Leuven in 2012-2014. Minutes sport per day and Physical activity level (PAL) were calculated from the Flemish Physical Activity Computerized Questionnaire. Cardiorespiratory fitness (CRF), morphological fitness (MORF; body mass index and waist circumference) and metabolic fitness (METF) (blood cholesterol and triglycerides) were used as fitness components. Diet quality indices (Healthy Eating Index-2010 (HEI), Diet Quality Index (DQI), Mediterranean Diet Score (MDS)) were calculated from a diet record. Tracking coefficients were calculated using Pearson/Spearman correlation coefficients (r Pearson ) and intra-class correlation coefficients (r ICC ). In both men (r Pearson&ICC =0.51) and women (r Pearson =0.62 and r ICC =0.60) PAL showed good stability, while minutes sport remained stable in women (r Pearson&ICC =0.57) but less in men (r Pearson&ICC =0.45). Most fitness components remained stable (r⩾0.50) except some METF components in women. In general the diet quality indices and their components were unstable (r<0.50). PAL and the majority of the fitness components remained stable, while diet quality was unstable over 10 years. For unstable parameters such as diet quality measurements are needed at both time points in prospective research.

  18. Numerical Stability and Control Analysis Towards Falling-Leaf Prediction Capabilities of Splitflow for Two Generic High-Performance Aircraft Models

    NASA Technical Reports Server (NTRS)

    Charlton, Eric F.

    1998-01-01

    Aerodynamic analysis are performed using the Lockheed-Martin Tactical Aircraft Systems (LMTAS) Splitflow computational fluid dynamics code to investigate the computational prediction capabilities for vortex-dominated flow fields of two different tailless aircraft models at large angles of attack and sideslip. These computations are performed with the goal of providing useful stability and control data to designers of high performance aircraft. Appropriate metrics for accuracy, time, and ease of use are determined in consultations with both the LMTAS Advanced Design and Stability and Control groups. Results are obtained and compared to wind-tunnel data for all six components of forces and moments. Moment data is combined to form a "falling leaf" stability analysis. Finally, a handful of viscous simulations were also performed to further investigate nonlinearities and possible viscous effects in the differences between the accumulated inviscid computational and experimental data.

  19. 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.

  20. 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.

  1. 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.

  2. Development and Validation of High Performance Liquid Chromatography Method for Determination Atorvastatin in Tablet

    NASA Astrophysics Data System (ADS)

    Yugatama, A.; Rohmani, S.; Dewangga, A.

    2018-03-01

    Atorvastatin is the primary choice for dyslipidemia treatment. Due to patent expiration of atorvastatin, the pharmaceutical industry makes copy of the drug. Therefore, the development methods for tablet quality tests involving atorvastatin concentration on tablets needs to be performed. The purpose of this research was to develop and validate the simple atorvastatin tablet analytical method by HPLC. HPLC system used in this experiment consisted of column Cosmosil C18 (150 x 4,6 mm, 5 µm) as the stationary reverse phase chomatography, a mixture of methanol-water at pH 3 (80:20 v/v) as the mobile phase, flow rate of 1 mL/min, and UV detector at wavelength of 245 nm. Validation methods were including: selectivity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). The results of this study indicate that the developed method had good validation including selectivity, linearity, accuracy, precision, LOD, and LOQ for analysis of atorvastatin tablet content. LOD and LOQ were 0.2 and 0.7 ng/mL, and the linearity range were 20 - 120 ng/mL.

  3. Development and validation of a web-based questionnaire for surveying the health and working conditions of high-performance marine craft populations.

    PubMed

    de Alwis, Manudul Pahansen; Lo Martire, Riccardo; Äng, Björn O; Garme, Karl

    2016-06-20

    High-performance marine craft crews are susceptible to various adverse health conditions caused by multiple interactive factors. However, there are limited epidemiological data available for assessment of working conditions at sea. Although questionnaire surveys are widely used for identifying exposures, outcomes and associated risks with high accuracy levels, until now, no validated epidemiological tool exists for surveying occupational health and performance in these populations. To develop and validate a web-based questionnaire for epidemiological assessment of occupational and individual risk exposure pertinent to the musculoskeletal health conditions and performance in high-performance marine craft populations. A questionnaire for investigating the association between work-related exposure, performance and health was initially developed by a consensus panel under four subdomains, viz. demography, lifestyle, work exposure and health and systematically validated by expert raters for content relevance and simplicity in three consecutive stages, each iteratively followed by a consensus panel revision. The item content validity index (I-CVI) was determined as the proportion of experts giving a rating of 3 or 4. The scale content validity index (S-CVI/Ave) was computed by averaging the I-CVIs for the assessment of the questionnaire as a tool. Finally, the questionnaire was pilot tested. The S-CVI/Ave increased from 0.89 to 0.96 for relevance and from 0.76 to 0.94 for simplicity, resulting in 36 items in the final questionnaire. The pilot test confirmed the feasibility of the questionnaire. The present study shows that the web-based questionnaire fulfils previously published validity acceptance criteria and is therefore considered valid and feasible for the empirical surveying of epidemiological aspects among high-performance marine craft crews and similar populations. Published by the BMJ Publishing Group Limited. For permission to use (where not already granted

  4. Development and validation of a web-based questionnaire for surveying the health and working conditions of high-performance marine craft populations

    PubMed Central

    de Alwis, Manudul Pahansen; Lo Martire, Riccardo; Äng, Björn O; Garme, Karl

    2016-01-01

    Background High-performance marine craft crews are susceptible to various adverse health conditions caused by multiple interactive factors. However, there are limited epidemiological data available for assessment of working conditions at sea. Although questionnaire surveys are widely used for identifying exposures, outcomes and associated risks with high accuracy levels, until now, no validated epidemiological tool exists for surveying occupational health and performance in these populations. Aim To develop and validate a web-based questionnaire for epidemiological assessment of occupational and individual risk exposure pertinent to the musculoskeletal health conditions and performance in high-performance marine craft populations. Method A questionnaire for investigating the association between work-related exposure, performance and health was initially developed by a consensus panel under four subdomains, viz. demography, lifestyle, work exposure and health and systematically validated by expert raters for content relevance and simplicity in three consecutive stages, each iteratively followed by a consensus panel revision. The item content validity index (I-CVI) was determined as the proportion of experts giving a rating of 3 or 4. The scale content validity index (S-CVI/Ave) was computed by averaging the I-CVIs for the assessment of the questionnaire as a tool. Finally, the questionnaire was pilot tested. Results The S-CVI/Ave increased from 0.89 to 0.96 for relevance and from 0.76 to 0.94 for simplicity, resulting in 36 items in the final questionnaire. The pilot test confirmed the feasibility of the questionnaire. Conclusions The present study shows that the web-based questionnaire fulfils previously published validity acceptance criteria and is therefore considered valid and feasible for the empirical surveying of epidemiological aspects among high-performance marine craft crews and similar populations. PMID:27324717

  5. Fabrication and characteristics of high-performance and high-stability aluminum-doped zinc oxide thin-film transistors

    NASA Astrophysics Data System (ADS)

    Shan, Dongfang; Han, Dedong; Huang, Fuqing; Tian, Yu; Zhang, Suoming; Qi, Lin; Cong, Yingying; Zhang, Shengdong; Zhang, Xing; Wang, Yi

    2014-01-01

    Fully transparent aluminum-doped zinc oxide (AZO) thin-film transistors (TFTs) were successfully fabricated on glass substrates at room temperature. Superior properties, such as a high saturation mobility of 59.3 cm2 V-1 s-1, a positive threshold voltage of 1.3 V, a steep subthreshold swing of 122.9 mV/dec, an off-state current on the order of 10-12 A, and an on/off ratio of 2.7 × 108, were obtained. The electrical properties of the AZO TFTs were successively studied within a period of six months. Small property degenerations could be observed from the test results obtained within the study period, which proved the high-performance and high-stability characteristics of AZO TFTs. Furthermore, hysteresis loop scanning of AZO TFTs was performed, and a small hysteresis could be detected in the scanning curves, which suggested the superior properties of a dielectric and a channel-insulator interface. Lastly, we succeeded in manufacturing an organic LED (OLED) flat panel display panel driven by AZO TFTs and obtained an excellent display effect from it. We believe that AZO TFTs are a promising candidate successor to Si-based TFTs in next-generation flat panel displays.

  6. Performance of a Highly Stabilized and High-resolution Beamline BL17SU for Advanced Soft X-ray Spectroscopy at SPring-8

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

    Ohashi, Haruhiko; Tanaka, Takashi; Kitamura, Hideo

    2007-01-19

    A new soft x-ray beamline BL17SU (RIKEN) has been constructed at SPring-8. The beamline consists of two branches with each varied-line-spacing-plane-grating-monochromator. Both monochromators perform high energy resolution (E/{delta}E > 10,000) between 0.2 and 1 keV. One of the monochromator achieves high energy stability of 10 meV over a period of half a day.

  7. A comparison of four embedded validity indices for the RBANS in a memory disorders clinic.

    PubMed

    Paulson, Daniel; Horner, Michael David; Bachman, David

    2015-05-01

    This examination of four embedded validity indices for the Repeated Battery for the Assessment of Neuropsychological Status (RBANS) explores the potential utility of integrating cognitive and self-reported depressive measures. Examined indices include the proposed RBANS Performance Validity Index (RBANS PVI) and the Charleston Revised Index of Effort for the RBANS (CRIER). The CRIER represented the novel integration of cognitive test performance and depression self-report information. The sample included 234 patients without dementia who could be identified as having demonstrated either valid or invalid responding, based on standardized criteria. Sensitivity and specificity for invalid responding varied widely, with the CRIER emerging as the best all-around index (sensitivity = 0.84, specificity = 0.90, AUC = 0.94). Findings support the use of embedded response validity indices, and suggest that the integration of cognitive and self-report depression data may optimize detection of invalid responding among older Veterans. © The Author 2015. Published by Oxford University Press. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  8. Development and validation of stability indicating the RP-HPLC method for the estimation of related compounds of guaifenesin in pharmaceutical dosage forms.

    PubMed

    Reddy, Sunil Pingili; Babu, K Sudhakar; Kumar, Navneet; Sekhar, Y V V Sasi

    2011-10-01

    A stability-indicating gradient reverse phase liquid chromatographic (RP-LC) method was developed for the quantitative determination of related substances of guaifenesin in pharmaceutical formulations. The baseline separation for guaifenesin and all impurities was achieved by utilizing a Water Symmetry C18 (150 mm × 4.6 mm) 5 μm column particle size and a gradient elution method. The mobile phase A contains a mixture of 0.02 M KH2PO4 (pH 3.2) and methanol in the ratio of 90:10 v/v, while the mobile phase B contains 0.02 M KH2PO4 (pH 3.2) and methanol in the ratio of 10:90 v/v, respectively. The flow rate of the mobile phase was 0.8 ml/min with a column temperature of 25°C and detection wavelength at 273 nm. Guaifenesin was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, and photolytic degradation. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness.

  9. Using DEMATEL approach to develop relationships of performance indicators on sustainable service only supply chain performance measurement

    NASA Astrophysics Data System (ADS)

    Leksono, EB; Suparno; Vanany, I.

    2018-04-01

    Service only supply chain (SOSC) concept is service supply chain (SSC) implementation on pure services. The globalization and stakeholder pressure makes operation of SSC should give the attention to the environment effect, community, economic and intangibility assets. SOSC performance measurement (SOSCPM) may be developed for measuring of performance for sustainability aspects and intangibility assets to meet customer satisfaction. This article discusses sustainable SOSCPM based on balanced scorecard (BSC), include sustainability aspects, intangibility and relations between perspectives and indicators. From literature review, it is found 34 performance indicators that must be confirm to expert and SC actors by survey. From survey validation using weighted average and level of consensus, it is found 29 valid indicators for processed by DEMATEL. From DEMATEL, it is found 26 indicators can be used on sustainable SOSCPM. Furthermore, innovation and growth perspective most influence to other, and customer perspective most important. Intangibility indicators incorporated on innovation and growth perspective very related with human resources. Finally, relations between perspectives and indicator used to design of BSC strategy maps.

  10. Embedded performance validity testing in neuropsychological assessment: Potential clinical tools.

    PubMed

    Rickards, Tyler A; Cranston, Christopher C; Touradji, Pegah; Bechtold, Kathleen T

    2018-01-01

    The article aims to suggest clinically-useful tools in neuropsychological assessment for efficient use of embedded measures of performance validity. To accomplish this, we integrated available validity-related and statistical research from the literature, consensus statements, and survey-based data from practicing neuropsychologists. We provide recommendations for use of 1) Cutoffs for embedded performance validity tests including Reliable Digit Span, California Verbal Learning Test (Second Edition) Forced Choice Recognition, Rey-Osterrieth Complex Figure Test Combination Score, Wisconsin Card Sorting Test Failure to Maintain Set, and the Finger Tapping Test; 2) Selecting number of performance validity measures to administer in an assessment; and 3) Hypothetical clinical decision-making models for use of performance validity testing in a neuropsychological assessment collectively considering behavior, patient reporting, and data indicating invalid or noncredible performance. Performance validity testing helps inform the clinician about an individual's general approach to tasks: response to failure, task engagement and persistence, compliance with task demands. Data-driven clinical suggestions provide a resource to clinicians and to instigate conversation within the field to make more uniform, testable decisions to further the discussion, and guide future research in this area.

  11. Deriving and Validating a Road Safety Performance Indicator for Vehicle Fleet Passive Safety

    PubMed Central

    Page, Marianne; Rackliff, Lucy

    2006-01-01

    Road safety performance indicators (RSPI) are policy tools which describe the extent of insecure operational safety conditions within traffic systems. This study describes the production of an RSPI which represents the presence within a country’s vehicle fleet, of vehicles that may not effectively protect an occupant in a collision. This work is highly original, as it uses the entire vehicle database of European Union Member States in order to estimate the average level of passive safety offered by the entire fleet in each country. The EuroNCAP safety ratings and vehicle age of each vehicle in each fleet have been obtained to calculate the RSPI. The methodology used could be adopted as an international standard. PMID:16968645

  12. Enhanced high-performance liquid chromatography method for the determination of retinoic acid in plasma. Development, optimization and validation.

    PubMed

    Teglia, Carla M; Gil García, María D; Galera, María Martínez; Goicoechea, Héctor C

    2014-08-01

    When determining endogenous compounds in biological samples, the lack of blank or analyte-free matrix samples involves the use of alternative strategies for calibration and quantitation. This article deals with the development, optimization and validation of a high performance liquid chromatography method for the determination of retinoic acid in plasma, obtaining at the same time information about its isomers, taking into account the basal concentration of these endobiotica. An experimental design was used for the optimization of three variables: mobile phase composition, flow rate and column temperature through a central composite design. Four responses were selected for optimization purposes (area under the peaks, quantity of peaks, analysis time and resolution between the first principal peak and the following one). The optimum conditions resulted in a mobile phase consisting of methanol 83.4% (v/v), acetonitrile 0.6% (v/v) and acid aqueous solution 16.0% (v/v); flow rate of 0.68 mL min(-1) and an column temperature of 37.10 °C. Detection was performed at 350 nm by a diode array detector. The method was validated following a holistic approach that included not only the classical parameters related to method performance but also the robustness and the expected proportion of acceptable results lying inside predefined acceptability intervals, i.e., the uncertainty of measurements. The method validation results indicated a high selectivity and good precision characteristics that were studied at four concentration levels, with RSD less than 5.0% for retinoic acid (less than 7.5% for the LOQ concentration level), in intra and inter-assay precision studies. Linearity was proved for a range from 0.00489 to 15.109 ng mL(-1) of retinoic acid and the recovery, which was studied at four different fortification levels in phuman plasma samples, varied from 99.5% to 106.5% for retinoic acid. The applicability of the method was demonstrated by determining retinoic acid and

  13. NEXT Performance Curve Analysis and Validation

    NASA Technical Reports Server (NTRS)

    Saripalli, Pratik; Cardiff, Eric; Englander, Jacob

    2016-01-01

    Performance curves of the NEXT thruster are highly important in determining the thruster's ability in performing towards mission-specific goals. New performance curves are proposed and examined here. The Evolutionary Mission Trajectory Generator (EMTG) is used to verify variations in mission solutions based on both available thruster curves and the new curves generated. Furthermore, variations in BOL and EOL curves are also examined. Mission design results shown here validate the use of EMTG and the new performance curves.

  14. High Stability Engine Control (HISTEC) Flight Test Results

    NASA Technical Reports Server (NTRS)

    Southwick, Robert D.; Gallops, George W.; Kerr, Laura J.; Kielb, Robert P.; Welsh, Mark G.; DeLaat, John C.; Orme, John S.

    1998-01-01

    The High Stability Engine Control (HISTEC) Program, managed and funded by the NASA Lewis Research Center, is a cooperative effort between NASA and Pratt & Whitney (P&W). The program objective is to develop and flight demonstrate an advanced high stability integrated engine control system that uses real-time, measurement-based estimation of inlet pressure distortion to enhance engine stability. Flight testing was performed using the NASA Advanced Controls Technologies for Integrated Vehicles (ACTIVE) F-15 aircraft at the NASA Dryden Flight Research Center. The flight test configuration, details of the research objectives, and the flight test matrix to achieve those objectives are presented. Flight test results are discussed that show the design approach can accurately estimate distortion and perform real-time control actions for engine accommodation.

  15. 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.

  16. 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.

  17. High Stability Performance of Quinary Indium Gallium Zinc Aluminum Oxide Films and Thin-Film Transistors Deposited Using Vapor Cooling Condensation Method

    NASA Astrophysics Data System (ADS)

    Lin, Yung-Hao; Lee, Ching-Ting

    2017-08-01

    High-quality indium gallium zinc aluminum oxide (IGZAO) thin films with various Al contents have been deposited using the vapor cooling condensation method. The electron mobility of the IGZAO films was improved by 89.4% on adding Al cation to IGZO film. The change in the electron concentration and mobility of the IGZAO films was 7.3% and 7.0%, respectively, when the temperature was changed from 300 K to 225 K. These experimental results confirm the high performance and stability of the IGZAO films. The performance stability mechanisms of IGZAO thin-film transistors (TFTs) were investigated in comparison with IGZO TFTs.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. Stability Indices derived from Atmospheric Measurements on a Cable Car

    NASA Astrophysics Data System (ADS)

    Herma, F.; Seidel, J.; Bárdossy, A.

    2012-04-01

    Stability indices are meteorological parameters to describe vertical atmospheric layering and therefore it is possible to predict convective events such as thunderstorms. Commonly, weather balloons with radiosondes are used for the analysis of vertical atmospheric layering. These weather balloons reach high altitudes and atmospheric layering can be determined for the entire troposphere. On the other hand, these balloon ascents are expensive, require the appropriate equipment and permissions and cannot be conducted several times a day on an operational basis. Due to the limitations of the application of weather balloons the unconventional idea came up to equip a cable car with meteorological instruments for vertical profile measurements. To some extent the meteorological instruments had to be customized to the particular requirements and data are transmitted via GSM. The investigated area is a small alpine catchment which is prone to flash floods and thus a reliable forecast for such floods mostly caused by convective rainfall events is important. Therefore the purpose of this contribution is to proof if a cable car can be used for measuring continuous data during the operating hours and whether it is possible to derive reliable conclusions about the stability in the lower troposphere. Several stability indices (e.g. Lifted-, Showalter-, Boyden- and Convective-Index) were investigated. Indices which are calculated on the basis of the "Lifted Parcel Theory" were tested with different approaches to determine the most unstable parcel and therefore the initial values of the required parameters. The derived indices were flagged in active (thunderstorms) and non-active (no thunderstorms) cases. The classification results from available lightning maps in this region. Threshold values were established to distinguish stable, potential indifferent and unstable atmospheric conditions. On the basis of this division pre-warnings for the occurrence of thunderstorms are declared

  3. Development and validation of stability indicating the RP-HPLC method for the estimation of related compounds of guaifenesin in pharmaceutical dosage forms

    PubMed Central

    Reddy, Sunil Pingili; Babu, K. Sudhakar; Kumar, Navneet; Sekhar, Y. V. V. Sasi

    2011-01-01

    Aim and background: A stability-indicating gradient reverse phase liquid chromatographic (RP-LC) method was developed for the quantitative determination of related substances of guaifenesin in pharmaceutical formulations. Materials and methods: The baseline separation for guaifenesin and all impurities was achieved by utilizing a Water Symmetry C18 (150 mm × 4.6 mm) 5 μm column particle size and a gradient elution method. The mobile phase A contains a mixture of 0.02 M KH2PO4 (pH 3.2) and methanol in the ratio of 90:10 v/v, while the mobile phase B contains 0.02 M KH2PO4 (pH 3.2) and methanol in the ratio of 10:90 v/v, respectively. The flow rate of the mobile phase was 0.8 ml/min with a column temperature of 25°C and detection wavelength at 273 nm. Results: Guaifenesin was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, and photolytic degradation. Conclusion: The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness. PMID:23781462

  4. Improving the Stability of High-Performance Multilayer MoS2 Field-Effect Transistors.

    PubMed

    Liu, Na; Baek, Jongyeol; Kim, Seung Min; Hong, Seongin; Hong, Young Ki; Kim, Yang Soo; Kim, Hyun-Suk; Kim, Sunkook; Park, Jozeph

    2017-12-13

    In this study, we propose a method for improving the stability of multilayer MoS 2 field-effect transistors (FETs) by O 2 plasma treatment and Al 2 O 3 passivation while sustaining the high performance of bulk MoS 2 FET. The MoS 2 FETs were exposed to O 2 plasma for 30 s before Al 2 O 3 encapsulation to achieve a relatively small hysteresis and high electrical performance. A MoO x layer formed during the plasma treatment was found between MoS 2 and the top passivation layer. The MoO x interlayer prevents the generation of excess electron carriers in the channel, owing to Al 2 O 3 passivation, thereby minimizing the shift in the threshold voltage (V th ) and increase of the off-current leakage. However, prolonged exposure of the MoS 2 surface to O 2 plasma (90 and 120 s) was found to introduce excess oxygen into the MoO x interlayer, leading to more pronounced hysteresis and a high off-current. The stable MoS 2 FETs were also subjected to gate-bias stress tests under different conditions. The MoS 2 transistors exhibited negligible decline in performance under positive bias stress, positive bias illumination stress, and negative bias stress, but large negative shifts in V th were observed under negative bias illumination stress, which is attributed to the presence of sulfur vacancies. This simple approach can be applied to other transition metal dichalcogenide materials to understand their FET properties and reliability, and the resulting high-performance hysteresis-free MoS 2 transistors are expected to open up new opportunities for the development of sophisticated electronic applications.

  5. Evaluation of biologic occupational risk control practices: quality indicators development and validation.

    PubMed

    Takahashi, Renata Ferreira; Gryschek, Anna Luíza F P L; Izumi Nichiata, Lúcia Yasuko; Lacerda, Rúbia Aparecida; Ciosak, Suely Itsuko; Gir, Elucir; Padoveze, Maria Clara

    2010-05-01

    There is growing demand for the adoption of qualification systems for health care practices. This study is aimed at describing the development and validation of indicators for evaluation of biologic occupational risk control programs. The study involved 3 stages: (1) setting up a research team, (2) development of indicators, and (3) validation of the indicators by a team of specialists recruited to validate each attribute of the developed indicators. The content validation method was used for the validation, and a psychometric scale was developed for the specialists' assessment. A consensus technique was used, and every attribute that obtained a Content Validity Index of at least 0.75 was approved. Eight indicators were developed for the evaluation of the biologic occupational risk prevention program, with emphasis on accidents caused by sharp instruments and occupational tuberculosis prevention. The indicators included evaluation of the structure, process, and results at the prevention and biologic risk control levels. The majority of indicators achieved a favorable consensus regarding all validated attributes. The developed indicators were considered validated, and the method used for construction and validation proved to be effective. Copyright (c) 2010 Association for Professionals in Infection Control and Epidemiology, Inc. Published by Mosby, Inc. All rights reserved.

  6. Stability evaluation of tramadol enantiomers using a chiral stability-indicating capillary electrophoresis method and its application to pharmaceutical analysis.

    PubMed

    Mohammadi, Ali; Nojavan, Saeed; Rouini, Mohammadreza; Fakhari, Ali Reza

    2011-07-01

    In this study, a chiral stability-indicating CE assay was developed for the stability evaluation of tramadol (TR) enantiomers in commercial tablets using maltodextrin as chiral selector. To investigate the stability-indicating power of the analytical method as well as stability evaluation of TR enantiomers, active pharmaceutical ingredient and TR tablets were subjected to photolysis, heat, oxidation and hydrolysis to conduct stress testing. Best separation for the TR enantiomers was achieved on an uncoated fused-silica capillary at 20 °C using borate buffer (50 mM, pH 10.2) containing 10% m/v maltodextrin. All determinations were performed by a UV detector at 214 nm. A constant voltage of 20 kV was applied to obtain the separation. The range of quantitation for both enantiomers was 5-100 μg/mL (R>0.996). Intra- and inter-day RSD (n=6) were less than 10%. The percent relevant errors were obtained to be less than 4.0 for both enantiomers. The limits of quantitation and detection for both enantiomers were 5 and 1.5 μg/mL, respectively. Degradation products resulting from the stress studies were the same for both enantiomers and did not interfere with the detection of the enantiomers. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. 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.

  8. 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.

  9. Development and Validation of highly Sensitive Stability Indicating Spectrofluorimetric Method for Determination of Amlodipine in Pharmaceutical Preparations and Human Plasma.

    PubMed

    Mohamed, Abdel-Maaboud I; Omar, Mahmoud A; Hammad, Mohamed A; Mohamed, Abobakr A

    2016-11-01

    A highly sensitive and simple spectrofluorimetric method was developed for the determination of Amlodipine besylate (AML) in its pharmaceutical formulations and spiked human plasma. The proposed method is based on the investigation of the fluorescence spectral behaviour of AML in Tween-80 micellar system. In aqueous solution, the fluorescence intensity of AML was greatly enhanced (160 %) in the presence of Tween-80. The fluorescence intensity was measured at 427 nm after excitation at 385 nm. The fluorescence-concentration plot was rectilinear over the concentration range 0.1-4.0 μg/ml, with lower detection limit of 0.03 μg/ml. The suggested method was successfully applied for the analysis of AML in its commercial tablets alone or in combination with either Atorvastatin or Valsartan. The application of the proposed method was extended to the assay of AML in spiked human plasma and stability studies of AML after exposure to different forced degradation conditions, such as acidic, alkaline, photo- and oxidative conditions, according to ICH guidelines. The results were statistically compared to those obtained by comparison methods and were found to be in good agreement.

  10. 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.

  11. Adaptation and validation of indicators concerning the sterilization process of supplies in Primary Health Care services.

    PubMed

    Passos, Isis Pienta Batista Dias; Padoveze, Maria Clara; Roseira, Camila Eugênia; de Figueiredo, Rosely Moralez

    2015-01-01

    to adapt and validate, by expert consensus, a set of indicators used to assess the sterilization process of dental, medical and hospital supplies to be used in PHC services. qualitative methodological study performed in two stages. The first stage included a focal group composed of experts to adapt the indicators to be used in PHC. In the second stage, the indicators were validated using a 4-point Likert scale, which was completed by judges. A Content Validity Index of ≥ 0.75 was considered to show approval of the indicators. the adaptations implemented by the focal group mainly referred to the physical structure, inclusion of dental care professionals, inclusion of chemical disinfection, and replacement of the hot air and moist heat sterilization methods. The validation stage resulted in an index of 0.96, which ranged from 0.90 to 1.00, for the components of the indicators. the judges considered the indicators after adaptation to be validated. Even though there may be differences among items processed around the world, there certainly are common characteristics, especially in countries with economic and cultural environments similar to Brazil. The inclusion of these indicators to assess the safety of healthcare supplies used in PHC services should be considered.

  12. 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.

  13. Optimizing performance by improving core stability and core strength.

    PubMed

    Hibbs, Angela E; Thompson, Kevin G; French, Duncan; Wrigley, Allan; Spears, Iain

    2008-01-01

    Core stability and core strength have been subject to research since the early 1980s. Research has highlighted benefits of training these processes for people with back pain and for carrying out everyday activities. However, less research has been performed on the benefits of core training for elite athletes and how this training should be carried out to optimize sporting performance. Many elite athletes undertake core stability and core strength training as part of their training programme, despite contradictory findings and conclusions as to their efficacy. This is mainly due to the lack of a gold standard method for measuring core stability and strength when performing everyday tasks and sporting movements. A further confounding factor is that because of the differing demands on the core musculature during everyday activities (low load, slow movements) and sporting activities (high load, resisted, dynamic movements), research performed in the rehabilitation sector cannot be applied to the sporting environment and, subsequently, data regarding core training programmes and their effectiveness on sporting performance are lacking. There are many articles in the literature that promote core training programmes and exercises for performance enhancement without providing a strong scientific rationale of their effectiveness, especially in the sporting sector. In the rehabilitation sector, improvements in lower back injuries have been reported by improving core stability. Few studies have observed any performance enhancement in sporting activities despite observing improvements in core stability and core strength following a core training programme. A clearer understanding of the roles that specific muscles have during core stability and core strength exercises would enable more functional training programmes to be implemented, which may result in a more effective transfer of these skills to actual sporting activities.

  14. 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.

  15. Simultaneous quantification of withanolides in Withania somnifera by a validated high-performance thin-layer chromatographic method.

    PubMed

    Srivastava, Pooja; Tiwari, Neerja; Yadav, Akhilesh K; Kumar, Vijendra; Shanker, Karuna; Verma, Ram K; Gupta, Madan M; Gupta, Anil K; Khanuja, Suman P S

    2008-01-01

    This paper describes a sensitive, selective, specific, robust, and validated densitometric high-performance thin-layer chromatographic (HPTLC) method for the simultaneous determination of 3 key withanolides, namely, withaferin-A, 12-deoxywithastramonolide, and withanolide-A, in Ashwagandha (Withania somnifera) plant samples. The separation was performed on aluminum-backed silica gel 60F254 HPTLC plates using dichloromethane-methanol-acetone-diethyl ether (15 + 1 + 1 + 1, v/v/v/v) as the mobile phase. The withanolides were quantified by densitometry in the reflection/absorption mode at 230 nm. Precise and accurate quantification could be performed in the linear working concentration range of 66-330 ng/band with good correlation (r2 = 0.997, 0.999, and 0.996, respectively). The method was validated for recovery, precision, accuracy, robustness, limit of detection, limit of quantitation, and specificity according to International Conference on Harmonization guidelines. Specificity of quantification was confirmed using retention factor (Rf) values, UV-Vis spectral correlation, and electrospray ionization mass spectra of marker compounds in sample tracks.

  16. 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.

  17. Smart stability-indicating spectrophotometric methods for determination of binary mixtures without prior separation.

    PubMed

    El-Bardicy, Mohammad G; Lotfy, Hayam M; El-Sayed, Mohammad A; El-Tarras, Mohammad F

    2008-01-01

    Ratio subtraction and isosbestic point methods are 2 innovating spectrophotometric methods used to determine vincamine in the presence of its acid degradation product and a mixture of cinnarizine (CN) and nicergoline (NIC). Linear correlations were obtained in the concentration range from 8-40 microg/mL for vincamine (I), 6-22 microg/mL for CN (II), and 6-36 microg/mL for NIC (III), with mean accuracies 99.72 +/- 0.917% for I, 99.91 +/- 0.703% for II, and 99.58 +/- 0.847 and 99.83 +/- 1.039% for III. The ratio subtraction method was utilized for the analysis of laboratory-prepared mixtures containing different ratios of vincamine and its degradation product, and it was valid in the presence of up to 80% degradation product. CN and NIC in synthetic mixtures were analyzed by the 2 proposed methods with the total content of the mixture determined at their respective isosbestic points of 270.2 and 235.8 nm, and the content of CN was determined by the ratio subtraction method. The proposed method was validated and found to be suitable as a stability-indicating assay method for vincamine in pharmaceutical formulations. The standard addition technique was applied to validate the results and to ensure the specificity of the proposed methods.

  18. Atomic-Scale Origin of Long-Term Stability and High Performance of p-GaN Nanowire Arrays for Photocatalytic Overall Pure Water Splitting.

    PubMed

    Kibria, Md Golam; Qiao, Ruimin; Yang, Wanli; Boukahil, Idris; Kong, Xianghua; Chowdhury, Faqrul Alam; Trudeau, Michel L; Ji, Wei; Guo, Hong; Himpsel, F J; Vayssieres, Lionel; Mi, Zetian

    2016-10-01

    The atomic-scale origin of the unusually high performance and long-term stability of wurtzite p-GaN oriented nanowire arrays is revealed. Nitrogen termination of both the polar (0001¯) top face and the nonpolar (101¯0) side faces of the nanowires is essential for long-term stability and high efficiency. Such a distinct atomic configuration ensures not only stability against (photo) oxidation in air and in water/electrolyte but, as importantly, also provides the necessary overall reverse crystal polarization needed for efficient hole extraction in p-GaN. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Validity and reliability of the Short Physical Performance Battery (SPPB)

    PubMed Central

    Curcio, Carmen-Lucía; Alvarado, Beatriz; Zunzunegui, María Victoria; Guralnik, Jack

    2013-01-01

    Objectives: To assess the validity (convergent and construct) and reliability of the Short Physical Performance Battery (SPPB) among non-disabled adults between 65 to 74 years of age residing in the Andes Mountains of Colombia. Methods: Design Validation study; Participants: 150 subjects aged 65 to 74 years recruited from elderly associations (day-centers) in Manizales, Colombia. Measurements: The SPPB tests of balance, including time to walk 4 meters and time required to stand from a chair 5 times were administered to all participants. Reliability was analyzed with a 7-day interval between assessments and use of repeated ANOVA testing. Construct validity was assessed using factor analysis and by testing the relationship between SPPB and depressive symptoms, cognitive function, and self rated health (SRH), while the concurrent validity was measured through relationships with mobility limitations and disability in Activities of Daily Living (ADL). ANOVA tests were used to establish these associations. Results: Test-retest reliability of the SPPB was high: 0.87 (CI95%: 0.77-0.96). A one factor solution was found with three SPPB tests. SPPB was related to self-rated health, limitations in walking and climbing steps and to indicators of disability, as well as to cognitive function and depression. There was a graded decrease in the mean SPPB score with increasing disability and poor health. Conclusion: The Spanish version of SPPB is reliable and valid to assess physical performance among older adults from our region. Future studies should establish their clinical applications and explore usage in population studies. PMID:24892614

  20. Demonstration and Validation of Two Coat High Performance Coating System for Steel Structures in Corrosive Environments

    DTIC Science & Technology

    2016-12-01

    System for Steel Structures in Corrosive Environments Final Report on Project F12-AR06 Co ns tr uc tio n En gi ne er in g R es ea rc h La bo ra...Prevention and Control Program ERDC/CERL TR-16-27 December 2016 Demonstration and Validation of Two-Coat High- Performance Coating System for Steel ...Performance Coating System for Steel Structures in Corrosive Environments” ERDC/CERL TR-16-27 ii Abstract Department of Defense (DoD) installations

  1. 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.

  2. Geometrical analysis of the LiCN vibrational dynamics: a stability geometrical indicator.

    PubMed

    Vergel, A; Benito, R M; Losada, J C; Borondo, F

    2014-02-01

    The vibrational dynamics of the LiNC/LiCN molecular system is examined making use of the Riemannian geometry. Stability and chaoticity are analyzed, in this context, by means of the Jacobi-Levi-Civita equations, derived from the Jacobi metric, and its solutions. A dynamical indicator, called stability geometrical indicator, is introduced in order to ascertain the dynamical characteristics of stability and chaos in the molecule under study.

  3. Soil aggregate stability as an indicator for eco-engineering effectiveness?

    NASA Astrophysics Data System (ADS)

    Graf, Frank

    2015-04-01

    Eco-engineering aims at stabilising soil and slopes by applying technical and biological measures. Engineering structures are commonly well defined, immediately usable and operative, and their stability effects quantifiable and verifiable. Differently, the use of plants requires more restrictive boundary conditions and the protection potential is rarely easily calculable and develop-ing as a function of growth rate. Although the use of vegetation is widely appreciated and their stabilising effect recognised, there is an increasing demand on sound facts on its efficiency, in particular, in relation to time. Conclusively, a certain necessity has been recognised to monitor, assess and quantify the effectiveness of ecological restora-tion measures in order to facilitate the transfer of technology and knowledge. Recent theoretical models emphasize the im-portance of taking an integrated monitoring approach that considers multiple variables. However, limited financial and time resources often prevent such comprehensive assessments. A solution to this problem may be to use integrated indicators that reflect multiple aspects and, therefore, allow extensive information on ecosystem status to be gathered in a relatively short time. Among various other indicators, such as fractal dimension of soil particle size distribution or microbiological parameters, soil aggregate stability seems the most appropriate indicator with regard to protecting slopes from superficial soil failure as it is critical to both plant growth and soil structure. Soil aggregation processes play a crucial role in re-establishing soil structure and function and, conclusively, for successful and sustainable re-colonisation. Whereas the key role of soil aggregate stability in ecosystem functioning is well known concerning water, gas, and nutrient fluxes, only limited information is available with regard to soil mechanical and geotechnical aspects. Correspondingly, in the last couple of years several studies

  4. 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.

  5. Field Validation of the Stability Limit of a Multi MW Turbine

    NASA Astrophysics Data System (ADS)

    Kallesøe, Bjarne S.; Kragh, Knud A.

    2016-09-01

    Long slender blades of modern multi-megawatt turbines exhibit a flutter like instability at rotor speeds above a critical rotor speed. Knowing the critical rotor speed is crucial to a safe turbine design. The flutter like instability can only be estimated using geometrically non-linear aeroelastic codes. In this study, the estimated rotor speed stability limit of a 7 MW state of the art wind turbine is validated experimentally. The stability limit is estimated using Siemens Wind Powers in-house aeroelastic code, and the results show that the predicted stability limit is within 5% of the experimentally observed limit.

  6. Performance Validation Approach for the GTX Air-Breathing Launch Vehicle

    NASA Technical Reports Server (NTRS)

    Trefny, Charles J.; Roche, Joseph M.

    2002-01-01

    The primary objective of the GTX effort is to determine whether or not air-breathing propulsion can enable a launch vehicle to achieve orbit in a single stage. Structural weight, vehicle aerodynamics, and propulsion performance must be accurately known over the entire flight trajectory in order to make a credible assessment. Structural, aerodynamic, and propulsion parameters are strongly interdependent, which necessitates a system approach to design, evaluation, and optimization of a single-stage-to-orbit concept. The GTX reference vehicle serves this purpose, by allowing design, development, and validation of components and subsystems in a system context. The reference vehicle configuration (including propulsion) was carefully chosen so as to provide high potential for structural and volumetric efficiency, and to allow the high specific impulse of air-breathing propulsion cycles to be exploited. Minor evolution of the configuration has occurred as analytical and experimental results have become available. With this development process comes increasing validation of the weight and performance levels used in system performance determination. This paper presents an overview of the GTX reference vehicle and the approach to its performance validation. Subscale test rigs and numerical studies used to develop and validate component performance levels and unit structural weights are outlined. The sensitivity of the equivalent, effective specific impulse to key propulsion component efficiencies is presented. The role of flight demonstration in development and validation is discussed.

  7. 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.

  8. 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.

  9. 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.

  10. The Validity and Incremental Validity of Knowledge Tests, Low-Fidelity Simulations, and High-Fidelity Simulations for Predicting Job Performance in Advanced-Level High-Stakes Selection

    ERIC Educational Resources Information Center

    Lievens, Filip; Patterson, Fiona

    2011-01-01

    In high-stakes selection among candidates with considerable domain-specific knowledge and experience, investigations of whether high-fidelity simulations (assessment centers; ACs) have incremental validity over low-fidelity simulations (situational judgment tests; SJTs) are lacking. Therefore, this article integrates research on the validity of…

  11. Short-term stability of high-silica glasses

    NASA Technical Reports Server (NTRS)

    Leiser, D. B.

    1981-01-01

    The devitrification characteristics of high-silica (70-90%) glasses for use in potential higher temperature coatings on advanced insulation systems for space vehicles were determined at 1260 C after 24 h. These data indicate that additives can be used to maintain the stability of these coatings relative to cristobalite formation.

  12. Test Scores, Dropout Rates, and Transfer Rates as Alternative Indicators of High School Performance

    ERIC Educational Resources Information Center

    Rumberger, Russell W.; Palardy, Gregory J.

    2005-01-01

    This study investigated the relationships among several different indicators of high school performance: test scores, dropout rates, transfer rates, and attrition rates. Hierarchical linear models were used to analyze panel data from a sample of 14,199 students who took part in the National Education Longitudinal Survey of 1988. The results…

  13. 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

  14. 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.

  15. Prediction of pilot-aircraft stability boundaries and performance contours

    NASA Technical Reports Server (NTRS)

    Stengel, R. F.; Broussard, J. R.

    1977-01-01

    Control-theoretic pilot models can provide important new insights regarding the stability and performance characteristics of the pilot-aircraft system. Optimal-control pilot models can be formed for a wide range of flight conditions, suggesting that the human pilot can maintain stability if he adapts his control strategy to the aircraft's changing dynamics. Of particular concern is the effect of sub-optimal pilot adaptation as an aircraft transitions from low to high angle-of-attack during rapid maneuvering, as the changes in aircraft stability and control response can be extreme. This paper examines the effects of optimal and sub-optimal effort during a typical 'high-g' maneuver, and it introduces the concept of minimum-control effort (MCE) adaptation. Limited experimental results tend to support the MCE adaptation concept.

  16. [Preventable drug-related morbidity: determining valid indicators for primary care in Portugal].

    PubMed

    Guerreiro, Mara Pereira; Cantrill, Judith A; Martins, Ana Paula

    2007-01-01

    Preventable drug-related morbidity (PDRM) indicators are operational measures of therapeutic risk management. These clinical indicators, which cover a wide range of drugs, combine process and outcome in the same instrument. They were developed in the US and have been validated for primary care settings in the US, UK and Canada. This study is part of a research programme; it aimed to determine a valid set of PDRM indicators for adult patients in primary care in Portugal. Face validity of 61 US and UK-derived indicators translated to Portuguese was preliminarily determined by means of a postal questionnaire using a purposive sample of four Portuguese pharmacists with different backgrounds. Preliminary content validity of indicators approved in the previous stage was determined by cross-checking each definition of PDRM with standard drug information sources in Portugal. Face and content validity of indicators yielded by preliminary work were then established by a 37 expert panel (20 community pharmacists and 17 general practitioners) using a two-round Delphi survey. Data were analysed using SPSS release 11.5. Nineteen indicators were ruled out in preliminary validation. Changes were made in the content of eight of the remaining 42 indicators; these were related to differences in the drugs being marketed and patterns of drug monitoring between countries. Thirty-five indicators were consensus approved as PDRM for adult patients in Portuguese primary care by the Delphi panel.

  17. Evaluation of the stability indices for the thunderstorm forecasting in the region of Belgrade, Serbia

    NASA Astrophysics Data System (ADS)

    Vujović, D.; Paskota, M.; Todorović, N.; Vučković, V.

    2015-07-01

    The pre-convective atmosphere over Serbia during the ten-year period (2001-2010) was investigated using the radiosonde data from one meteorological station and the thunderstorm observations from thirteen SYNOP meteorological stations. In order to verify their ability to forecast a thunderstorm, several stability indices were examined. Rank sum scores (RSSs) were used to segregate indices and parameters which can differentiate between a thunderstorm and no-thunderstorm event. The following indices had the best RSS values: Lifted index (LI), K index (KI), Showalter index (SI), Boyden index (BI), Total totals (TT), dew-point temperature and mixing ratio. The threshold value test was used in order to determine the appropriate threshold values for these variables. The threshold with the best skill scores was chosen as the optimal. The thresholds were validated in two ways: through the control data set, and comparing the calculated indices thresholds with the values of indices for a randomly chosen day with an observed thunderstorm. The index with the highest skill for thunderstorm forecasting was LI, and then SI, KI and TT. The BI had the poorest skill scores.

  18. Interpretive Structural Model of Key Performance Indicators for Sustainable Maintenance Evaluatian in Rubber Industry

    NASA Astrophysics Data System (ADS)

    Amrina, E.; Yulianto, A.

    2018-03-01

    Sustainable maintenance is a new challenge for manufacturing companies to realize sustainable development. In this paper, an interpretive structural model is developed to evaluate sustainable maintenance in the rubber industry. The initial key performance indicators (KPIs) is identified and derived from literature and then validated by academic and industry experts. As a result, three factors of economic, social, and environmental dividing into a total of thirteen indicators are proposed as the KPIs for sustainable maintenance evaluation in rubber industry. Interpretive structural modeling (ISM) methodology is applied to develop a network structure model of the KPIs consisting of three levels. The results show the economic factor is regarded as the basic factor, the social factor as the intermediate factor, while the environmental factor indicated to be the leading factor. Two indicators of social factor i.e. labor relationship, and training and education have both high driver and dependence power, thus categorized as the unstable indicators which need further attention. All the indicators of environmental factor and one indicator of social factor are indicated as the most influencing indicator. The interpretive structural model hoped can aid the rubber companies in evaluating sustainable maintenance performance.

  19. Rapid Development and Validation of Improved Reversed-Phase High-performance Liquid Chromatography Method for the Quantification of Mangiferin, a Polyphenol Xanthone Glycoside in Mangifera indica

    PubMed Central

    Naveen, P.; Lingaraju, H. B.; Prasad, K. Shyam

    2017-01-01

    Mangiferin, a polyphenolic xanthone glycoside from Mangifera indica, is used as traditional medicine for the treatment of numerous diseases. The present study was aimed to develop and validate a reversed-phase high-performance liquid chromatography (RP-HPLC) method for the quantification of mangiferin from the bark extract of M. indica. RP-HPLC analysis was performed by isocratic elution with a low-pressure gradient using 0.1% formic acid: acetonitrile (87:13) as a mobile phase with a flow rate of 1.5 ml/min. The separation was done at 26°C using a Kinetex XB-C18 column as stationary phase and the detection wavelength at 256 nm. The proposed method was validated for linearity, precision, accuracy, limit of detection, limit of quantification, and robustness by the International Conference on Harmonisation guidelines. In linearity, the excellent correlation coefficient more than 0.999 indicated good fitting of the curve and also good linearity. The intra- and inter-day precision showed < 1% of relative standard deviation of peak area indicated high reliability and reproducibility of the method. The recovery values at three different levels (50%, 100%, and 150%) of spiked samples were found to be 100.47, 100.89, and 100.99, respectively, and low standard deviation value < 1% shows high accuracy of the method. In robustness, the results remain unaffected by small variation in the analytical parameters, which shows the robustness of the method. Liquid chromatography–mass spectrometry analysis confirmed the presence of mangiferin with M/Z value of 421. The assay developed by HPLC method is a simple, rapid, and reliable for the determination of mangiferin from M. indica. SUMMARY The present study was intended to develop and validate an RP-HPLC method for the quantification of mangiferin from the bark extract of M. indica. The developed method was validated for linearity, precision, accuracy, limit of detection, limit of quantification and robustness by International

  20. Rapid Development and Validation of Improved Reversed-Phase High-performance Liquid Chromatography Method for the Quantification of Mangiferin, a Polyphenol Xanthone Glycoside in Mangifera indica.

    PubMed

    Naveen, P; Lingaraju, H B; Prasad, K Shyam

    2017-01-01

    Mangiferin, a polyphenolic xanthone glycoside from Mangifera indica , is used as traditional medicine for the treatment of numerous diseases. The present study was aimed to develop and validate a reversed-phase high-performance liquid chromatography (RP-HPLC) method for the quantification of mangiferin from the bark extract of M. indica . RP-HPLC analysis was performed by isocratic elution with a low-pressure gradient using 0.1% formic acid: acetonitrile (87:13) as a mobile phase with a flow rate of 1.5 ml/min. The separation was done at 26°C using a Kinetex XB-C18 column as stationary phase and the detection wavelength at 256 nm. The proposed method was validated for linearity, precision, accuracy, limit of detection, limit of quantification, and robustness by the International Conference on Harmonisation guidelines. In linearity, the excellent correlation coefficient more than 0.999 indicated good fitting of the curve and also good linearity. The intra- and inter-day precision showed < 1% of relative standard deviation of peak area indicated high reliability and reproducibility of the method. The recovery values at three different levels (50%, 100%, and 150%) of spiked samples were found to be 100.47, 100.89, and 100.99, respectively, and low standard deviation value < 1% shows high accuracy of the method. In robustness, the results remain unaffected by small variation in the analytical parameters, which shows the robustness of the method. Liquid chromatography-mass spectrometry analysis confirmed the presence of mangiferin with M/Z value of 421. The assay developed by HPLC method is a simple, rapid, and reliable for the determination of mangiferin from M. indica . The present study was intended to develop and validate an RP-HPLC method for the quantification of mangiferin from the bark extract of M. indica . The developed method was validated for linearity, precision, accuracy, limit of detection, limit of quantification and robustness by International

  1. Validity of police contacts as a performance indicator for the public mental health care system in Amsterdam: an open cohort study.

    PubMed

    Lauriks, S; Buster, M C A; de Wit, M A S; Arah, O A; Hoogendoorn, A W; Peen, J; Klazinga, N S

    2018-06-01

    The Public Mental Health Care (PMHC) system is a network of public services and care- and support institutions financed from public funds. Performance indicators based on the registration of police contacts could be a reliable and useful source of information for the stakeholders of the PMHC system to monitor performance. This study aimed to provide evidence on the validity of using police contacts as a performance indicator to assess the continuity of care in the PMHC system. Data on services received, police contacts and detention periods of 1928 people that entered the PMHC system in the city of Amsterdam were collected over a period of 51 months. Continuity of care was defined as receiving more than 90 days of uninterrupted service. The associations between police contacts and continuity were analyzed with multilevel Poisson and multivariate linear regression modeling. Clients had on average 2.12 police contacts per person-year. Clients with police contacts were younger, more often single, male, and more often diagnosed with psychiatric or substance abuse disorders than clients without police contacts. Incidence rates of police contacts were significantly lower for clients receiving continuous care than for clients receiving discontinuous care. The number of police contacts of clients receiving PMHC coordination per month was found to be a significant predictor of the percentage of clients in continuous care. The number of police contacts of clients can be used as a performance indicator for an urban PMHC system to evaluate the continuity of care in the PMHC system.

  2. 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.

  3. Development and validation of a normal-phase high-performance thin layer chromatographic method for the analysis of sulfamethoxazole and trimethoprim in co-trimoxazole tablets.

    PubMed

    Shewiyo, D H; Kaale, E; Risha, P G; Dejaegher, B; Smeyers-Verbeke, J; Vander Heyden, Y

    2009-10-16

    Pneumocystis carinii pneumonia (PCP) is often the ultimate mortal cause for immunocompromised individuals, such as HIV/AIDS patients. Currently, the most effective medicine for treatment and prophylaxis is co-trimoxazole, a synergistic combination of sulfamethoxazole (SMX) and trimethoprim (TMP). In order to ensure a continued availability of high quality co-trimoxazole tablets within resource-limited countries, Medicines Regulatory Authorities must perform quality control of these products. However, most pharmacopoeial methods are based on high-performance liquid chromatographic (HPLC) methods. Because of the lack of equipment, the Tanzania Food and Drugs Authority (TFDA) laboratory decided to develop and validate an alternative method of analysis based on the TLC technique with densitometric detection, for the routine quality control of co-trimoxazole tablets. SMX and TMP were separated on glass-backed silica gel 60 F(254) plates in a high-performance thin layer chromatograph (HPTLC). The mobile phase was comprised of toluene, ethylacetate and methanol (50:28.5:21.5, v:v:v). Detection wavelength was 254 nm. The R(f) values were 0.30 and 0.61 for TMP and SMX, respectively. This method was validated for linearity, precision, trueness, specificity and robustness. Cochran's criterion test indicated homoscedasticity of variances for the calibration data. The F-tests for lack-of-fit indicated that straight lines were adequate to describe the relationship between spot areas and concentrations for each compound. The percentage relative standard deviations for repeatability and time-different precisions were 0.98 and 1.32, and 0.83 and 1.64 for SMX and TMP, respectively. Percentage recovery values were 99.00%+/-1.83 and 99.66%+/-1.21 for SMX and TMP, respectively. The method was found to be robust and was then successfully applied to analyze co-trimoxazole tablet samples.

  4. 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.

  5. A C-Te-based binary OTS device exhibiting excellent performance and high thermal stability for selector application.

    PubMed

    Chekol, Solomon Amsalu; Yoo, Jongmyung; Park, Jaehyuk; Song, Jeonghwan; Sung, Changhyuck; Hwang, Hyunsang

    2018-08-24

    In this letter, we demonstrate a new binary ovonic threshold switching (OTS) selector device scalable down to ø30 nm based on C-Te. Our proposed selector device exhibits outstanding performance such as a high switching ratio (I on /I off  > 10 5 ), an extremely low off-current (∼1 nA), an extremely fast operating speed of <10 ns (transition time of <2 ns and delay time of <8 ns), high endurance (10 9 ), and high thermal stability (>450 °C). The observed high thermal stability is caused by the relatively small atomic size of C, compared to Te, which can effectively suppress the segregation and crystallization of Te in the OTS film. Furthermore, to confirm the functionality of the selector in a crossbar array, we evaluated a 1S-1R device by integrating our OTS device with a ReRAM (resistive random access memory) device. The 1S-1R integrated device exhibits a successful suppression of leakage current at the half-selected cell and shows an excellent read-out margin (>2 12 word lines) in a fast read operation.

  6. 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.

  7. LOX/hydrocarbon rocket engine analytical design methodology development and validation. Volume 2: Appendices

    NASA Technical Reports Server (NTRS)

    Niiya, Karen E.; Walker, Richard E.; Pieper, Jerry L.; Nguyen, Thong V.

    1993-01-01

    This final report includes a discussion of the work accomplished during the period from Dec. 1988 through Nov. 1991. The objective of the program was to assemble existing performance and combustion stability models into a usable design methodology capable of designing and analyzing high-performance and stable LOX/hydrocarbon booster engines. The methodology was then used to design a validation engine. The capabilities and validity of the methodology were demonstrated using this engine in an extensive hot fire test program. The engine used LOX/RP-1 propellants and was tested over a range of mixture ratios, chamber pressures, and acoustic damping device configurations. This volume contains time domain and frequency domain stability plots which indicate the pressure perturbation amplitudes and frequencies from approximately 30 tests of a 50K thrust rocket engine using LOX/RP-1 propellants over a range of chamber pressures from 240 to 1750 psia with mixture ratios of from 1.2 to 7.5. The data is from test configurations which used both bitune and monotune acoustic cavities and from tests with no acoustic cavities. The engine had a length of 14 inches and a contraction ratio of 2.0 using a 7.68 inch diameter injector. The data was taken from both stable and unstable tests. All combustion instabilities were spontaneous in the first tangential mode. Although stability bombs were used and generated overpressures of approximately 20 percent, no tests were driven unstable by the bombs. The stability instrumentation included six high-frequency Kistler transducers in the combustion chamber, a high-frequency Kistler transducer in each propellant manifold, and tri-axial accelerometers. Performance data is presented, both characteristic velocity efficiencies and energy release efficiencies, for those tests of sufficient duration to record steady state values.

  8. 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…

  9. Performance indicators: healthcare professionals' views.

    PubMed

    Gu, Xiuzhu; Itoh, Kenji

    2016-08-08

    Purpose - The purpose of this paper is to capture factors behind professional views of indicator usefulness as a common structure for assessing healthcare performance and their important characteristics to design limited key performance indicators (PIs) for holistic hospital management. Design/methodology/approach - Two surveys were conducted using self-administered questionnaires, in which hospital manager/staff respondents were asked to rate the 52 PIs' usefulness. In total, 228 manager and 894 staff responses were collected. Findings - Eight factors were elicited from manager and staff responses as performance measures with 72 percent cumulative variance accounted for. Hospital managers and staff showed similar performance measure perceptions: high-utility acknowledgment on safety, operational efficiency and patient/employee satisfaction but relatively low-employee development concerns. Manager indicator usefulness perceptions were rather homogeneous and significantly higher than staff for almost all performance measures. Practical implications - Homogeneous manager views mean that a single key PI set for hospital management may be established regardless of hospital attributes. The following aspects may be measures that should be managed in a healthcare organization based on their key PIs: patient/employee safety, operational efficiency, financial effectiveness and patient/employee satisfaction. Originality/value - This is a pilot study on hospital management PIs in Japan. The eight-dimensional factor structure and findings about healthcare provider perceptions may be useful for healthcare management.

  10. 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.

  11. Development and Validation of a Stability-Indicating RP-HPLC Method for Duloxetine Hydrochloride in its Bulk and Tablet Dosage Form

    PubMed Central

    Chhalotiya, Usmangani K.; Bhatt, Kashyap K.; Shah, Dimal A.; Baldania, Sunil L.

    2010-01-01

    The objective of the present work was to develop a stability-indicating RP-HPLC method for duloxetine hydrochloride (DUL) in the presence of its degradation products generated from forced decomposition studies. The drug substance was found to be susceptible to stress conditions of acid hydrolysis. The drug was found to be stable to dry heat, photodegradation, oxidation and basic condition attempted. Successful separation of the drug from the degradation products formed under acidic stress conditions was achieved on a Hypersil C-18 column (250 mm × 4.6 mm id, 5μm particle size) using acetonitrile: 0.01 M potassium dihydrogen phosphate buffer (pH 5.4 adjusted with orthophosphoric acid) (50:50, v/v) as the mobile phase at a flow rate of 1.0 ml/min. Quantification was achieved with photodiode array detection at 229 nm over the concentration range 1–25 μg/ml with range of recovery 99.8–101.3 % for DUL by the RP-HPLC method. Statistical analysis proved the method to be repeatable, specific, and accurate for estimation of DUL. It can be used as a stability-indicating method due to its effective separation of the drug from its degradation products, PMID:21179321

  12. 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

  13. Investigation into the temporal stability of aqueous standard solutions of psilocin and psilocybin using high performance liquid chromatography.

    PubMed

    Anastos, N; Barnett, N W; Pfeffer, F M; Lewis, S W

    2006-01-01

    This paper reports an investigation into the temporal stability of aqueous solutions of psilocin and psilocybin reference drug standards over a period of fourteen days. This study was performed using high performance liquid chromatography utilising a (95:5% v/v) methanol: 10 mM ammonium formate, pH 3.5 mobile phase and absorption detection at 269 nm. It was found that the exclusion of light significantly prolonged the useful life of standards, with aqueous solutions of both psilocin and psilocybin being stable over a period of seven days.

  14. Cognitively Elite, Cognitively Normal, and Cognitively Impaired Aging: Neurocognitive Status and Stability Moderate Memory Performance

    PubMed Central

    Dixon, Roger A.; de Frias, Cindy M.

    2014-01-01

    Objective Although recent theories of brain and cognitive aging distinguish among normal, exceptional, and impaired groups, further empirical evidence is required. We adapted and applied standard procedures for classifying groups of cognitively impaired (CI) and cognitively normal (CN) older adults to a third classification, cognitively healthy, exceptional, or elite (CE) aging. We then examined concurrent and two-wave longitudinal performance on composite variables of episodic, semantic, and working memory. Method We began with a two-wave source sample from the Victoria Longitudinal Study (VLS) (source n=570; baseline age=53–90 years). The goals were to: (a) apply standard and objective classification procedures to discriminate three cognitive status groups, (b) conduct baseline comparisons of memory performance, (c) develop two-wave status stability and change subgroups, and (d) compare of stability subgroup differences in memory performance and change. Results As expected, the CE group performed best on all three memory composites. Similarly, expected status stability effects were observed: (a) stable CE and CN groups performed memory tasks better than their unstable counterparts and (b) stable (and chronic) CI group performed worse than its unstable (variable) counterpart. These stability group differences were maintained over two waves. Conclusion New data validate the expectations that (a) objective clinical classification procedures for cognitive impairment can be adapted for detecting cognitively advantaged older adults and (b) performance in three memory systems is predictably related to the tripartite classification. PMID:24742143

  15. Stability indicating HPLC method for simultaneous determination of mephenesin and diclofenac diethylamine.

    PubMed

    Mulgund, S V; Phoujdar, M S; Londhe, S V; Mallade, P S; Kulkarni, T S; Deshpande, A S; Jain, K S

    2009-01-01

    A simple, specific, accurate and stability-indicating reversed phase high performance liquid chromatographic method was developed for the simultaneous determination of mephenesin and diclofenac diethylamine, using a Spheri-5-RP-18 column and a mobile phase composed of methanol: water (70:30, v/v), pH 3.0 adjusted with o-phosphoric acid. The retention times of mephenesin and diclofenac diethylamine were found to be 3.9 min and 14.5 min, respectively. Linearity was established for mephenesin and diclofenac diethylamine in the range of 50-300 mug/ml and 10-60 mug/ml, respectively. The percentage recoveries of mephenesin and diclofenac diethylamine were found to be in the range of 99.06-100.60% and 98.95-99.98%, respectively. Both the drugs were subjected to acid, alkali and neutral hydrolysis, oxidation, dry heat, photolytic and UV degradation. The degradation studies indicated, mephenesin to be susceptible to neutral hydrolysis, while diclofenac diethylamine showed degradation in acid, H(2)O(2), photolytic and in presence of UV radiation. The degradation products of diclofenac diethylamine in acidic and photolytic conditions were well resolved from the pure drug with significant differences in their retention time values. This method can be successfully employed for simultaneous quantitative analysis of mephenesin and diclofenac diethylamine in bulk drugs and formulations.

  16. 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.

  17. Experimental validation of prototype high voltage bushing

    NASA Astrophysics Data System (ADS)

    Shah, Sejal; Tyagi, H.; Sharma, D.; Parmar, D.; M. N., Vishnudev; Joshi, K.; Patel, K.; Yadav, A.; Patel, R.; Bandyopadhyay, M.; Rotti, C.; Chakraborty, A.

    2017-08-01

    Prototype High voltage bushing (PHVB) is a scaled down configuration of DNB High Voltage Bushing (HVB) of ITER. It is designed for operation at 50 kV DC to ensure operational performance and thereby confirming the design configuration of DNB HVB. Two concentric insulators viz. Ceramic and Fiber reinforced polymer (FRP) rings are used as double layered vacuum boundary for 50 kV isolation between grounded and high voltage flanges. Stress shields are designed for smooth electric field distribution. During ceramic to Kovar brazing, spilling cannot be controlled which may lead to high localized electrostatic stress. To understand spilling phenomenon and precise stress calculation, quantitative analysis was performed using Scanning Electron Microscopy (SEM) of brazed sample and similar configuration modeled while performing the Finite Element (FE) analysis. FE analysis of PHVB is performed to find out electrical stresses on different areas of PHVB and are maintained similar to DNB HV Bushing. With this configuration, the experiment is performed considering ITER like vacuum and electrical parameters. Initial HV test is performed by temporary vacuum sealing arrangements using gaskets/O-rings at both ends in order to achieve desired vacuum and keep the system maintainable. During validation test, 50 kV voltage withstand is performed for one hour. Voltage withstand test for 60 kV DC (20% higher rated voltage) have also been performed without any breakdown. Successful operation of PHVB confirms the design of DNB HV Bushing. In this paper, configuration of PHVB with experimental validation data is presented.

  18. Performance Evaluation of a Data Validation System

    NASA Technical Reports Server (NTRS)

    Wong, Edmond (Technical Monitor); Sowers, T. Shane; Santi, L. Michael; Bickford, Randall L.

    2005-01-01

    Online data validation is a performance-enhancing component of modern control and health management systems. It is essential that performance of the data validation system be verified prior to its use in a control and health management system. A new Data Qualification and Validation (DQV) Test-bed application was developed to provide a systematic test environment for this performance verification. The DQV Test-bed was used to evaluate a model-based data validation package known as the Data Quality Validation Studio (DQVS). DQVS was employed as the primary data validation component of a rocket engine health management (EHM) system developed under NASA's NGLT (Next Generation Launch Technology) program. In this paper, the DQVS and DQV Test-bed software applications are described, and the DQV Test-bed verification procedure for this EHM system application is presented. Test-bed results are summarized and implications for EHM system performance improvements are discussed.

  19. Predictive validity of pre-admission assessments on medical student performance.

    PubMed

    Dabaliz, Al-Awwab; Kaadan, Samy; Dabbagh, M Marwan; Barakat, Abdulaziz; Shareef, Mohammad Abrar; Al-Tannir, Mohamad; Obeidat, Akef; Mohamed, Ayman

    2017-11-24

    To examine the predictive validity of pre-admission variables on students' performance in a medical school in Saudi Arabia. In this retrospective study, we collected admission and college performance data for 737 students in preclinical and clinical years. Data included high school scores and other standardized test scores, such as those of the National Achievement Test and the General Aptitude Test. Additionally, we included the scores of the Test of English as a Foreign Language (TOEFL) and the International English Language Testing System (IELTS) exams. Those datasets were then compared with college performance indicators, namely the cumulative Grade Point Average (cGPA) and progress test, using multivariate linear regression analysis. In preclinical years, both the National Achievement Test (p=0.04, B=0.08) and TOEFL (p=0.017, B=0.01) scores were positive predictors of cGPA, whereas the General Aptitude Test (p=0.048, B=-0.05) negatively predicted cGPA. Moreover, none of the pre-admission variables were predictive of progress test performance in the same group. On the other hand, none of the pre-admission variables were predictive of cGPA in clinical years. Overall, cGPA strongly predict-ed students' progress test performance (p<0.001 and B=19.02). Only the National Achievement Test and TOEFL significantly predicted performance in preclinical years. However, these variables do not predict progress test performance, meaning that they do not predict the functional knowledge reflected in the progress test. We report various strengths and deficiencies in the current medical college admission criteria, and call for employing more sensitive and valid ones that predict student performance and functional knowledge, especially in the clinical years.

  20. Performance Validity Testing in Neuropsychology: Scientific Basis and Clinical Application-A Brief Review.

    PubMed

    Greher, Michael R; Wodushek, Thomas R

    2017-03-01

    Performance validity testing refers to neuropsychologists' methodology for determining whether neuropsychological test performances completed in the course of an evaluation are valid (ie, the results of true neurocognitive function) or invalid (ie, overly impacted by the patient's effort/engagement in testing). This determination relies upon the use of either standalone tests designed for this sole purpose, or specific scores/indicators embedded within traditional neuropsychological measures that have demonstrated this utility. In response to a greater appreciation for the critical role that performance validity issues play in neuropsychological testing and the need to measure this variable to the best of our ability, the scientific base for performance validity testing has expanded greatly over the last 20 to 30 years. As such, the majority of current day neuropsychologists in the United States use a variety of measures for the purpose of performance validity testing as part of everyday forensic and clinical practice and address this issue directly in their evaluations. The following is the first article of a 2-part series that will address the evolution of performance validity testing in the field of neuropsychology, both in terms of the science as well as the clinical application of this measurement technique. The second article of this series will review performance validity tests in terms of methods for development of these measures, and maximizing of diagnostic accuracy.

  1. 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.

  2. High performance aluminum–cerium alloys for high-temperature applications

    DOE PAGES

    Sims, Zachary C.; Rios, Orlando R.; Weiss, David; ...

    2017-08-01

    Light-weight high-temperature alloys are important to the transportation industry where weight, cost, and operating temperature are major factors in the design of energy efficient vehicles. Aluminum alloys fill this gap economically but lack high-temperature mechanical performance. Alloying aluminum with cerium creates a highly castable alloy, compatible with traditional aluminum alloy additions, that exhibits dramatically improved high-temperature performance. These compositions display a room temperature ultimate tensile strength of 400 MPa and yield strength of 320 MPa, with 80% mechanical property retention at 240 °C. A mechanism is identified that addresses the mechanical property stability of the Al-alloys to at least 300more » °C and their microstructural stability to above 500 °C which may enable applications without the need for heat treatment. Lastly, neutron diffraction under load provides insight into the unusual mechanisms driving the mechanical strength.« less

  3. Double Cross-Validation in Multiple Regression: A Method of Estimating the Stability of Results.

    ERIC Educational Resources Information Center

    Rowell, R. Kevin

    In multiple regression analysis, where resulting predictive equation effectiveness is subject to shrinkage, it is especially important to evaluate result replicability. Double cross-validation is an empirical method by which an estimate of invariance or stability can be obtained from research data. A procedure for double cross-validation is…

  4. Collar height and heel counter-stiffness for ankle stability and athletic performance in basketball.

    PubMed

    Liu, Hui; Wu, Zitian; Lam, Wing-Kai

    2017-01-01

    This study examined the effects of collar height and heel counter-stiffness of basketball shoes on ankle stability during sidestep cutting and athletic performance. 15 university basketball players wore customized shoes with different collar heights (high and low) and heel counter-stiffness (regular, stiffer and stiffest) for this study. Ankle stability was evaluated in sidestep cutting while athletic performance evaluated in jumping and agility tasks. All variables were analysed using two-way repeated ANOVA. Results showed shorter time to peak ankle inversion for both high collar and stiff heel counter conditions (P < 0.05), while smaller initial ankle inversion angle, peak inversion velocity and total range of inversion for wearing high collar shoes (P < 0.05). No shoe differences were found for performance variables. These findings imply that the collar height might play a larger role in lateral stability than heel counter-stiffness, while both collar height and counter-stiffness have no effect on athletic performance.

  5. 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).

  6. Development and validation of a high performance liquid chromatography assay for 17alpha-methyltestosterone in fish feed.

    PubMed

    Marwah, Ashok; Marwah, Padma; Lardy, Henry

    2005-09-25

    17alpha-Methyltestosterone (MT) is used to manipulate the gender of a variety of fish species. A high performance liquid chromatography (HPLC) internal standard method for the determination of 17alpha-methyltestosterone in fish feed using 3beta-methoxy-17beta-hydroxyandrost-5-en-7-one as internal standard (IS) has been developed. The method has been validated for the quantitation of MT in fish feed using 245 nm UV absorbance as the parent wavelength and 255 nm as a qualifier wavelength. The method was validated in the concentration range of 15.0-120 mg/kg of 17alpha-methyltestosterone in fish feed. Method was also found to be suitable for other feeds.

  7. Test of the Hill Stability Criterion against Chaos Indicators

    NASA Astrophysics Data System (ADS)

    Satyal, Suman; Quarles, Billy; Hinse, Tobias

    2012-10-01

    The efficacy of Hill Stability (HS) criterion is tested against other known chaos indicators such as Maximum Lyapunov Exponents (MLE) and Mean Exponential Growth of Nearby Orbits (MEGNO) maps. First, orbits of four observationally verified binary star systems: γ Cephei, Gliese-86, HD41004, and HD196885 are integrated using standard integration packages (MERCURY, SWIFTER, NBI, C/C++). The HS which measures orbital perturbation of a planet around the primary star due to the secondary star is calculated for each system. The LEs spectra are generated to measure the divergence/convergence rate of stable manifolds and the MEGNO maps are generated by using the variational equations of the system during the integration process. These maps allow to accurately differentiate between stable and unstable dynamical systems. Then the results obtained from the analysis of HS, MLE, and MEGNO maps are checked for their dynamical variations and resemblance. The HS of most of the planets seems to be stable, quasi-periodic for at least ten million years. The MLE and the MEGNO maps also indicate the local quasi-periodicity and global stability in relatively short integration period. The HS criterion is found to be a comparably efficient tool to measure the stability of planetary orbits.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. Spectrofluorimetric methods of stability-indicating assay of certain drugs affecting the cardiovascular system

    NASA Astrophysics Data System (ADS)

    Moussa, B. A.; Mohamed, M. F.; Youssef, N. F.

    2011-01-01

    Two stability-indicating spectrofluorimetric methods have been developed for the determination of ezetimibe and olmesartan medoxomil, drugs affecting the cardiovascular system, and validated in the presence of their degradation products. The first method, for ezetimibe, is based on an oxidative coupling reaction of ezetimibe with 3-methylbenzothiazolin-2-one hydrazone hydrochloride in the presence of cerium (IV) ammonium sulfate in an acidic medium. The quenching effect of ezetimibe on the fluorescence of excess cerous ions is measured at the emission wavelength, λem, of 345 nm with the excitation wavelength, λex, of 296 nm. Factors affecting the reaction were carefully studied and optimized. The second method, for olmesartan medoxomil, is based on measuring the native fluorescence intensity of olmesartan medoxomil in methanol at λem = 360 nm with λex = 286 nm. Regression plots revealed good linear relationships in the assay limits of 10-120 and 8-112 g/ml for ezetimibe and olmesartan medoxomil, respectively. The validity of the methods was assessed according to the United States Pharmacopeya guidelines. Statistical analysis of the results exposed good Student's t-test and F-ratio values. The introduced methods were successfully applied to the analysis of ezetimibe and olmesartan medoxomil in drug substances and drug products as well as in the presence of their degradation products.

  14. Development and validation of a high-performance liquid chromatography method for determination of cefquinome concentrations in sheep plasma and its application to pharmacokinetic studies.

    PubMed

    Uney, Kamil; Altan, Feray; Elmas, Muammer

    2011-02-01

    Cefquinome has a broad spectrum of antibacterial activity and was developed especially for use in animals. A simple and sensitive high-performance liquid chromatography (HPLC) method with UV-visible detection for quantification of cefquinome concentrations in sheep plasma was developed and validated. Separation of cefquinome from plasma components was achieved on a Phenomenex Gemini C(18) column (250 mm by 4.6 mm; internal diameter [i.d.], 5 μm). The mobile phase consisted of acetonitrile and 0.1% trifluoroacetic acid in water and was delivered at a rate of 0.9 ml/min. A simple and rapid sample preparation involved the addition of methanol to 200 μl of plasma to precipitate plasma proteins followed by direct injection of 50 μl of supernatant into the high-performance liquid chromatography system. The linearity range of the proposed method was 0.02 to 12 μg/ml. The intraday and interday coefficients of variation obtained from cefquinome were less than 5%, and biases ranged from -3.76% to 1.24%. Mean recovery based on low-, medium-, and high-quality control standards ranged between 92.0 and 93.9%. Plasma samples were found to be stable in various storage conditions (freeze-thaw, postpreparative, short-term, and long-term stability). The method described was found to be readily available, practicable, cheap, rapid, sensitive, precise, and accurate. It was successfully applied to the study of the pharmacokinetics of cefquinome in sheep. This method can be very useful and an alternate to performing pharmacokinetic studies in the determination of cefquinome for clinical use.

  15. A recursive field-normalized bibliometric performance indicator: an application to the field of library and information science.

    PubMed

    Waltman, Ludo; Yan, Erjia; van Eck, Nees Jan

    2011-10-01

    Two commonly used ideas in the development of citation-based research performance indicators are the idea of normalizing citation counts based on a field classification scheme and the idea of recursive citation weighing (like in PageRank-inspired indicators). We combine these two ideas in a single indicator, referred to as the recursive mean normalized citation score indicator, and we study the validity of this indicator. Our empirical analysis shows that the proposed indicator is highly sensitive to the field classification scheme that is used. The indicator also has a strong tendency to reinforce biases caused by the classification scheme. Based on these observations, we advise against the use of indicators in which the idea of normalization based on a field classification scheme and the idea of recursive citation weighing are combined.

  16. A Lithium-Air Battery Stably Working at High Temperature with High Rate Performance.

    PubMed

    Pan, Jian; Li, Houpu; Sun, Hao; Zhang, Ye; Wang, Lie; Liao, Meng; Sun, Xuemei; Peng, Huisheng

    2018-02-01

    Driven by the increasing requirements for energy supply in both modern life and the automobile industry, the lithium-air battery serves as a promising candidate due to its high energy density. However, organic solvents in electrolytes are likely to rapidly vaporize and form flammable gases under increasing temperatures. In this case, serious safety problems may occur and cause great harm to people. Therefore, a kind of lithium-air that can work stably under high temperature is desirable. Herein, through the use of an ionic liquid and aligned carbon nanotubes, and a fiber shaped design, a new type of lithium-air battery that can effectively work at high temperatures up to 140 °C is developed. Ionic liquids can offer wide electrochemical windows and low vapor pressures, as well as provide high thermal stability for lithium-air batteries. The aligned carbon nanotubes have good electric and heat conductivity. Meanwhile, the fiber format can offer both flexibility and weavability, and realize rapid heat conduction and uniform heat distribution of the battery. In addition, the high temperature has also largely improved the specific powers by increasing the ionic conductivity and catalytic activity of the cathode. Consequently, the lithium-air battery can work stably at 140 °C with a high specific current of 10 A g -1 for 380 cycles, indicating high stability and good rate performance at high temperatures. This work may provide an effective paradigm for the development of high-performance energy storage devices. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. 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.

  18. [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.

  19. Association between attempted suicide and academic performance indicators among middle and high school students in Mexico: results from a national survey.

    PubMed

    Orozco, Ricardo; Benjet, Corina; Borges, Guilherme; Moneta Arce, María Fátima; Fregoso Ito, Diana; Fleiz, Clara; Villatoro, Jorge Ameth

    2018-01-01

    Students' mental health is associated to academic performance. In high income countries, higher students' grades are related to lower odds of suicidal behaviors, but studies on other indicators of academic performance are more limited, specially in middle income countries. Data from 28,519 middle and high school students selected with multistage clustered sampling in the Mexican National Survey of Student's Drug Use. Using a self-administered questionnaire, lifetime suicidal attempt and four indicators of academic performance were assessed: age inconsistency with grade level, not being a student in the last year, perceived academic performance and number of failed courses. Multiple logistic regression models were used to control for sociodemographic and school characteristics. The lifetime prevalence of attempted suicide was 3.0% for middle school students and 4.2% for high school students. Among middle school students, statistically adjusted significant associations of suicide attempt with academic performance indicators were: not being a student the year before, worse self-perceived performance and a higher number of failed courses; among high school students, predictors were failed courses and self-perceived academic performance, with ORs of 1.65 and 1.96 for the categories of good and fair/poor respectively, compared to those who reported very good performance. Self-perceived academic performance was the main indicator for suicide in both school levels. Suicide prevention efforts in Mexico's schools should include asking students about the perception they have about their own academic performance.

  20. 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

  1. Simultaneous determination and stability studies of linezolid, meropenem and vancomycin in bacterial growth medium by high-performance liquid chromatography.

    PubMed

    Wicha, Sebastian G; Kloft, Charlotte

    2016-08-15

    For pharmacokinetic/pharmacodynamic (PK/PD) assessment of antibiotics combinations in in vitro infection models, accurate and precise quantification of drug concentrations in bacterial growth medium is crucial for derivation of valid PK/PD relationships. We aimed to (i) develop a high-performance liquid chromatography (HPLC) assay to simultaneously quantify linezolid (LZD), vancomycin (VAN) and meropenem (MER), as typical components of broad-spectrum antibiotic combination therapy, in bacterial growth medium cation-adjusted Mueller-Hinton broth (CaMHB) and (ii) determine the stability profiles of LZD, VAN and MER under conditions in in vitro infection models. To separate sample matrix components, the final method comprised the pretreatment of 100μL sample with 400μL methanol, the evaporation of supernatant and its reconstitution in water. A low sample volume of 2μL processed sample was injected onto an Accucore C-18 column (2.6μm, 100×2.1mm) coupled to a Dionex Ultimate 3000 HPLC+ system. UV detection at 251, 240 and 302nm allowed quantification limits of 0.5, 2 and 0.5μg/mL for LZD, VAN and MER, respectively. The assay was successfully validated according to the relevant EMA guideline. The rapid method (14min) was successfully applied to quantify significant degradation of LZD, VAN and MER in in vitro infection models: LZD was stable, VAN degraded to 90.6% and MER to 62.9% within 24h compared to t=0 in CaMHB at 37°C, which should be considered when deriving PK/PD relationships in in vitro infection models. Inclusion of further antibiotics into the flexible gradient-based HPLC assay seems promising. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Predictive validity of pre-admission assessments on medical student performance

    PubMed Central

    Dabaliz, Al-Awwab; Kaadan, Samy; Dabbagh, M. Marwan; Barakat, Abdulaziz; Shareef, Mohammad Abrar; Al-Tannir, Mohamad; Obeidat, Akef

    2017-01-01

    Objectives To examine the predictive validity of pre-admission variables on students’ performance in a medical school in Saudi Arabia.  Methods In this retrospective study, we collected admission and college performance data for 737 students in preclinical and clinical years. Data included high school scores and other standardized test scores, such as those of the National Achievement Test and the General Aptitude Test. Additionally, we included the scores of the Test of English as a Foreign Language (TOEFL) and the International English Language Testing System (IELTS) exams. Those datasets were then compared with college performance indicators, namely the cumulative Grade Point Average (cGPA) and progress test, using multivariate linear regression analysis. Results In preclinical years, both the National Achievement Test (p=0.04, B=0.08) and TOEFL (p=0.017, B=0.01) scores were positive predictors of cGPA, whereas the General Aptitude Test (p=0.048, B=-0.05) negatively predicted cGPA. Moreover, none of the pre-admission variables were predictive of progress test performance in the same group. On the other hand, none of the pre-admission variables were predictive of cGPA in clinical years. Overall, cGPA strongly predict-ed students’ progress test performance (p<0.001 and B=19.02). Conclusions Only the National Achievement Test and TOEFL significantly predicted performance in preclinical years. However, these variables do not predict progress test performance, meaning that they do not predict the functional knowledge reflected in the progress test. We report various strengths and deficiencies in the current medical college admission criteria, and call for employing more sensitive and valid ones that predict student performance and functional knowledge, especially in the clinical years. PMID:29176032

  3. Ternary blends containing demercurated lighting phosphor and MSWI fly ash as high-performance binders for stabilizing and recycling electroplating sludge.

    PubMed

    Huang, Wu-Jang; Wu, Chia-Teng; Wu, Chang-En; Hsieh, Lin-Huey; Li, Chang-Chien; Lain, Chi-Yuan; Chu, Wei

    2008-08-15

    This paper describes the solidification and stabilization of electroplating sludge treated with a high-performance binder made from portland type-I cement, municipal solid waste incineration fly ash, and lighting phosphor powder (called as cement-fly ash-phosphor binder, CFP). The highest 28-day unconfined compressive strength of the CFP-treated paste was 816 kg/cm(2) at a ratio of cement to fly ash to lighting phosphor powder of 90:5:5; the strength of this composition also fulfilled the requirement of a high-strength concrete (>460 kg/cm(2) at 28 days). The CFP-stabilized sludge paste samples passed the Taiwanese EPA toxicity characteristic leaching procedure test and, therefore, could be used either as a building material or as a controlled low-strength material, depending on the sludge-to-CFP binder ratio.

  4. Simultaneous, stability indicating, HPLC-DAD determination of guaifenesin and methyl and propyl-parabens in cough syrup.

    PubMed

    Grosa, Giorgio; Del Grosso, Erika; Russo, Roberta; Allegrone, Gianna

    2006-06-07

    A stability indicating high performance liquid chromatography procedure has been developed for the simultaneous determination of guaifenesin (GUA), methyl p-hydroxybenzoate (MHB) and propyl p-hydroxybenzoate (PHB) in a commercial cough syrup dosage form. The method was specific and stability indicating as chromatographic conditions were selected to provide adequate separation of GUA, MHB and PHB from the putative degradation products guaiacol (GUAI) and p-hydroxybenzoic acid (HBA) as well as from excipients. The isocratic separation and quantitation were achieved within 17 min on a 150-mm column with an ether-linked phenyl stationary phase and a hydrophilic endcapping. The mobile phase was constituted of eluant A: aqueous phosphate buffer (pH 3.0, 10 mM)/acetonitrile 25/75 (v/v) and eluant B:methanol; the A:B ratio was 85:15 (v/v) with a flow rate 1 ml min-1 and detection of analytes at 254 and 276 nm. The method showed good linearity for the GUA-MHB-PHB mixture in the 95-285, 4-12, and 1-3 microg ml-1 ranges, respectively, being all the square of the correlation coefficients greater than 0.999. The interday R.S.D.s were 1.17, 1.14, and 0.91%, for GUA, MHB, and PHP, respectively. The method demonstrated also to be accurate; indeed the average recoveries, at 100% of the target assay concentration, were 100.5, 100.3, and 100.7% with relative standard deviations of 0.8, 0.7, and 0.4% for GUA, MHB, and PHB, respectively, from laboratory prepared samples. The applicability of the method was evaluated in commercial dosage form analysis as well as in stability studies.

  5. 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.

  6. Stability Indicating HPLC Method for Simultaneous Determination of Mephenesin and Diclofenac Diethylamine

    PubMed Central

    Mulgund, S. V.; Phoujdar, M. S.; Londhe, S. V.; Mallade, P. S.; Kulkarni, T. S.; Deshpande, A. S.; Jain, K. S.

    2009-01-01

    A simple, specific, accurate and stability-indicating reversed phase high performance liquid chromatographic method was developed for the simultaneous determination of mephenesin and diclofenac diethylamine, using a Spheri-5-RP-18 column and a mobile phase composed of methanol: water (70:30, v/v), pH 3.0 adjusted with o-phosphoric acid. The retention times of mephenesin and diclofenac diethylamine were found to be 3.9 min and 14.5 min, respectively. Linearity was established for mephenesin and diclofenac diethylamine in the range of 50-300 μg/ml and 10-60 μg/ml, respectively. The percentage recoveries of mephenesin and diclofenac diethylamine were found to be in the range of 99.06-100.60% and 98.95-99.98%, respectively. Both the drugs were subjected to acid, alkali and neutral hydrolysis, oxidation, dry heat, photolytic and UV degradation. The degradation studies indicated, mephenesin to be susceptible to neutral hydrolysis, while diclofenac diethylamine showed degradation in acid, H2O2, photolytic and in presence of UV radiation. The degradation products of diclofenac diethylamine in acidic and photolytic conditions were well resolved from the pure drug with significant differences in their retention time values. This method can be successfully employed for simultaneous quantitative analysis of mephenesin and diclofenac diethylamine in bulk drugs and formulations. PMID:20177453

  7. Use of the color trails test as an embedded measure of performance validity.

    PubMed

    Henry, George K; Algina, James

    2013-01-01

    One hundred personal injury litigants and disability claimants referred for a forensic neuropsychological evaluation were administered both portions of the Color Trails Test (CTT) as part of a more comprehensive battery of standardized tests. Subjects who failed two or more free-standing tests of cognitive performance validity formed the Failed Performance Validity (FPV) group, while subjects who passed all free-standing performance validity measures were assigned to the Passed Performance Validity (PPV) group. A cutscore of ≥45 seconds to complete Color Trails 1 (CT1) was associated with a classification accuracy of 78%, good sensitivity (66%) and high specificity (90%), while a cutscore of ≥84 seconds to complete Color Trails 2 (CT2) was associated with a classification accuracy of 82%, good sensitivity (74%) and high specificity (90%). A CT1 cutscore of ≥58 seconds, and a CT2 cutscore ≥100 seconds was associated with 100% positive predictive power at base rates from 20 to 50%.

  8. Taking the Next Step: Combining Incrementally Valid Indicators to Improve Recidivism Prediction

    ERIC Educational Resources Information Center

    Walters, Glenn D.

    2011-01-01

    The possibility of combining indicators to improve recidivism prediction was evaluated in a sample of released federal prisoners randomly divided into a derivation subsample (n = 550) and a cross-validation subsample (n = 551). Five incrementally valid indicators were selected from five domains: demographic (age), historical (prior convictions),…

  9. 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.

  10. Key performance indicators to benchmark hospital information systems - a delphi study.

    PubMed

    Hübner-Bloder, G; Ammenwerth, E

    2009-01-01

    To identify the key performance indicators for hospital information systems (HIS) that can be used for HIS benchmarking. A Delphi survey with one qualitative and two quantitative rounds. Forty-four HIS experts from health care IT practice and academia participated in all three rounds. Seventy-seven performance indicators were identified and organized into eight categories: technical quality, software quality, architecture and interface quality, IT vendor quality, IT support and IT department quality, workflow support quality, IT outcome quality, and IT costs. The highest ranked indicators are related to clinical workflow support and user satisfaction. Isolated technical indicators or cost indicators were not seen as useful. The experts favored an interdisciplinary group of all the stakeholders, led by hospital management, to conduct the HIS benchmarking. They proposed benchmarking activities both in regular (annual) intervals as well as at defined events (for example after IT introduction). Most of the experts stated that in their institutions no HIS benchmarking activities are being performed at the moment. In the context of IT governance, IT benchmarking is gaining importance in the healthcare area. The found indicators reflect the view of health care IT professionals and researchers. Research is needed to further validate and operationalize key performance indicators, to provide an IT benchmarking framework, and to provide open repositories for a comparison of the HIS benchmarks of different hospitals.

  11. 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.

  12. 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.

  13. Development and validation of a high-fidelity phonomicrosurgical trainer.

    PubMed

    Klein, Adam M; Gross, Jennifer

    2017-04-01

    To validate the use of a high-fidelity phonomicrosurgical trainer. A high-fidelity phonomicrosurgical trainer, based on a previously validated model by Contag et al., 1 was designed with multilayered vocal folds that more closely mimic the consistency of true vocal folds, containing intracordal lesions to practice phonomicrosurgical removal. A training module was developed to simulate the true phonomicrosurgical experience. A validation study with novice and expert surgeons was conducted. Novices and experts were instructed to remove the lesion from the synthetic vocal folds, and novices were given four training trials. Performances were measured by the amount of time spent and tissue injury (microflap, superficial, deep) to the vocal fold. An independent Student t test and Fisher exact tests were used to compare subjects. A matched-paired t test and Wilcoxon signed rank tests were used to compare novice performance on the first and fourth trials and assess for improvement. Experts completed the excision with less total errors than novices (P = .004) and made less injury to the microflap (P = .05) and superficial tissue (P = .003). Novices improved their performance with training, making less total errors (P = .002) and superficial tissue injuries (P = .02) and spending less time for removal (P = .002) after several practice trials. This high-fidelity phonomicrosurgical trainer has been validated for novice surgeons. It can distinguish between experts and novices; and after training, it helped to improve novice performance. N/A. Laryngoscope, 127:888-893, 2017. © 2016 The American Laryngological, Rhinological and Otological Society, Inc.

  14. 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)…

  15. Stability of Materials in High Temperature Water Vapor: SOFC Applications

    NASA Technical Reports Server (NTRS)

    Opila, E. J.; Jacobson, N. S.

    2010-01-01

    Solid oxide fuel cell material systems require long term stability in environments containing high-temperature water vapor. Many materials in fuel cell systems react with high-temperature water vapor to form volatile hydroxides which can degrade cell performance. In this paper, experimental methods to characterize these volatility reactions including the transpiration technique, thermogravimetric analysis, and high pressure mass spectrometry are reviewed. Experimentally determined data for chromia, silica, and alumina volatility are presented. In addition, data from the literature for the stability of other materials important in fuel cell systems are reviewed. Finally, methods for predicting material recession due to volatilization reactions are described.

  16. 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.

  17. Temporal Stability and Convergent Validity of the Behavior Assessment System for Children.

    ERIC Educational Resources Information Center

    Merydith, Scott P.

    2001-01-01

    Assesses the temporal stability and convergent validity of the Behavioral Assessment System for Children (BASC). Teachers and parents rated kindergarten and first-grade students using BASC. Teachers were more stable in rating children's externalizing behaviors and attention problems. Discusses results in terms of the accuracy of information…

  18. 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.

  19. Indicators of patients with major depressive disorder in need of highly specialized care: A systematic review.

    PubMed

    van Krugten, Frédérique C W; Kaddouri, Meriam; Goorden, Maartje; van Balkom, Anton J L M; Bockting, Claudi L H; Peeters, Frenk P M L; Hakkaart-van Roijen, Leona

    2017-01-01

    Early identification of patients with major depressive disorder (MDD) that cannot be managed by secondary mental health services and who require highly specialized mental healthcare could enhance need-based patient stratification. This, in turn, may reduce the number of treatment steps needed to achieve and sustain an adequate treatment response. The development of a valid tool to identify patients with MDD in need of highly specialized care is hampered by the lack of a comprehensive understanding of indicators that distinguish patients with and without a need for highly specialized MDD care. The aim of this study, therefore, was to systematically review studies on indicators of patients with MDD likely in need of highly specialized care. A structured literature search was performed on the PubMed and PsycINFO databases following PRISMA guidelines. Two reviewers independently assessed study eligibility and determined the quality of the identified studies. Three reviewers independently executed data extraction by using a pre-piloted, standardized extraction form. The resulting indicators were grouped by topical similarity, creating a concise summary of the findings. The systematic search of all databases yielded a total of 7,360 references, of which sixteen were eligible for inclusion. The sixteen papers yielded a total of 48 unique indicators. Overall, a more pronounced depression severity, a younger age of onset, a history of prior poor treatment response, psychiatric comorbidity, somatic comorbidity, childhood trauma, psychosocial impairment, older age, and a socioeconomically disadvantaged status were found to be associated with proxies of need for highly specialized MDD care. Several indicators are associated with the need for highly specialized MDD care. These indicators provide easily measurable factors that may serve as a starting point for the development of a valid tool to identify patients with MDD in need of highly specialized care.

  20. Indicators of patients with major depressive disorder in need of highly specialized care: A systematic review

    PubMed Central

    Kaddouri, Meriam; Goorden, Maartje; van Balkom, Anton J. L. M.; Bockting, Claudi L. H.; Peeters, Frenk P. M. L.; Hakkaart-van Roijen, Leona

    2017-01-01

    Objectives Early identification of patients with major depressive disorder (MDD) that cannot be managed by secondary mental health services and who require highly specialized mental healthcare could enhance need-based patient stratification. This, in turn, may reduce the number of treatment steps needed to achieve and sustain an adequate treatment response. The development of a valid tool to identify patients with MDD in need of highly specialized care is hampered by the lack of a comprehensive understanding of indicators that distinguish patients with and without a need for highly specialized MDD care. The aim of this study, therefore, was to systematically review studies on indicators of patients with MDD likely in need of highly specialized care. Methods A structured literature search was performed on the PubMed and PsycINFO databases following PRISMA guidelines. Two reviewers independently assessed study eligibility and determined the quality of the identified studies. Three reviewers independently executed data extraction by using a pre-piloted, standardized extraction form. The resulting indicators were grouped by topical similarity, creating a concise summary of the findings. Results The systematic search of all databases yielded a total of 7,360 references, of which sixteen were eligible for inclusion. The sixteen papers yielded a total of 48 unique indicators. Overall, a more pronounced depression severity, a younger age of onset, a history of prior poor treatment response, psychiatric comorbidity, somatic comorbidity, childhood trauma, psychosocial impairment, older age, and a socioeconomically disadvantaged status were found to be associated with proxies of need for highly specialized MDD care. Conclusions Several indicators are associated with the need for highly specialized MDD care. These indicators provide easily measurable factors that may serve as a starting point for the development of a valid tool to identify patients with MDD in need of highly

  1. Stability and performance of notch filter control for unbalance response

    NASA Technical Reports Server (NTRS)

    Knospe, C. R.

    1992-01-01

    Many current applications of magnetic bearings for rotating machinery employ notch filters in the feedback control loop to reduce the synchronous forces transmitted through the bearings. The capabilities and limitations of notch filter control are investigated. First, a rigid rotor is examined with some classical root locus techniques. Notch filter control is shown to result in conditional stability whenever complete synchronous attenuation is required. Next, a nondimensional parametric symmetric flexible three mass rotor model is constructed. An examination of this model for several test cases illustrates the limited attenuation possible with notch filters at and near the system critical speeds when the bearing damping is low. The notch filter's alteration of the feedback loop is shown to cause stability problems which limits performance. Poor transient response may also result. A high speed compressor is then examined as a candidate for notch filter control. A collocated 22 mass station model with lead-lag control is used. The analysis confirms the reduction in stability robustness that can occur with notch filter control. It is concluded that other methods of synchronous vibration control yield greater performance without compromising stability.

  2. 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.

  3. 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.

  4. 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.

  5. Performance Indicators in Spine Surgery.

    PubMed

    St-Pierre, Godefroy Hardy; Yang, Michael H; Bourget-Murray, Jonathan; Thomas, Ken C; Hurlbert, Robin John; Matthes, Nikolas

    2018-02-15

    Systematic review. To elucidate how performance indicators are currently used in spine surgery. The Patient Protection and Affordable Care Act has given significant traction to the idea that healthcare must provide value to the patient through the introduction of hospital value-based purchasing. The key to implementing this new paradigm is to measure this value notably through performance indicators. MEDLINE, CINAHL Plus, EMBASE, and Google Scholar were searched for studies reporting the use of performance indicators specific to spine surgery. We followed the Prisma-P methodology for a systematic review for entries from January 1980 to July 2016. All full text articles were then reviewed to identify any measure of performance published within the article. This measure was then examined as per the three criteria of established standard, exclusion/risk adjustment, and benchmarking to determine if it constituted a performance indicator. The initial search yielded 85 results among which two relevant studies were identified. The extended search gave a total of 865 citations across databases among which 15 new articles were identified. The grey literature search provided five additional reports which in turn led to six additional articles. A total of 27 full text articles and reports were retrieved and reviewed. We were unable to identify performance indicators. The articles presenting a measure of performance were organized based on how many criteria they lacked. We further examined the next steps to be taken to craft the first performance indicator in spine surgery. The science of performance measurement applied to spine surgery is still in its infancy. Current outcome metrics used in clinical settings require refinement to become performance indicators. Current registry work is providing the necessary foundation, but requires benchmarking to truly measure performance. 1.

  6. A Study of the Validity of Language Usage as an Indicator of Ethnic Identification.

    ERIC Educational Resources Information Center

    Patella, Victoria Morrow

    In determining whether Spanish usage is a valid indicator of ethnic identification, 669 Texas high school sophomores (3 Negroes, 70 Anglos, and 596 Mexican Americans) were interviewed. Mexican American respondents were then isolated on the basis of response to 4 questions, and their responses regarding family were grouped under 2 headings: (1)…

  7. Identification and selection of Environmental Performance Indicators for sustainable port development.

    PubMed

    Puig, Martí; Wooldridge, Chris; Darbra, Rosa Mari

    2014-04-15

    In this paper an identification and selection of Environmental Performance Indicators (EPIs) in port areas has been conducted. A comprehensive inventory of existing EPIs in use in the seaport sector has been identified for monitoring performance of operational (e.g. dust, noise, dredging, and waste), managerial (e.g. certification, compliance, and complaints) and environmental condition (e.g. air, water, sediment and ecosystems). These indicators have been filtered against specific criteria and have been assessed and evaluated by port stakeholders in order to obtain a final set of indicators suitable to be implemented at EU level. A user friendly tool has been developed specifically to assist port authorities in calculating and reporting the proposed indicators. This study has drawn on major research projects to blend academic research with input from marine professionals in order to identify, select, evaluate and validate EPIs that are acceptable and feasible to the sector, and practicable in their application and implementation. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. Reliability and validity of the Computerized Comprehension Task (CCT): data from American English and Mexican Spanish infants*

    PubMed Central

    FRIEND, MARGARET; KEPLINGER, MELANIE

    2017-01-01

    Early language comprehension may be one of the most important predictors of developmental risk. The need for performance-based assessment is predicated on limitations identified in the exclusive use of parent report and on the need for a performance measure with which to assess the convergent validity of parent report of comprehension. Child performance data require the development of procedures to facilitate infant attention and compliance. Forty infants (20 at 1;4 and 20 at 1;8) acquiring English completed a standard picture book task and the same task was administered on a touch-sensitive screen. The computerized task significantly improved task attention, compliance and performance. Reliability was high, indicating that infants were not responding randomly. Convergent validity with parent report and 4-month stability was substantial. Preliminary data extending this approach to Mexican-Spanish are presented. Results are discussed in terms of the promise of this technique for clinical and research settings and the potential influences of cultural factors on performance. PMID:18300430

  9. 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.

  10. 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.

  11. 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.

  12. The temporal stability and predictive validity of pupils' causal attributions for difficult classroom behaviour.

    PubMed

    Lambert, Nathan; Miller, Andy

    2010-12-01

    Recent studies have investigated the causal attributions for difficult pupil behaviour made by teachers, pupils, and parents but none have investigated the temporal stability or predictive validity of these attributions. This study examines the causal attributions made for difficult classroom behaviour by students on two occasions 30 months apart. The longitudinal stability of these attributions is considered as is the predictive validity of the first set of attributions in relation to teachers' later judgments about individual students' behaviour. Two hundred and seventeen secondary school age pupils (114 males, 103 females) provided data on the two occasions. Teachers also rated each student's behaviour at the two times. A questionnaire listing 63 possible causes of classroom misbehaviour was delivered to pupils firstly when they were in Year 7 (aged 11-12) and then again, 30 months later. Responses were analysed through exploratory factor analysis (EFA). Additionally, teachers were asked to rate the standard of behaviour of each of the students on the two occasions. EFA of the Years 7 and 10 data indicated that pupils' attributions yielded broadly similar five-factor models with the perceived relative importance of these factors remaining the same. Analysis also revealed a predictive relationship between pupils' attributions regarding the factor named culture of misbehaviour in Year 7, and teachers' judgments of their standard of behaviour in Year 10. The present study suggests that young adolescents' causal attributions for difficult classroom behaviour remain stable over time and are predictive of teachers' later judgments about their behaviour.

  13. 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.

  14. 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.

  15. Overall Key Performance Indicator to Optimizing Operation of High-Pressure Homogenizers for a Reliable Quantification of Intracellular Components in Pichia pastoris.

    PubMed

    Garcia-Ortega, Xavier; Reyes, Cecilia; Montesinos, José Luis; Valero, Francisco

    2015-01-01

    The most commonly used cell disruption procedures may present lack of reproducibility, which introduces significant errors in the quantification of intracellular components. In this work, an approach consisting in the definition of an overall key performance indicator (KPI) was implemented for a lab scale high-pressure homogenizer (HPH) in order to determine the disruption settings that allow the reliable quantification of a wide sort of intracellular components. This innovative KPI was based on the combination of three independent reporting indicators: decrease of absorbance, release of total protein, and release of alkaline phosphatase activity. The yeast Pichia pastoris growing on methanol was selected as model microorganism due to it presents an important widening of the cell wall needing more severe methods and operating conditions than Escherichia coli and Saccharomyces cerevisiae. From the outcome of the reporting indicators, the cell disruption efficiency achieved using HPH was about fourfold higher than other lab standard cell disruption methodologies, such bead milling cell permeabilization. This approach was also applied to a pilot plant scale HPH validating the methodology in a scale-up of the disruption process. This innovative non-complex approach developed to evaluate the efficacy of a disruption procedure or equipment can be easily applied to optimize the most common disruption processes, in order to reach not only reliable quantification but also recovery of intracellular components from cell factories of interest.

  16. Overall Key Performance Indicator to Optimizing Operation of High-Pressure Homogenizers for a Reliable Quantification of Intracellular Components in Pichia pastoris

    PubMed Central

    Garcia-Ortega, Xavier; Reyes, Cecilia; Montesinos, José Luis; Valero, Francisco

    2015-01-01

    The most commonly used cell disruption procedures may present lack of reproducibility, which introduces significant errors in the quantification of intracellular components. In this work, an approach consisting in the definition of an overall key performance indicator (KPI) was implemented for a lab scale high-pressure homogenizer (HPH) in order to determine the disruption settings that allow the reliable quantification of a wide sort of intracellular components. This innovative KPI was based on the combination of three independent reporting indicators: decrease of absorbance, release of total protein, and release of alkaline phosphatase activity. The yeast Pichia pastoris growing on methanol was selected as model microorganism due to it presents an important widening of the cell wall needing more severe methods and operating conditions than Escherichia coli and Saccharomyces cerevisiae. From the outcome of the reporting indicators, the cell disruption efficiency achieved using HPH was about fourfold higher than other lab standard cell disruption methodologies, such bead milling cell permeabilization. This approach was also applied to a pilot plant scale HPH validating the methodology in a scale-up of the disruption process. This innovative non-complex approach developed to evaluate the efficacy of a disruption procedure or equipment can be easily applied to optimize the most common disruption processes, in order to reach not only reliable quantification but also recovery of intracellular components from cell factories of interest. PMID:26284241

  17. Quality Management and Key Performance Indicators in Oncologic Esophageal Surgery.

    PubMed

    Gockel, Ines; Ahlbrand, Constantin Johannes; Arras, Michael; Schreiber, Elke Maria; Lang, Hauke

    2015-12-01

    Ranking systems and comparisons of quality and performance indicators will be of increasing relevance for complex "high-risk" procedures such as esophageal cancer surgery. The identification of evidence-based standards relevant for key performance indicators in esophageal surgery is essential for establishing monitoring systems and furthermore a requirement to enhance treatment quality. In the course of this review, we analyze the key performance indicators case volume, radicality of resection, and postoperative morbidity and mortality, leading to continuous quality improvement. Ranking systems established on this basis will gain increased relevance in highly complex procedures within the national and international comparison and furthermore improve the treatment of patients with esophageal carcinoma.

  18. Performance indicators of work activity.

    PubMed

    Lahoz, Manoela de Assis; Camarotto, João Alberto

    2012-01-01

    The measurement of performance is a current topic in the management of people in companies, used as a parameter of effectiveness of processes and operations of production. The methods and models of the indicators of current use in the production have concentrated in the assessment of people's performance as determinative resource of the organizational success in the search for the competitiveness. Associated with the classic indicators of performance assessment of the production proceeding, other indicators are used in the assessment of risks and hazards, however with methods focused in the tasks, without connection with the real work activity. The present article explores literature on the models of performance measurement in use in companies and a field research to understand how companies interpret and use indicators that relate health and work, to direct future studies on the subject. Regarding the literature review, one can see that health indicators can be basically divided into two major groups: the legal and managerial indicators. When conducting case studies, it can be realized that companies do not have precisely the concept of health indicator, or were unable to define which of the indicators could be considered indicators of health, considering that absenteeism was the indicator mentioned by the four companies.

  19. Synthesis of high-temperature viscosity stabilizer used in drilling fluid

    NASA Astrophysics Data System (ADS)

    Zhang, Yanna; Luo, Huaidong; Shi, Libao; Huang, Hongjun

    2018-02-01

    Abstract For a well performance drilling fluid, when it operates in deep wells under high temperature, the most important property required is the thermal stability. The drilling fluid properties under high temperature can be controlled by proper selection of viscosity stabilizer, which can capture oxygen to protect polymer agent in the drilling fluid. In this paper a viscosity stabilizer PB-854 is described, which was synthesized by 4-phenoxybutyl bromide, paraformaldehyde, and phloroglucinol using etherification method and condensation reaction. We studied the effect of catalyst dosage, temperature, time, and stirring rate on the synthetic yield. Under this condition: molar ratio of 2-tert-Butylphenol, paraformaldehyde and phloroglucinol of 2:1:2.5, reacting temperature of 100 °C, stirring rate of 100 r min-1, and mass content of catalyst of 15 %, char yield of 5-bromine-3-tert-butyl salicylaldehyde reached 86 %. Under this condition: molar ratio of 5-bromine-3-tert-butyl salicylaldehyde and phloroglucinol of 4, reacting temperature of 60 °C, reacting time of 30 min, volume content of sulphuric acid of 80 %, char yield of the target product viscosity stabilizer PB-854 is 86%. Finally, in this paper, infrared spectroscopy is adopted to analyse the structure of the synthetic product PB-854.The improvement in the stability of drilling fluid was further shown after adding the viscosity stabilizer in the common polymer drilling fluid under high temperature conditions of 120 °C ˜ 180 °C. The results show significant change in terms of fluid stability in the presence of this new stabilizer as it provides better stability.

  20. Assessing the validity and reliability of three indicators self-reported on the pregnancy risk assessment monitoring system survey.

    PubMed

    Ahluwalia, Indu B; Helms, Kristen; Morrow, Brian

    2013-01-01

    We investigated the reliability and validity of three self-reported indicators from the Pregnancy Risk Assessment Monitoring System (PRAMS) survey. We used 2008 PRAMS (n=15,646) data from 12 states that had implemented the 2003 revised U.S. Certificate of Live Birth. We estimated reliability by kappa coefficient and validity by sensitivity and specificity using the birth certificate data as the reference for the following: prenatal participation in the Special Supplemental Nutrition Program for Women, Infants, and Children (WIC); Medicaid payment for delivery; and breastfeeding initiation. These indicators were examined across several demographic subgroups. The reliability was high for all three measures: 0.81 for WIC participation, 0.67 for Medicaid payment of delivery, and 0.72 for breastfeeding initiation. The validity of PRAMS indicators was also high: WIC participation (sensitivity = 90.8%, specificity = 90.6%), Medicaid payment for delivery (sensitivity = 82.4%, specificity = 85.6%), and breastfeeding initiation (sensitivity = 94.3%, specificity = 76.0%). The prevalence estimates were higher on PRAMS than the birth certificate for each of the indicators except Medicaid-paid delivery among non-Hispanic black women. Kappa values within most subgroups remained in the moderate range (0.40-0.80). Sensitivity and specificity values were lower for Hispanic women who responded to the PRAMS survey in Spanish and for breastfeeding initiation among women who delivered very low birthweight and very preterm infants. The validity and reliability of the PRAMS data for measures assessed were high. Our findings support the use of PRAMS data for epidemiological surveillance, research, and planning.

  1. Novel LLM series high density energy materials: Synthesis, characterization, and thermal stability

    NASA Astrophysics Data System (ADS)

    Pagoria, Philip; Zhang, Maoxi; Tsyshevskiy, Roman; Kuklja, Maija

    Novel high density energy materials must satisfy specific requirements, such as an increased performance, reliably high stability to external stimuli, cost-efficiency and ease of synthesis, be environmentally benign, and be safe for handling and transportation. During the last decade, the attention of researchers has drifted from widely used nitroester-, nitramine-, and nitroaromatic-based explosives to nitrogen-rich heterocyclic compounds. Good thermal stability, the low melting point, high density, and moderate sensitivity make heterocycle materials attractive candidates for use as oxidizers in rocket propellants and fuels, secondary explosives, and possibly as melt-castable ingredients of high explosive formulations. In this report, the synthesis, characterization, and results of quantum-chemical DFT study of thermal stability of LLM-191, LLM-192 and LLM-200 high density energy materials are presented. Work performed under the auspices of the DOE by the LLNL (Contract DE-AC52-07NA27344). This research is supported in part by ONR (Grant N00014-12-1-0529) and NSF. We used NSF XSEDE (Grant DMR-130077) and DOE NERSC (Contract DE-AC02-05CH11231) resources.

  2. 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.

  3. A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations

    PubMed Central

    Badr, Jihan M.

    2013-01-01

    Background: Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. Materials and Method: In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Harmonization (ICH) guidelines. The method employed thin layer chromatography aluminum sheets precoated with silica gel as the stationary phase and the mobile phase consisted of chloroform:methanol:ammonia (97:3:0.2), which gave compact bands of yohimbine hydrochloride. Results: Linear regression data for the calibration curves of standard yohimbine hydrochloride showed a good linear relationship over a concentration range of 80–1000 ng/spot with respect to the area and correlation coefficient (R2) was 0.9965. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 5 and 40 ng/spot, respectively. The proposed method efficiently separated yohimbine hydrochloride from other components even in complex mixture containing powdered plants. The amount of yohimbine hydrochloride ranged from 2.3 to 5.2 mg/tablet or capsule in preparations containing the pure alkaloid, while it varied from zero (0) to 1.5–1.8 mg/capsule in dietary supplements containing powdered yohimbe bark. Conclusion: We concluded that this method employing high performance thin layer chromatography (HPTLC) in quantitative determination of yohimbine hydrochloride in pharmaceutical preparations is efficient, simple, accurate, and validated. PMID:23661986

  4. A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations.

    PubMed

    Badr, Jihan M

    2013-01-01

    Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Harmonization (ICH) guidelines. The method employed thin layer chromatography aluminum sheets precoated with silica gel as the stationary phase and the mobile phase consisted of chloroform:methanol:ammonia (97:3:0.2), which gave compact bands of yohimbine hydrochloride. Linear regression data for the calibration curves of standard yohimbine hydrochloride showed a good linear relationship over a concentration range of 80-1000 ng/spot with respect to the area and correlation coefficient (R(2)) was 0.9965. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 5 and 40 ng/spot, respectively. The proposed method efficiently separated yohimbine hydrochloride from other components even in complex mixture containing powdered plants. The amount of yohimbine hydrochloride ranged from 2.3 to 5.2 mg/tablet or capsule in preparations containing the pure alkaloid, while it varied from zero (0) to 1.5-1.8 mg/capsule in dietary supplements containing powdered yohimbe bark. We concluded that this method employing high performance thin layer chromatography (HPTLC) in quantitative determination of yohimbine hydrochloride in pharmaceutical preparations is efficient, simple, accurate, and validated.

  5. Stability and maturity of biowaste composts derived by small municipalities: Correlation among physical, chemical and biological indices.

    PubMed

    Oviedo-Ocaña, E R; Torres-Lozada, P; Marmolejo-Rebellon, L F; Hoyos, L V; Gonzales, S; Barrena, R; Komilis, D; Sanchez, A

    2015-10-01

    Stability and maturity are important criteria to guarantee the quality of a compost that is applied to agriculture or used as amendment in degraded soils. Although different techniques exist to evaluate stability and maturity, the application of laboratory tests in municipalities in developing countries can be limited due to cost and application complexities. In the composting facilities of such places, some classical low cost on-site tests to monitor the composting process are usually implemented; however, such tests do not necessarily clearly identify conditions of stability and maturity. In this article, we have applied and compared results of stability and maturity tests that can be easily employed on site (i.e. temperature, pH, moisture, electrical conductivity [EC], odor and color), and of tests that require more complex laboratory techniques (volatile solids, C/N ratio, self-heating, respirometric index, germination index [GI]). The evaluation of the above was performed in the field scale using 2 piles of biowaste applied compost. The monitoring period was from day 70 to day 190 of the process. Results showed that the low-cost tests traditionally employed to monitor the composting process on-site, such as temperature, color and moisture, do not provide consistent determinations with the more complex laboratory tests used to assess stability (e.g. respiration index, self-heating, volatile solids). In the case of maturity tests (GI, pH, EC), both the on-site tests (pH, EC) and the laboratory test (GI) provided consistent results. Although, stability was indicated for most of the samples, the maturity tests indicated that products were consistently immature. Thus, a stable product is not necessarily mature. Conclusively, the decision on the quality of the compost in the installations located in developing countries requires the simultaneous use of a combination of tests that are performed both in the laboratory and on-site. Copyright © 2015 Elsevier Ltd. All

  6. 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

  7. A validated high-performance liquid chromatographic method for the determination of moclobemide and its two metabolites in human plasma and application to pharmacokinetic studies.

    PubMed

    Plenis, Alina; Chmielewska, Aleksandra; Konieczna, Lucyna; Lamparczyk, Henryk

    2007-09-01

    A rapid and sensitive reversed-phase high-performance liquid chromatographic method (RP-HPLC) with ultraviolet detection has been developed for the determination of moclobemide and its metabolites, p-chloro-N-(-2-morpholinoethyl)benzamide N'-oxide (Ro 12-5637) and p-chloro-N-[2-(3-oxomorpholino)ethyl]-benzamide (Ro 12-8095), in human plasma. The assay was performed after single liquid-liquid extraction with dichloromethane at alkaline pH using phenacetin as the internal standard. Chromatographic separation was performed on a C(18) column using a mixture of acetonitrile and water (25:75, v/v), adjusted to pH 2.7 with ortho-phosphoric acid, as mobile phase. Spectrophotometric detection was performed at 239 nm. The method has been validated for accuracy, precision, selectivity, linearity, recovery and stability. The quantification limit for moclobemide and Ro 12-8095 was 10 ng/mL, and for Ro 12-5637 was 30 ng/mL. Linearity of the method was confirmed for the range 20-2500 ng/mL for moclobemide (r = 0.9998), 20-1750 ng/mL for Ro 12-8095 (r = 0.9996) and 30-350 ng/mL for Ro 12-5637 (r = 0.9991). Moreover, within-day and between-day precisions and accuracies of the method were established. The described method was successfully applied in pharmacokinetic studies of parent drug and its two metabolites after a single oral administration of 150 mg of moclobemide to 20 healthy volunteers. Copyright (c) 2007 John Wiley & Sons, Ltd.

  8. 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.

  9. Derivation and Cross-Validation of Cutoff Scores for Patients With Schizophrenia Spectrum Disorders on WAIS-IV Digit Span-Based Performance Validity Measures.

    PubMed

    Glassmire, David M; Toofanian Ross, Parnian; Kinney, Dominique I; Nitch, Stephen R

    2016-06-01

    Two studies were conducted to identify and cross-validate cutoff scores on the Wechsler Adult Intelligence Scale-Fourth Edition Digit Span-based embedded performance validity (PV) measures for individuals with schizophrenia spectrum disorders. In Study 1, normative scores were identified on Digit Span-embedded PV measures among a sample of patients (n = 84) with schizophrenia spectrum diagnoses who had no known incentive to perform poorly and who put forth valid effort on external PV tests. Previously identified cutoff scores resulted in unacceptable false positive rates and lower cutoff scores were adopted to maintain specificity levels ≥90%. In Study 2, the revised cutoff scores were cross-validated within a sample of schizophrenia spectrum patients (n = 96) committed as incompetent to stand trial. Performance on Digit Span PV measures was significantly related to Full Scale IQ in both studies, indicating the need to consider the intellectual functioning of examinees with psychotic spectrum disorders when interpreting scores on Digit Span PV measures. © The Author(s) 2015.

  10. Antioxidant effect of thiazolidine molecules in cell culture media improves stability and performance.

    PubMed

    Kuschelewski, Jennifer; Schnellbaecher, Alisa; Pering, Sascha; Wehsling, Maria; Zimmer, Aline

    2017-05-01

    The ability of cell culture media components to generate reactive species as well as their sensitivity to oxidative degradation, affects the overall stability of media and the behavior of cells cultured in vitro. This study investigates the influence of thiazolidine molecules, formed from the condensation between cysteine and alpha-ketoacids, on the stability of these complex mixtures and on the performance of cell culture processes aiming to produce therapeutically relevant monoclonal antibodies. Results presented in this study indicate that 2-methyl-1,3-thiazolidine-2,4-dicarboxylic acid and 2-(2-carboxyethyl)-1,3-thiazolidine-2,4-dicarboxylic acid, obtained by condensation of cysteine with pyruvate or alpha-ketoglutarate, respectively, are able to stabilize cell culture media formulations, in particular redox sensitive molecules like folic acid, thiamine, l-methionine (met) and l-tryptophan (trp). The use of thiazolidine containing feeds in Chinese hamster ovary fed-batch processes showed prolonged culture duration and increased productivity. This enhanced performance was correlated with lower reactive species generation, extracellularly and intracellularly. Moreover, an anti-oxidative response was triggered via the induction of superoxide dismutase and an increase in the total glutathione pool, the major intracellular antioxidant. In total, the results confirm that cells in vitro are not cultured in an oxidant-free environment, a concept that has to be considered when studying the influence of reactive species in human diseases. Furthermore, this study indicates that thiazolidines are an interesting class of antioxidant molecules, capable of increasing cell culture media stability and process performance. © 2017 American Institute of Chemical Engineers Biotechnol. Prog., 33:759-770, 2017. © 2017 American Institute of Chemical Engineers.

  11. Postdivorce Family Stability and Changes in Adolescents' Academic Performance: A Growth-Curve Model

    ERIC Educational Resources Information Center

    Sun, Yongmin; Li, Yuanzhang

    2009-01-01

    Three waves of panel data from 7,897 adolescents in the National Education Longitudinal Studies have been used to investigate whether a stabilized postdivorce family environment benefits adolescents' academic performance trajectories. The analyses indicate that compared with peers who grow up in stable postdivorce families, children of divorce who…

  12. Assessing Temporal Stability for Coarse Scale Satellite Moisture Validation in the Maqu Area, Tibet

    PubMed Central

    Bhatti, Haris Akram; Rientjes, Tom; Verhoef, Wouter; Yaseen, Muhammad

    2013-01-01

    This study evaluates if the temporal stability concept is applicable to a time series of satellite soil moisture images so to extend the common procedure of satellite image validation. The area of study is the Maqu area, which is located in the northeastern part of the Tibetan plateau. The network serves validation purposes of coarse scale (25–50 km) satellite soil moisture products and comprises 20 stations with probes installed at depths of 5, 10, 20, 40, 80 cm. The study period is 2009. The temporal stability concept is applied to all five depths of the soil moisture measuring network and to a time series of satellite-based moisture products from the Advance Microwave Scanning Radiometer (AMSR-E). The in-situ network is also assessed by Pearsons's correlation analysis. Assessments by the temporal stability concept proved to be useful and results suggest that probe measurements at 10 cm depth best match to the satellite observations. The Mean Relative Difference plot for satellite pixels shows that a RMSM pixel can be identified but in our case this pixel does not overlay any in-situ station. Also, the RMSM pixel does not overlay any of the Representative Mean Soil Moisture (RMSM) stations of the five probe depths. Pearson's correlation analysis on in-situ measurements suggests that moisture patterns over time are more persistent than over space. Since this study presents first results on the application of the temporal stability concept to a series of satellite images, we recommend further tests to become more conclusive on effectiveness to broaden the procedure of satellite validation. PMID:23959237

  13. Designing Liquid Rocket Engine Injectors for Performance, Stability, and Cost

    NASA Technical Reports Server (NTRS)

    Westra, Douglas G.; West, Jeffrey S.

    2014-01-01

    NASA is developing the Space Launch System (SLS) for crewed exploration missions beyond low Earth orbit. Marshall Space Flight Center (MSFC) is designing rocket engines for the SLS Advanced Booster (AB) concepts being developed to replace the Shuttle-derived solid rocket boosters. One AB concept uses large, Rocket-Propellant (RP)-fueled engines that pose significant design challenges. The injectors for these engines require high performance and stable operation while still meeting aggressive cost reduction goals for access to space. Historically, combustion stability problems have been a critical issue for such injector designs. Traditional, empirical injector design tools and methodologies, however, lack the ability to reliably predict complex injector dynamics that often lead to combustion stability. Reliance on these tools alone would likely result in an unaffordable test-fail-fix cycle for injector development. Recently at MSFC, a massively parallel computational fluid dynamics (CFD) program was successfully applied in the SLS AB injector design process. High-fidelity reacting flow simulations were conducted for both single-element and seven-element representations of the full-scale injector. Data from the CFD simulations was then used to significantly augment and improve the empirical design tools, resulting in a high-performance, stable injector design.

  14. 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.

  15. [Nurse's competence indicators: linguistic and cultural validation of the Nurse Competence Scale].

    PubMed

    Finotto, Stefano; Cantarelli, William

    2009-01-01

    For some years, the clinical performance of new-graduate nurses, has been a leading topic in international scientific literature. In Italy there are many criticisms to basic education; ever since the basic education moved from the regional schools to the university, the main question that the teachers, the clinical nurses and the nursing managers are asking is whether the level of competence of new-graduates is appropriate to the demands of the world of work. Many criticisms have been addressed to the gap between theory and practice and between education and clinic. In Italy this has stimulated a debate towards a shared definition of competence and especially towards defining indicators that can assess/measure this phenomenon. The purposes of this study are: translating the indicators of Nurse Competence Scale (NCS) in the Italian language and test its validity and reliability; provide a tool for evaluating competence in Italian in order to use it in the context of our country. after a research on the Medline and Cinhal electronic data base, the NCS was identified and submitted to a process of linguistic translation (English-Italian-English) and to a process of validation using the test-retest methodology (test of Wilcoxon), the Intraclass Correlation Coefficient (ICC) and Cronbach's alpha. the evaluation given by nurses in the first administration does not differ significantly with those of the second one. For all sections of the NCS the ICC reports values greater than 0.85. the Nurse Competence Scale appears valid in its Italian version and it might be used to measure the competences of Italian nurses.

  16. Analysis of architect’s performance indicators in project delivery process

    NASA Astrophysics Data System (ADS)

    Marisa, A.

    2018-03-01

    Architect as a professional in the construction industry should possess a good performance in project delivery process. As a design professional, architect has an important role to ensure that the process is well-conducted by delivering a high-quality product for the clients. Thus, analyzing architect’s performance indicators is crucial in the project delivery process. This study aims to analyze the relative importance of architect performance indicators in project delivery process among registered architects in North Sumatera, Indonesia. A total of five indicators that measure architect performance in project delivery process were identified and 110 completed questionnaires were obtained and used for data analysis. A relative importance index is used to rank the relative importance of architect performance indicators. Results indicate that focus on the clients is the most important indicator of architect performance in project delivery process. This study demonstrates project communication as one of crucial indicators perceived by the architects for measuring their performance, and fills a knowledge gap on the importance of identifying the most important indicator for measuring architect performance from their own perspectives which previous studies have overlooked to improve performance assessment in project delivery process.

  17. High-performance IR detector modules

    NASA Astrophysics Data System (ADS)

    Wendler, Joachim; Cabanski, Wolfgang; Rühlich, Ingo; Ziegler, Johann

    2004-02-01

    The 3rd generation of infrared (IR) detection modules is expected to provide higher video resolution, advanced functions like multi band or multi color capability, higher frame rates, and better thermal resolution. AIM has developed staring and linear high performance focal plane arrays (FPA) integrated into detector/dewar cooler assemblies (IDCA). Linear FPA"s support high resolution formats such as 1920 x 1152 (HDTV), 1280 x 960, or 1536 x 1152. Standard format for staring FPA"s is 640 x 512. In this configuration, QEIP devices sensitive in the 8 10 µm band as well as MCT devices sensitive in the 3.4 5.0 µm band are available. A 256 x 256 high speed detection module allows a full frame rate >800 Hz. Especially usability of long wavelength devices in high performance FLIR systems does not only depend on the classical electrooptical performance parameters such as NEDT, detectivity, and response homogeneity, but are mainly characterized by the stability of the correction coefficients used for image correction. The FPA"s are available in suited integrated detector/dewar cooler assemblies. The linear cooling engines are designed for maximum stability of the focal plane temperature, low operating temperatures down to 60K, high MTTF lifetimes of 6000h and above even under high ambient temperature conditions. The IDCA"s are equipped with AIM standard or custom specific command and control electronics (CCE) providing a well defined interface to the system electronics. Video output signals are provided as 14 bit digital data rates up to 80 MHz for the high speed devices.

  18. The Riso-Hudson Enneagram Type Indicator: Estimates of Reliability and Validity

    ERIC Educational Resources Information Center

    Newgent, Rebecca A.; Parr, Patricia E.; Newman, Isadore; Higgins, Kristin K.

    2004-01-01

    This investigation was conducted to estimate the reliability and validity of scores on the Riso-Hudson Enneagram Type Indicator (D. R. Riso & R. Hudson, 1999a). Results of 287 participants were analyzed. Alpha suggests an adequate degree of internal consistency. Evidence provides mixed support for construct validity using correlational and…

  19. Physics validation for design change of KSTAR passive stabilizer

    NASA Astrophysics Data System (ADS)

    Jeon, Y. M.; Kim, J. Y.; Oh, Y. K.; Yang, H. L.; Kim, W. C.; Kim, H. K.; Sabbagh, S. A.; Bialek, J. M.; Humphreys, D. A.; Welander, A. S.; Walker, M. L.

    2009-11-01

    Recently, the design of the passive stabilizer in KSTAR has been changed to improve controllability of the active control system and reduce the possibility of producing an additional error field. Originally the passive stabilizer in KSTAR was designed for RWM and vertical instability (or VDE) stabilizations and plasma startup efficiency, so that current bridges were designed and combined through 3D saddle-loop connections. Since the key design change is removing the current bridges, it's essential to assure satisfactory control performance for these instabilities under the design change. Control capability for n=1 RWM and achievable βN will be addressed as a primary goal of the passive stabilizer together with vertical instability control and effects on plasma startup. In addition, the changes in electro-magnetic force on conducting structures will be discussed qualitatively as a key engineering issue of the design change.

  20. 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.

  1. Optimal placement of unified power flow controllers to improve dynamic voltage stability using power system variable based voltage stability indices.

    PubMed

    Albatsh, Fadi M; Ahmad, Shameem; Mekhilef, Saad; Mokhlis, Hazlie; Hassan, M A

    2015-01-01

    This study examines a new approach to selecting the locations of unified power flow controllers (UPFCs) in power system networks based on a dynamic analysis of voltage stability. Power system voltage stability indices (VSIs) including the line stability index (LQP), the voltage collapse proximity indicator (VCPI), and the line stability index (Lmn) are employed to identify the most suitable locations in the system for UPFCs. In this study, the locations of the UPFCs are identified by dynamically varying the loads across all of the load buses to represent actual power system conditions. Simulations were conducted in a power system computer-aided design (PSCAD) software using the IEEE 14-bus and 39- bus benchmark power system models. The simulation results demonstrate the effectiveness of the proposed method. When the UPFCs are placed in the locations obtained with the new approach, the voltage stability improves. A comparison of the steady-state VSIs resulting from the UPFCs placed in the locations obtained with the new approach and with particle swarm optimization (PSO) and differential evolution (DE), which are static methods, is presented. In all cases, the UPFC locations given by the proposed approach result in better voltage stability than those obtained with the other approaches.

  2. Optimal Placement of Unified Power Flow Controllers to Improve Dynamic Voltage Stability Using Power System Variable Based Voltage Stability Indices

    PubMed Central

    Albatsh, Fadi M.; Ahmad, Shameem; Mekhilef, Saad; Mokhlis, Hazlie; Hassan, M. A.

    2015-01-01

    This study examines a new approach to selecting the locations of unified power flow controllers (UPFCs) in power system networks based on a dynamic analysis of voltage stability. Power system voltage stability indices (VSIs) including the line stability index (LQP), the voltage collapse proximity indicator (VCPI), and the line stability index (Lmn) are employed to identify the most suitable locations in the system for UPFCs. In this study, the locations of the UPFCs are identified by dynamically varying the loads across all of the load buses to represent actual power system conditions. Simulations were conducted in a power system computer-aided design (PSCAD) software using the IEEE 14-bus and 39- bus benchmark power system models. The simulation results demonstrate the effectiveness of the proposed method. When the UPFCs are placed in the locations obtained with the new approach, the voltage stability improves. A comparison of the steady-state VSIs resulting from the UPFCs placed in the locations obtained with the new approach and with particle swarm optimization (PSO) and differential evolution (DE), which are static methods, is presented. In all cases, the UPFC locations given by the proposed approach result in better voltage stability than those obtained with the other approaches. PMID:25874560

  3. 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.

  4. The validity, stability, and utility of measuring uric acid in saliva.

    PubMed

    Riis, Jenna L; Bryce, Crystal I; Matin, Marla J; Stebbins, John L; Kornienko, Olga; Huisstede, Lauren van; Granger, Douglas A

    2018-06-06

    Serum uric acid (UA) is associated with many health conditions, including kidney, cardiovascular, and metabolic disorders. We examined the validity and stability of salivary UA as a noninvasive measure of serum UA. Using serum and salivary UA data from healthy adults (n = 99), we examined the UA serum-saliva correlation, and UA associations with adiponectin and C-reactive protein. Using longitudinal data from young adults (n = 182), we examined salivary UA stability. We found robust positive serum-saliva correlations for UA. UA and adiponectin were inversely related in serum and saliva. Salivary UA was relatively stable; 62-66% of variance could be attributed to a latent trait-like component. Salivary UA may be an important biomarker indexing health and disease risk.

  5. High- β equilibrium and ballooning stability of the low aspect ratio CNT stellarator

    DOE PAGES

    Hammond, K. C.; Lazerson, S. A.; Volpe, F. A.

    2017-04-07

    In the paper, the existence and ballooning-stability of low aspect ratio stellarator equilibria is predicted for the Columbia Neutral Torus (CNT) with the aid of 3D numerical tools. In addition to having a low aspect ratio, CNT is characterized by a low magnetic field and small plasma volume. Also, highly overdense plasmas were recently heated in CNT by means of microwaves. These characteristics suggest that CNT might attain relatively high values of plasma beta and thus be of use in the experimental study of stellarator stability to high-beta instabilities such as ballooning modes. As a first step in that direction,more » here the ballooning stability limit is found numerically. Depending on the particular magnetic configuration we expect volume-averaged β limits in the range 0.9%–3.0%, and possibly higher, and observe indications of a second region of ballooning stability. As the aspect ratio is reduced, stability is found to increase in some configurations and decrease in others. Energy-balance estimates using stellarator scaling laws indicate that the lower β limit may be attainable with overdense heating at powers of 40 to 100 kW. The present study serves the additional purpose of testing VMEC and other stellarator codes at high values of β and at low aspect ratios. For this reason, the study was carried out both for free boundary, for maximum fidelity to experiment, as well as with a fixed boundary, as a numerical test.« less

  6. Development and Validation of High Performance Unshrouded Centrifugal Impeller

    NASA Technical Reports Server (NTRS)

    Chen, Wei-Chung; Williams, M.; Paris, John K.; Prueger, G. H.; Williams, Robert; Turner, James E. (Technical Monitor)

    2001-01-01

    The feasibility of using a two-stage unshrouded impeller turbopump to replace the current three-stage reusable launch vehicle engine shrouded impeller hydrogen pump has been evaluated from the standpoint of turbopump weight reduction and overall payload improvement. These advantages are a by-product of the higher tip speeds that an unshrouded impeller can sustain. The issues associated with the effect of unshrouded impeller tip clearance on pump efficiency and head have been evaluated with one-dimensional tools and full three-dimensional rotordynamic fluid reaction forces and coefficients have been established through time dependent computational fluid dynamics (CFD) simulation of the whole 360 degree impeller with different rotor eccentricities and whirling ratios. Unlike the shrouded impeller, the unshrouded impeller forces are evaluated as the sum of the pressure forces on the blade and the pressure forces on the hub using the CFD results. The turbopump axial thrust control has been optimized by adjusting the first stage impeller backend wear ring seal diameter and diverting the second stage backend balance piston flow to the proper location. The structural integrity associated with the high tip speed has been checked by analyzing a 3D-Finite Element Model at maximum design conditions (6% higher than the design speed). This impeller was fabricated and tested in the NASA Marshall Space Flight Center water-test rig. The experimental data will be compared with the analytical predictions and presented in another paper. The experimental data provides validation data for the numerical design and analysis methodology. The validated numerical methodology can be used to help design different unshrouded impeller configurations.

  7. Environmental stability of high-mobility indium-oxide based transparent electrodes

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

    Tohsophon, Thanaporn; Dabirian, Ali; De Wolf, Stefaan

    2015-11-01

    Large-scale deployment of a wide range of optoelectronic devices, including solar cells, critically depends on the long-term stability of their front electrodes. Here, we investigate the performance of Sn-doped In{sub 2}O{sub 3} (ITO), H-doped In{sub 2}O{sub 3} (IO:H), and Zn-doped In{sub 2}O{sub 3} (IZO) electrodes under damp heat (DH) conditions (85 °C, 85% relative humidity). ITO, IO:H capped with ITO, and IZO show high stability with only 3%, 9%, and 13% sheet resistance (R{sub s}) degradation after 1000 h of DH, respectively. For uncapped IO:H, we find a 75% R{sub s} degradation, due to losses in electron Hall mobility (μ{sub Hall}).more » We propose that this degradation results from chemisorbed OH- or H{sub 2}O-related species in the film, which is confirmed by thermal desorption spectroscopy and x-ray photoelectron spectroscopy. While μ{sub Hall} strongly degrades during DH, the optical mobility (μ{sub optical}) remains unchanged, indicating that the degradation mainly occurs at grain boundaries.« less

  8. Subtle alternating electrocardiographic morphology as an indicator of decreased cardiac electrical stability

    NASA Technical Reports Server (NTRS)

    Smith, J. M.; Blue, B.; Clancy, E.; Valeri, C. R.; Cohen, R. J.

    1985-01-01

    Observations from finite-element computer models, together with analytic developments based on percolation theory have suggested that subtle fluctuations of ECG morphology might serve as an indicator diminished cardiac electrical stability. With fixed-rate atrial pacing in canines, we have previously observed a pattern of alternation in T wave energy which correlated with cardiac electrical stability. We report here on a series of 20 canine experiments in which cardiac electrical stability (measured via Ventricular Fibrillation Threshold determination) was compared to a non-degenerate, multidimensional measurement of the degree of alternating activity present in the ECG complex morphology. The decrease in cardiac electrical stability brought on by both coronary artery occlusion and systemic hypothermia was consistently accompanied by subtle alternation in ECG morphology, with the absolute degree of alternating activity being significantly (negatively) correlated with cardiac electrical stability.

  9. Yield performance and stability of CMS-based triticale hybrids.

    PubMed

    Mühleisen, Jonathan; Piepho, Hans-Peter; Maurer, Hans Peter; Reif, Jochen Christoph

    2015-02-01

    CMS-based triticale hybrids showed only marginal midparent heterosis for grain yield and lower dynamic yield stability compared to inbred lines. Hybrids of triticale (×Triticosecale Wittmack) are expected to possess outstanding yield performance and increased dynamic yield stability. The objectives of the present study were to (1) examine the optimum choice of the biometrical model to compare yield stability of hybrids versus lines, (2) investigate whether hybrids exhibit a more pronounced grain yield performance and yield stability, and (3) study optimal strategies to predict yield stability of hybrids. Thirteen female and seven male parental lines and their 91 factorial hybrids as well as 30 commercial lines were evaluated for grain yield in up to 20 environments. Hybrids were produced using a cytoplasmic male sterility (CMS)-inducing cytoplasm that originated from Triticumtimopheevii Zhuk. We found that the choice of the biometrical model can cause contrasting results and concluded that a group-by-environment interaction term should be added to the model when estimating stability variance of hybrids and lines. midparent heterosis for grain yield was on average 3 % with a range from -15.0 to 11.5 %. No hybrid outperformed the best inbred line. Hybrids had, on average, lower dynamic yield stability compared to the inbred lines. Grain yield performance of hybrids could be predicted based on midparent values and general combining ability (GCA)-predicted values. In contrast, stability variance of hybrids could be predicted only based on GCA-predicted values. We speculated that negative effects of the used CMS cytoplasm might be the reason for the low performance and yield stability of the hybrids. For this purpose a detailed study on the reasons for the drawback of the currently existing CMS system in triticale is urgently required comprising also the search of potentially alternative hybridization systems.

  10. Landslide model performance in a high resolution small-scale landscape

    NASA Astrophysics Data System (ADS)

    De Sy, V.; Schoorl, J. M.; Keesstra, S. D.; Jones, K. E.; Claessens, L.

    2013-05-01

    The frequency and severity of shallow landslides in New Zealand threatens life and property, both on- and off-site. The physically-based shallow landslide model LAPSUS-LS is tested for its performance in simulating shallow landslide locations induced by a high intensity rain event in a small-scale landscape. Furthermore, the effect of high resolution digital elevation models on the performance was tested. The performance of the model was optimised by calibrating different parameter values. A satisfactory result was achieved with a high resolution (1 m) DEM. Landslides, however, were generally predicted lower on the slope than mapped erosion scars. This discrepancy could be due to i) inaccuracies in the DEM or in other model input data such as soil strength properties; ii) relevant processes for this environmental context that are not included in the model; or iii) the limited validity of the infinite length assumption in the infinite slope stability model embedded in the LAPSUS-LS. The trade-off between a correct prediction of landslides versus stable cells becomes increasingly worse with coarser resolutions; and model performance decreases mainly due to altering slope characteristics. The optimal parameter combinations differ per resolution. In this environmental context the 1 m resolution topography resembles actual topography most closely and landslide locations are better distinguished from stable areas than for coarser resolutions. More gain in model performance could be achieved by adding landslide process complexities and parameter heterogeneity of the catchment.

  11. 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.

  12. A Self-Validation Method for High-Temperature Thermocouples Under Oxidizing Atmospheres

    NASA Astrophysics Data System (ADS)

    Mokdad, S.; Failleau, G.; Deuzé, T.; Briaudeau, S.; Kozlova, O.; Sadli, M.

    2015-08-01

    Thermocouples are prone to significant drift in use particularly when they are exposed to high temperatures. Indeed, high-temperature exposure can affect the response of a thermocouple progressively by changing the structure of the thermoelements and inducing inhomogeneities. Moreover, an oxidizing atmosphere contributes to thermocouple drift by changing the chemical nature of the metallic wires by the effect of oxidation. In general, severe uncontrolled drift of thermocouples results from these combined influences. A periodic recalibration of the thermocouple can be performed, but sometimes it is not possible to remove the sensor out of the process. Self-validation methods for thermocouples provide a solution to avoid this drawback, but there are currently no high-temperature contact thermometers with self-validation capability at temperatures up to . LNE-Cnam has developed fixed-point devices integrated to the thermocouples consisting of machined alumina-based devices for operation under oxidizing atmospheres. These devices require small amounts of pure metals (typically less than 2 g). They are suitable for self-validation of high-temperature thermocouples up to . In this paper the construction and the characterization of these integrated fixed-point devices are described. The phase-transition plateaus of gold, nickel, and palladium, which enable coverage of the temperature range between and , are assessed with this self-validation technique. Results of measurements performed at LNE-Cnam with the integrated self-validation module at several levels of temperature will be presented. The performance of the devices are assessed and discussed, in terms of robustness and metrological characteristics. Uncertainty budgets are also proposed and detailed.

  13. Stability-Indicating HPTLC Method for Simultaneous Estimation of Flurbiprofen and Chloramphenicol in Ophthalmic Solution.

    PubMed

    Sadakwala, Vaishnavi M; Chauhan, Renu S; Shah, Shailesh A; Shah, Dinesh R

    2016-01-01

    A specific, accurate and reproducible stability-indicating high performance thin layer chromatography (HPTLC) method was developed for the estimation of flurbiprofen and chloramphenicol in the presence of their degradation products. Degradation studies of both the drugs were carried out in acidic, alkaline, neutral, oxidative, photolytic and thermal stress conditions. Separation was performed on thin layer chromatography plate precoated with silica gel 60 F254 using ethyl acetate : n-hexane : methanol : tri-ethyl amine (5 : 4 : 2 : 0.5, v/v/v/v). Spots at retention factor 0.29 and 0.62 were recognized as flurbiprofen and chloramphenicol, respectively, and were quantified through densitometric measurements at wavelength 267 nm. Method was found to be linear over the concentration range 12-60 ng/spot with correlation coefficient of 0.9997 for flurbiprofen and 200-1,000 ng/spot with correlation coefficient of 0.9977 for chloramphenicol. The proposed method was applied to the estimation of flurbiprofen and chloramphenicol in commercial ophthalmic formulation. The developed HPTLC method can be applied for routine analysis of flurbiprofen and chloramphenicol in the presence of their degradation products in their individual as well as combined pharmaceutical formulations. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  14. Prediction of high-risk areas for visceral leishmaniasis using socioeconomic indicators and remote sensing data

    PubMed Central

    2014-01-01

    Spatial heterogeneity in the incidence of visceral leishmaniasis (VL) is an important aspect to be considered in planning control actions for the disease. The objective of this study was to predict areas at high risk for visceral leishmaniasis (VL) based on socioeconomic indicators and remote sensing data. We applied classification and regression trees to develop and validate prediction models. Performance of the models was assessed by means of sensitivity, specificity and area under the ROC curve. The model developed was able to discriminate 15 subsets of census tracts (CT) with different probabilities of containing CT with high risk of VL occurrence. The model presented, respectively, in the validation and learning samples, sensitivity of 79% and 52%, specificity of 75% and 66%, and area under the ROC curve of 83% and 66%. Considering the complex network of factors involved in the occurrence of VL in urban areas, the results of this study showed that the development of a predictive model for VL might be feasible and useful for guiding interventions against the disease, but it is still a challenge as demonstrated by the unsatisfactory predictive performance of the model developed. PMID:24885128

  15. 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®

  16. Improvement of a stability-indicating method by Quality-by-Design versus Quality-by-Testing: a case of a learning process.

    PubMed

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

    2014-01-01

    The understanding of the method is a major concern when developing a stability-indicating method and even more so when dealing with impurity assays from complex matrices. In the presented case study, a Quality-by-Design approach was applied in order to optimize a routinely used method. An analytical issue occurring at the last stage of a long-term stability study involving unexpected impurities perturbing the monitoring of characterized impurities needed to be resolved. A compliant Quality-by-Design (QbD) methodology based on a Design of Experiments (DoE) approach was evaluated within the framework of a Liquid Chromatography (LC) method. This approach allows the investigation of Critical Process Parameters (CPPs), which have an impact on Critical Quality Attributes (CQAs) and, consequently, on LC selectivity. Using polynomial regression response modeling as well as Monte Carlo simulations for error propagation, Design Space (DS) was computed in order to determine robust working conditions for the developed stability-indicating method. This QbD compliant development was conducted in two phases allowing the use of the Design Space knowledge acquired during the first phase to define the experimental domain of the second phase, which constitutes a learning process. The selected working condition was then fully validated using accuracy profiles based on statistical tolerance intervals in order to evaluate the reliability of the results generated by this LC/ESI-MS stability-indicating method. A comparison was made between the traditional Quality-by-Testing (QbT) approach and the QbD strategy, highlighting the benefit of this QbD strategy in the case of an unexpected impurities issue. On this basis, the advantages of a systematic use of the QbD methodology were discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. 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.

  18. Robustness of hydrological indicators for transient and stabilized climate states

    NASA Astrophysics Data System (ADS)

    Boulange, J. E.; Hanasaki, N.

    2017-12-01

    By signing the Paris agreement, countries have committed to pursue efforts to limit global warming to +1.5 °C relative to pre-industrial levels. Consequently, there is a growing interest in better understanding the impacts of a +1.5°C world. Previous analyses were conducted by considering a time slice period, centered on the year when the global mean temperature (GMT) crosses the +1.5°C threshold (Fig. 1). This time slice period is characterized by a transient state which may influence the reported results (transient climate state). Ideally, analyses should be carried under the condition the GMT is stabilized at +1.5°C (stabilized climate state) but, such targeted simulations do not exist for most GCMs.1A global hydrological model, the H08 model,2 and hydrological indicators (HI) obtained for the transient and stabilized states, are used to answer the following questions: (1) are there quantifiable differences between the HI computed for the transient and stabilized states? (2) can relations be derived between the HI computed for the transient and stabilized states? (3) what are the potential impacts induced by the differences in HI computed for the transient and stabilized states? Signal to noise ratios (S/N) obtained for the transient and stabilized states, in an identical warmer world (+1.7°C), are compared (Fig. 2). The S/N ratio computed for the stabilized state were significantly lower than those of the transient state for most regions and HI. However, at higher latitude, the S/N ratios computed for the two states were similar whereas for medium and low latitudes, the differences were more pronounced. For most regions and HI (except for surface temperature), the S/N ratios of the stabilized state were 10 to 20% weaker than those of the transient state. References:1 Knutti, R., Rogelj, J., Sedlacek, J. & Fischer, E. M. Nature Geosci (2016). 2 Hanasaki, N. et al. Hydrol. Earth Syst. Sci. (2008).

  19. High performance bilateral telerobot control.

    PubMed

    Kline-Schoder, Robert; Finger, William; Hogan, Neville

    2002-01-01

    Telerobotic systems are used when the environment that requires manipulation is not easily accessible to humans, as in space, remote, hazardous, or microscopic applications or to extend the capabilities of an operator by scaling motions and forces. The Creare control algorithm and software is an enabling technology that makes possible guaranteed stability and high performance for force-feedback telerobots. We have developed the necessary theory, structure, and software design required to implement high performance telerobot systems with time delay. This includes controllers for the master and slave manipulators, the manipulator servo levels, the communication link, and impedance shaping modules. We verified the performance using both bench top hardware as well as a commercial microsurgery system.

  20. Facilities Performance Indicators Report, 2008-09

    ERIC Educational Resources Information Center

    Hills, Christina, Ed.

    2010-01-01

    This paper features another expanded Web-based Facilities Performance Indicators Report (FPI). The purpose of APPA's Facilities Performance Indicators is to provide a representative set of statistics about facilities in educational institutions. The 2008-09 iteration of the Web-based Facilities Performance Indicators Survey was posted and…

  1. Use of comparative performance indicators in rehabilitation.

    PubMed

    Zidarov, Diana; Poissant, Lise; Sicotte, Claude

    The development of performance indicators that enable benchmarking between organizations is an important mechanism for accountability, organizational learning, and performance improvement. In the province of Quebec (Canada), 21 rehabilitation organizations developed a common set of performance indicators through interorganizational collaboration. The aims of this study were to describe the rehabilitation organizations' use of a common set of performance indicators and to identify the factors influencing such use. A qualitative survey was performed. Individual semistructured interviews were conducted with executives (n = 18) working at 16 rehabilitation organizations using a common set of performance indicators. A thematic analysis of the factors of use was performed according to the Consolidated Framework for Implementation Research. The use of performance indicators was categorized as purposeful, political, or passive. Our results showed that all organizations used the common set of performance indicators. Four factors were identified as important to all the rehabilitation organizations to explain their interest in comparative performance indicators: the need to develop their own performance indicators, the compatibility of performance information with organizational needs, complexity/simplicity of performance information, and the support offered by their common association. Sixty-three percent of rehabilitation organizations made purposeful or political use of performance indicators. Three main factors contributed to typify those organizations from the others: the perceived quality of the performance indicators, the leadership of decision makers, and the resources available. Our results showed that use of performance indicators can support the initiation of projects for improving the quality of care. Key recommendations are proposed to decision makers that may enhance performance indicators' use.

  2. Performance indicators for public mental healthcare: a systematic international inventory

    PubMed Central

    2012-01-01

    Background The development and use of performance indicators (PI) in the field of public mental health care (PMHC) has increased rapidly in the last decade. To gain insight in the current state of PI for PMHC in nations and regions around the world, we conducted a structured review of publications in scientific peer-reviewed journals supplemented by a systematic inventory of PI published in policy documents by (non-) governmental organizations. Methods Publications on PI for PMHC were identified through database- and internet searches. Final selection was based on review of the full content of the publications. Publications were ordered by nation or region and chronologically. Individual PI were classified by development method, assessment level, care domain, performance dimension, diagnostic focus, and data source. Finally, the evidence on feasibility, data reliability, and content-, criterion-, and construct validity of the PI was evaluated. Results A total of 106 publications were included in the sample. The majority of the publications (n = 65) were peer-reviewed journal articles and 66 publications specifically dealt with performance of PMHC in the United States. The objectives of performance measurement vary widely from internal quality improvement to increasing transparency and accountability. The characteristics of 1480 unique PI were assessed. The majority of PI is based on stakeholder opinion, assesses care processes, is not specific to any diagnostic group, and utilizes administrative data sources. The targeted quality dimensions varied widely across and within nations depending on local professional or political definitions and interests. For all PI some evidence for the content validity and feasibility has been established. Data reliability, criterion- and construct validity have rarely been assessed. Only 18 publications on criterion validity were included. These show significant associations in the expected direction on the majority of PI, but mixed

  3. Novel active stabilization technology in highly crosslinked UHMWPEs for superior stability

    NASA Astrophysics Data System (ADS)

    Oral, Ebru; Neils, Andrew L.; Wannomae, Keith K.; Muratoglu, Orhun K.

    2014-12-01

    Radiation cross-linked ultrahigh molecular weight polyethylene (UHMWPE) is the bearing of choice in joint arthroplasty. The demands on the longevity of this polymer are likely to increase with the recently advancing deterioration of the performance of alternative metal-on-metal implants. Vitamin E-stabilized, cross-linked UHMWPEs are considered the next generation of improved UHMWPE bearing surfaces for improving the oxidation resistance of the polymer. It was recently discovered that in the absence of radiation-induced free radicals, lipids absorbed into UHMWPE from the synovial fluid can initiate oxidation and result in new free radical-mediated oxidation mechanisms. In the presence of radiation-induced free radicals, it is possible for the polymer to oxidize through both existing free radicals at the time of implantation and through newly formed free radicals in vivo. Thus, we showed that reducing the radiation-induced free radicals in vitamin E-stabilized UHMWPE would increase its oxidative stability and presumably lead to improved longevity. We describe mechanical annealing and warm irradiation of irradiated vitamin E blends as novel methods to eliminate 99% of radiation-induced free radicals without sacrificing crystallinity. These are significant improvements in the processing of highly cross-linked UHMWPE for joint implants with improved longevity.

  4. Measuring sperm whales from their clicks: Stability of interpulse intervals and validation that they indicate whale length

    NASA Astrophysics Data System (ADS)

    Rhinelander, Marcus Q.; Dawson, Stephen M.

    2004-04-01

    Multiple pulses can often be distinguished in the clicks of sperm whales (Physeter macrocephalus). Norris and Harvey [in Animal Orientation and Navigation, NASA SP-262 (1972), pp. 397-417] proposed that this results from reflections within the head, and thus that interpulse interval (IPI) is an indicator of head length, and by extrapolation, total length. For this idea to hold, IPIs must be stable within individuals, but differ systematically among individuals of different size. IPI stability was examined in photographically identified individuals recorded repeatedly over different dives, days, and years. IPI variation among dives in a single day and days in a single year was statistically significant, although small in magnitude (it would change total length estimates by <3%). As expected, IPIs varied significantly among individuals. Most individuals showed significant increases in IPIs over several years, suggesting growth. Mean total lengths calculated from published IPI regressions were 13.1 to 16.1 m, longer than photogrammetric estimates of the same whales (12.3 to 15.3 m). These discrepancies probably arise from the paucity of large (12-16 m) whales in data used in published regressions. A new regression is offered for this size range.

  5. Analysis of genetic association using hierarchical clustering and cluster validation indices.

    PubMed

    Pagnuco, Inti A; Pastore, Juan I; Abras, Guillermo; Brun, Marcel; Ballarin, Virginia L

    2017-10-01

    It is usually assumed that co-expressed genes suggest co-regulation in the underlying regulatory network. Determining sets of co-expressed genes is an important task, based on some criteria of similarity. This task is usually performed by clustering algorithms, where the genes are clustered into meaningful groups based on their expression values in a set of experiment. In this work, we propose a method to find sets of co-expressed genes, based on cluster validation indices as a measure of similarity for individual gene groups, and a combination of variants of hierarchical clustering to generate the candidate groups. We evaluated its ability to retrieve significant sets on simulated correlated and real genomics data, where the performance is measured based on its detection ability of co-regulated sets against a full search. Additionally, we analyzed the quality of the best ranked groups using an online bioinformatics tool that provides network information for the selected genes. Copyright © 2017 Elsevier Inc. All rights reserved.

  6. Indicators of the relative availability of healthy versus unhealthy foods in supermarkets: a validation study.

    PubMed

    Vandevijvere, Stefanie; Mackenzie, Tara; Mhurchu, Cliona Ni

    2017-04-26

    In-store availability of healthy and unhealthy foods may influence consumer purchases. Methods used to measure food availability, however, vary widely. A simple, valid, and reliable indicator to collect comparable data on in-store food availability is needed. Cumulative linear shelf length of and variety within 22 healthy and 28 unhealthy food groups, determined based on a comparison of three nutrient profiling systems, were measured in 15 New Zealand supermarkets. Inter-rater reliability was tested in one supermarket by a second researcher. The construct validity of five simple indicators of relative availability of healthy versus unhealthy foods was assessed against this 'gold standard'. Cumulative linear shelf length was a more sensitive and feasible measure of food availability than variety. Four out of five shelf length ratio indicators were significantly associated with the gold standard (ρ = 0.70-0.75). Based on a non-significant difference from the 'gold standard' (d = 0.053 ± 0.040) and feasibility, the ratio of cumulative linear shelf length of fresh and frozen fruits and vegetables versus soft and energy drinks, crisps and snacks, sweet biscuits and confectionery performed best for use in New Zealand supermarkets. Four out of the five shelf length ratio indicators of the relative availability of healthy versus unhealthy foods in-store tested could be used for future research and monitoring, but additional validation studies in other settings and countries are recommended. Consistent use of those shelf length ratio indicators could enhance comparability of supermarket food availability between studies, and help inform policies to create healthy consumer food retail environments.

  7. Performance criteria and quality indicators for the post-analytical phase.

    PubMed

    Sciacovelli, Laura; Aita, Ada; Padoan, Andrea; Pelloso, Michela; Antonelli, Giorgia; Piva, Elisa; Chiozza, Maria Laura; Plebani, Mario

    2016-07-01

    Quality indicators (QIs) used as performance measurements are an effective tool in accurately estimating quality, identifying problems that may need to be addressed, and monitoring the processes over time. In Laboratory Medicine, QIs should cover all steps of the testing process, as error studies have confirmed that most errors occur in the pre- and post-analytical phase of testing. Aim of the present study is to provide preliminary results on QIs and related performance criteria in the post-analytical phase. This work was conducted according to a previously described study design based on the voluntary participation of clinical laboratories in the project on QIs of the Working Group "Laboratory Errors and Patient Safety" (WG-LEPS) of the International Federation of Clinical Chemistry and Laboratory Medicine (IFCC). Overall, data collected highlighted an improvement or stability in performances over time for all reported indicators thus demonstrating that the use of QIs is effective in the quality improvement strategy. Moreover, QIs data are an important source for defining the state-of-the-art concerning the error rate in the total testing process. The definition of performance specifications based on the state-of-the-art, as suggested by consensus documents, is a valuable benchmark point in evaluating the performance of each laboratory. Laboratory tests play a relevant role in the monitoring and evaluation of the efficacy of patient outcome thus assisting clinicians in decision-making. Laboratory performance evaluation is therefore crucial to providing patients with safe, effective and efficient care.

  8. Performance Stability of Silicone Oxide-Coated Plastic Parenteral Vials.

    PubMed

    Weikart, Christopher M; Pantano, Carlo G; Shallenberger, Jeff R

    2017-01-01

    A new packaging system was developed for parenteral pharmaceuticals that combines the best attributes of plastic and glass without their respective drawbacks. This technological advancement is based on the synergy between high-precision injection-molded plastics and plasma coating technology. The result is a shatter-resistant, optically clear, low-particulate, and chemically durable packaging system. The demand for this product is driven by the expanding market, regulatory constraints, and product recalls for injectable drugs and biologics packaged in traditional glass materials. It is shown that this new packaging system meets or exceeds the important performance characteristics of glass, especially in eliminating the glass delamination and breakage that has been observed in many products. The new packaging system is an engineered, multilayer, glass-coated plastic composite that provides a chemically stable contact surface and oxygen barrier performance that exceeds a 2 year shelf life requirement. Evaluation of the coating system characteristics and performance stability to chemical, temperature, and mechanical extremes are reported herein. LAY ABSTRACT: A new packaging system for parenteral pharmaceuticals was developed that combines the best attributes of plastic and glass without their respective drawbacks. This technological advancement is based on the synergy between high-precision injection-molded plastics and plasma coating technology. The result is a shatter-resistant, optically clear, low-particulate, and chemically durable packaging system. It is shown that this new packaging system meets or exceeds the important performance characteristics of glass, especially in eliminating the glass delamination and breakage that has been observed in many products. The new packaging system is an engineered, multilayer, glass-coated plastic composite that provides a chemically stable contact surface and oxygen barrier performance that exceeds a 2 year shelf life

  9. What do conscientious people do? Development and validation of the Behavioral Indicators of Conscientiousness (BIC).

    PubMed

    Jackson, Joshua J; Wood, Dustin; Bogg, Tim; Walton, Kate E; Harms, Peter D; Roberts, Brent W

    2010-08-01

    Typical assessments of personality traits collapse behaviors, thoughts, and feelings into a single measure without distinguishing between these different manifestations. To address this lack of specification, the current study develops and validates a measure that assesses a number of broad behaviors associated with the personality trait of conscientiousness (the Behavioral Indicators of Conscientiousness; BIC). Findings suggest that the lower-order structure of conscientious behaviors is mostly similar to the lower-order structure in extant trait measures. Furthermore, a daily diary method was used to validate the BIC against frequency counts of conscientious behavior. Overall, the results identify specific behaviors that conscientious individuals tend to perform and highlight possible advantages of this approach over broad trait assessment.

  10. 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

  11. Coated Porous Si for High Performance On-Chip Supercapacitors

    NASA Astrophysics Data System (ADS)

    Grigoras, K.; Keskinen, J.; Grönberg, L.; Ahopelto, J.; Prunnila, M.

    2014-11-01

    High performance porous Si based supercapacitor electrodes are demonstrated. High power density and stability is provided by ultra-thin TiN coating of the porous Si matrix. The TiN layer is deposited by atomic layer deposition (ALD), which provides sufficient conformality to reach the bottom of the high aspect ratio pores. Our porous Si supercapacitor devices exhibit almost ideal double layer capacitor characteristic with electrode volumetric capacitance of 7.3 F/cm3. Several orders of magnitude increase in power and energy density is obtained comparing to uncoated porous silicon electrodes. Good stability of devices is confirmed performing several thousands of charge/discharge cycles.

  12. Automated Performance Characterization of DSN System Frequency Stability Using Spacecraft Tracking Data

    NASA Technical Reports Server (NTRS)

    Pham, Timothy T.; Machuzak, Richard J.; Bedrossian, Alina; Kelly, Richard M.; Liao, Jason C.

    2012-01-01

    This software provides an automated capability to measure and qualify the frequency stability performance of the Deep Space Network (DSN) ground system, using daily spacecraft tracking data. The results help to verify if the DSN performance is meeting its specification, therefore ensuring commitments to flight missions; in particular, the radio science investigations. The rich set of data also helps the DSN Operations and Maintenance team to identify the trends and patterns, allowing them to identify the antennas of lower performance and implement corrective action in a timely manner. Unlike the traditional approach where the performance can only be obtained from special calibration sessions that are both time-consuming and require manual setup, the new method taps into the daily spacecraft tracking data. This new approach significantly increases the amount of data available for analysis, roughly by two orders of magnitude, making it possible to conduct trend analysis with good confidence. The software is built with automation in mind for end-to-end processing. From the inputs gathering to computation analysis and later data visualization of the results, all steps are done automatically, making the data production at near zero cost. This allows the limited engineering resource to focus on high-level assessment and to follow up with the exceptions/deviations. To make it possible to process the continual stream of daily incoming data without much effort, and to understand the results quickly, the processing needs to be automated and the data summarized at a high level. Special attention needs to be given to data gathering, input validation, handling anomalous conditions, computation, and presenting the results in a visual form that makes it easy to spot items of exception/ deviation so that further analysis can be directed and corrective actions followed.

  13. Automated Performance Characterization of DSN System Frequency Stability Using Spacecraft Tracking Data

    NASA Technical Reports Server (NTRS)

    Pham, Timothy T.; Machuzak, Richard J.; Bedrossian, Alina; Kelly, Richard M.; Liao, Jason C.

    2012-01-01

    This software provides an automated capability to measure and qualify the frequency stability performance of the Deep Space Network (DSN) ground system, using daily spacecraft tracking data. The results help to verify if the DSN performance is meeting its specification, therefore ensuring commitments to flight missions; in particular, the radio science investigations. The rich set of data also helps the DSN Operations and Maintenance team to identify the trends and patterns, allowing them to identify the antennas of lower performance and implement corrective action in a timely manner. Unlike the traditional approach where the performance can only be obtained from special calibration sessions that are both time-consuming and require manual setup, the new method taps into the daily spacecraft tracking data. This new approach significantly increases the amount of data available for analysis, roughly by two orders of magnitude, making it possible to conduct trend analysis with good confidence. The software is built with automation in mind for end-to-end processing. From the inputs gathering to computation analysis and later data visualization of the results, all steps are done automatically, making the data production at near zero cost. This allows the limited engineering resource to focus on high-level assessment and to follow up with the exceptions/deviations. To make it possible to process the continual stream of daily incoming data without much effort, and to understand the results quickly, the processing needs to be automated and the data summarized at a high level. Special attention needs to be given to data gathering, input validation, handling anomalous conditions, computation, and presenting the results in a visual form that makes it easy to spot items of exception/deviation so that further analysis can be directed and corrective actions followed.

  14. Development and Validation of the Career Competencies Indicator (CCI)

    ERIC Educational Resources Information Center

    Francis-Smythe, Jan; Haase, Sandra; Thomas, Erica; Steele, Catherine

    2013-01-01

    This article describes the development and validation of the Career Competencies Indicator (CCI); a 43-item measure to assess career competencies (CCs). Following an extensive literature review, a comprehensive item generation process involving consultation with subject matter experts, a pilot study and a factor analytic study on a large sample…

  15. 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

  16. ORBITAL STABILITY OF MULTI-PLANET SYSTEMS: BEHAVIOR AT HIGH MASSES

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

    Morrison, Sarah J.; Kratter, Kaitlin M., E-mail: morrison@lpl.arizona.edu, E-mail: kkratter@email.arizona.edu

    2016-06-01

    In the coming years, high-contrast imaging surveys are expected to reveal the characteristics of the population of wide-orbit, massive, exoplanets. To date, a handful of wide planetary mass companions are known, but only one such multi-planet system has been discovered: HR 8799. For low mass planetary systems, multi-planet interactions play an important role in setting system architecture. In this paper, we explore the stability of these high mass, multi-planet systems. While empirical relationships exist that predict how system stability scales with planet spacing at low masses, we show that extrapolating to super-Jupiter masses can lead to up to an ordermore » of magnitude overestimate of stability for massive, tightly packed systems. We show that at both low and high planet masses, overlapping mean-motion resonances trigger chaotic orbital evolution, which leads to system instability. We attribute some of the difference in behavior as a function of mass to the increasing importance of second order resonances at high planet–star mass ratios. We use our tailored high mass planet results to estimate the maximum number of planets that might reside in double component debris disk systems, whose gaps may indicate the presence of massive bodies.« less

  17. High Reynolds Number Thermal Stability Experiments

    NASA Technical Reports Server (NTRS)

    Emens, Jessica M.; Brown, Sarah P.; Frederick Robert A., Jr.; Wood, A. John

    2004-01-01

    This work represents preliminary thermal stability results for liquid hydrocarbon fuels. High Reynolds Number Thermal Stability experiments with Jet A and RP-1 resulted in a quantitative measurement of the thermal stability. Each fuel flowed through a heated capillary tube that held the outlet temperature at 290 C. An optical pyrometer measured the surface temperature of the tube at 12 locations as a function of time. The High Reynolds Number Thermal Stability number was then determined using standards published by the American Society for Testing and Materials. The results for Jet A showed lower thermal stability than similar tests conducted at another facility. The RP-1 results are the first reported using this technique. Because the temperature rise on the capillary tube during testing for the RP-1 fuels was not significant, a new standard for the testing conditions should be developed for these types of fuels.

  18. An Inventory Battery to Predict Navy and Marine Corps Recruiter Performance: Development and Validation

    DTIC Science & Technology

    1979-05-01

    Cross-Validation Strategies to Diferent Sections of the Predictor Batery ..................... 27 Personality Scales . . . . . . . . . . . . 0. . a...he generated several performance indices on the basis of assumptions about the recruiting environment and geographical differences in production

  19. 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.

  20. Respiration and enzymatic activities as indicators of stabilization of sewage sludge composting.

    PubMed

    Nikaeen, Mahnaz; Nafez, Amir Hossein; Bina, Bijan; Nabavi, BiBi Fatemeh; Hassanzadeh, Akbar

    2015-05-01

    The objective of this work was to study the evolution of physico-chemical and microbial parameters in the composting process of sewage sludge (SS) with pruning wastes (PW) in order to compare these parameters with respect to their applicability in the evaluation of organic matter (OM) stabilization. To evaluate the composting process and organic matter stability, different microbial activities were compared during composting of anaerobically digested SS with two volumetric ratios, 1:1 and 3:1 of PW:SS and two aeration techniques including aerated static piles (ASP) and turned windrows (TW). Dehydrogenase activity, fluorescein diacetate hydrolysis, and specific oxygen uptake rate (SOUR) were used as microbial activity indices. These indices were compared with traditional parameters, including temperature, pH, moisture content, organic matter, and C/N ratio. The results showed that the TW method and 3:1 (PW:SS) proportion was superior to the ASP method and 1:1 proportion, since the former accelerate the composting process by catalyzing the OM stabilization. Enzymatic activities and SOUR, which reflect microbial activity, correlated well with temperature fluctuations. Based on these results it appears that SOUR and the enzymatic activities are useful parameters to monitor the stabilization of SS compost. Copyright © 2015 Elsevier Ltd. All rights reserved.

  1. A Target-Lighted dsDNA-Indicator for High-Performance Monitoring of Mercury Pollution and Its Antagonists Screening.

    PubMed

    Qing, Zhihe; Zhu, Lixuan; Li, Xiaoxuan; Yang, Sheng; Zou, Zhen; Guo, Jingru; Cao, Zhong; Yang, Ronghua

    2017-10-17

    As well-known, the excessive discharge of heavy-metal mercury not only destroys the ecological environment, bust also leads to severe damage of human health after ingestion via drinking and bioaccumulation of food chains, and mercury ion (Hg 2+ ) is designated as one of most prevalent toxic metal ions in drinking water. Thus, the high-performance monitoring of mercury pollution is necessary. Functional nucleic acids have been widely used as recognition probes in biochemical sensing. In this work, a carbazole derivative, ethyl-4-[3,6-bis(1-methyl-4-vinylpyridium iodine)-9H-carbazol -9-yl)] butanoate (EBCB), has been synthesized and found as a target-lighted DNA fluorescent indicator. As a proof-of-concept, Hg 2+ detection was carried out based on EBCB and Hg 2+ -mediated conformation transformation of a designed DNA probe. By comparison with conventional nucleic acid indicators, EBCB held excellent advantages, such as minimal background interference and maximal sensitivity. Outstanding detection capabilities were displayed, especially including simple operation (add-and-read manner), ultrarapidity (30 s), and low detection limit (0.82 nM). Furthermore, based on these advantages, the potential for high-performance screening of mercury antagonists was also demonstrated by the fluorescence change of EBCB. Therefore, we believe that this work is meaningful in pollution monitoring, environment restoration and emergency treatment, and may pave a way to apply EBCB as an ideal signal transducer for development of high-performance sensing strategies.

  2. Performance Indicators: Accountable to Whom?

    ERIC Educational Resources Information Center

    Conlon, Michael

    2004-01-01

    In this paper the author examines the implementation of key performance indicators in Canadian post-secondary education institutions. More specifically he charts their implementation from the perspective of students and the effect they have on the quality and delivery of education. Key performance indicators (KPI) in Canada are administered by the…

  3. Validation of Helicopter Gear Condition Indicators Using Seeded Fault Tests

    NASA Technical Reports Server (NTRS)

    Dempsey, Paula; Brandon, E. Bruce

    2013-01-01

    A "seeded fault test" in support of a rotorcraft condition based maintenance program (CBM), is an experiment in which a component is tested with a known fault while health monitoring data is collected. These tests are performed at operating conditions comparable to operating conditions the component would be exposed to while installed on the aircraft. Performance of seeded fault tests is one method used to provide evidence that a Health Usage Monitoring System (HUMS) can replace current maintenance practices required for aircraft airworthiness. Actual in-service experience of the HUMS detecting a component fault is another validation method. This paper will discuss a hybrid validation approach that combines in service-data with seeded fault tests. For this approach, existing in-service HUMS flight data from a naturally occurring component fault will be used to define a component seeded fault test. An example, using spiral bevel gears as the targeted component, will be presented. Since the U.S. Army has begun to develop standards for using seeded fault tests for HUMS validation, the hybrid approach will be mapped to the steps defined within their Aeronautical Design Standard Handbook for CBM. This paper will step through their defined processes, and identify additional steps that may be required when using component test rig fault tests to demonstrate helicopter CI performance. The discussion within this paper will provide the reader with a better appreciation for the challenges faced when defining a seeded fault test for HUMS validation.

  4. A validated stability indicating RP-HPLC method for estimation of Armodafinil in pharmaceutical dosage forms and characterization of its base hydrolytic product.

    PubMed

    Venkateswarlu, Kambham; Rangareddy, Ardhgeri; Narasimhaiah, Kanaka; Sharma, Hemraj; Bandi, Naga Mallikarjuna Raja

    2017-01-01

    The main objective of present study was to develop a RP-HPLC method for estimation of Armodafinil in pharmaceutical dosage forms and characterization of its base hydrolytic product. The method was developed for Armodafinil estimation and base hydrolytic products were characterized. The separation was carried out on C18 column by using mobile phase as mixture of water and methanol (45:55%v/v). Eluents were detected at 220nm at 1ml/min. Stress studies were performed with milder conditions followed by stronger conditions so as to get sufficient degradation around 20%. A total of five degradation products were detected and separated from analyte. The linearity of the proposed method was investigated in the range of 20-120µg/ml for Armodafinil. The detection limit and quantification limit was found to be 0.01183μg/ml and 0.035µg/ml respectively. The precision % RSD was found to be less than 2% and the recovery was between 98-102%. Armodafinil was found to be more sensitive to the base hydrolysis and yielded its carboxylic acid as degradant. The developed method was stability indicating assay, suitable to quantify Armodafinil in presence of possible degradants. The drug was sensitive to acid, base &photolytic stress and resistant to thermal &oxidation.

  5. Application of a newly developed and validated high-performance thin-layer chromatographic method to control honey adulteration.

    PubMed

    Puscas, Anitta; Hosu, Anamaria; Cimpoiu, Claudia

    2013-01-11

    Honey is a saturated solution of sugars, used for a long time as a natural source of sugars and is an important ingredient in traditional medicine due to its antimicrobial, anti-inflammatory and antioxidant effects. Therefore, methods for quality control of honey and detection of its adulteration are very important. For this reason, the aim of this study is to develop and validate a new, simple and economical analytical method for detecting the adulteration of some Romanian honeys based on high-performance thin-layer chromatography (HPTLC) combined with image analysis. The proposed method involved the chromatographic separations of glucose, fructose and sucrose on silica gel HPTLC plates, developed twice with ethyl acetate-pyridine-water-acetic acid, 6:3:1:0.5 (v/v/v/v), followed by dipping in an immersion solution. The documentation of plates was performed using TLC visualization device and the images of plates were processed using a digital processor. The developed HPTLC method was validated for selectivity, linearity and range, LOD and LOQ, precision, robustness and accuracy. The method was then applied for quantitative determination of glucose, fructose and sucrose from different types of Romanian honeys, commercially available. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. 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…

  7. A High Stability Time Difference Readout Technique of RTD-Fluxgate Sensors

    PubMed Central

    Pang, Na; Cheng, Defu; Wang, Yanzhang

    2017-01-01

    The performance of Residence Times Difference (RTD)-fluxgate sensors is closely related to the time difference readout technique. The noise of the induction signal affects the quality of the output signal of the following circuit and the time difference detection, so the stability of the sensor is limited. Based on the analysis of the uncertainty of the RTD-fluxgate using the Bidirectional Magnetic Saturation Time Difference (BMSTD) readout scheme, the relationship between the saturation state of the magnetic core and the target (DC) magnetic field is studied in this article. It is proposed that combining the excitation and induction signals can provide the Negative Magnetic Saturation Time (NMST), which is a detection quantity used to measure the target magnetic field. Also, a mathematical model of output response between NMST and the target magnetic field is established, which analyzes the output NMST and sensitivity of the RTD-fluxgate sensor under different excitation conditions and is compared to the BMSTD readout scheme. The experiment results indicate that this technique can effectively reduce the noise influence. The fluctuation of time difference is less than ±0.1 μs in a target magnetic field range of ±5 × 104 nT. The accuracy and stability of the sensor are improved, so the RTD-fluxgate using the readout technique of high stability time difference is suitable for detecting weak magnetic fields. PMID:29023409

  8. 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.

  9. Development and validation of high-performance liquid chromatography and high-performance thin-layer chromatography methods for the quantification of khellin in Ammi visnaga seed

    PubMed Central

    Kamal, Abid; Khan, Washim; Ahmad, Sayeed; Ahmad, F. J.; Saleem, Kishwar

    2015-01-01

    Objective: The present study was used to design simple, accurate and sensitive reversed phase-high-performance liquid chromatography RP-HPLC and high-performance thin-layer chromatography (HPTLC) methods for the development of quantification of khellin present in the seeds of Ammi visnaga. Materials and Methods: RP-HPLC analysis was performed on a C18 column with methanol: Water (75: 25, v/v) as a mobile phase. The HPTLC method involved densitometric evaluation of khellin after resolving it on silica gel plate using ethyl acetate: Toluene: Formic acid (5.5:4.0:0.5, v/v/v) as a mobile phase. Results: The developed HPLC and HPTLC methods were validated for precision (interday, intraday and intersystem), robustness and accuracy, limit of detection and limit of quantification. The relationship between the concentration of standard solutions and the peak response was linear in both HPLC and HPTLC methods with the concentration range of 10–80 μg/mL in HPLC and 25–1,000 ng/spot in HPTLC for khellin. The % relative standard deviation values for method precision was found to be 0.63–1.97%, 0.62–2.05% in HPLC and HPTLC for khellin respectively. Accuracy of the method was checked by recovery studies conducted at three different concentration levels and the average percentage recovery was found to be 100.53% in HPLC and 100.08% in HPTLC for khellin. Conclusions: The developed HPLC and HPTLC methods for the quantification of khellin were found simple, precise, specific, sensitive and accurate which can be used for routine analysis and quality control of A. visnaga and several formulations containing it as an ingredient. PMID:26681890

  10. Scalable Fabrication of High-Performance Transparent Conductors Using Graphene Oxide-Stabilized Single-Walled Carbon Nanotube Inks

    PubMed Central

    He, Linxiang; Liao, Chengzhu

    2018-01-01

    Recent development in liquid-phase processing of single-walled carbon nanotubes (SWNTs) has revealed rod-coating as a promising approach for large-scale production of SWNT-based transparent conductors. Of great importance in the ink formulation is the stabilizer having excellent dispersion stability, environmental friendly and tunable rheology in the liquid state, and also can be readily removed to enhance electrical conductivity and mechanical stability. Herein we demonstrate the promise of graphene oxide (GO) as a synergistic stabilizer for SWNTs in water. SWNTs dispersed in GO is formulated into inks with homogeneous nanotube distribution, good wetting and rheological properties, and compatible with industrial rod coating practice. Microwave treatment of rod-coated films can reduce GOs and enhance electro-optical performance. The resultant films offer a sheet resistance of ~80 Ω/sq at 86% transparency, along with good mechanical flexibility. Doping the films with nitric acid can further decrease the sheet resistance to ~25 Ω/sq. Comparing with the films fabricated from typical surfactant-based SWNT inks, our films offer superior adhesion as assessed by the Scotch tape test. This study provides new insight into the selection of suitable stabilizers for functional SWNT inks with strong potential for printed electronics. PMID:29642446

  11. Stability indicating HPLC-UV method for detection of curcumin in Curcuma longa extract and emulsion formulation.

    PubMed

    Syed, Haroon Khalid; Liew, Kai Bin; Loh, Gabriel Onn Kit; Peh, Kok Khiang

    2015-03-01

    A stability-indicating HPLC-UV method for the determination of curcumin in Curcuma longa extract and emulsion was developed. The system suitability parameters, theoretical plates (N), tailing factor (T), capacity factor (K'), height equivalent of a theoretical plate (H) and resolution (Rs) were calculated. Stress degradation studies (acid, base, oxidation, heat and UV light) of curcumin were performed in emulsion. It was found that N>6500, T<1.1, K' was 2.68-3.75, HETP about 37 and Rs was 1.8. The method was linear from 2 to 200 μg/mL with a correlation coefficient of 0.9998. The intra-day precision and accuracy for curcumin were ⩽0.87% and ⩽2.0%, while the inter-day precision and accuracy values were ⩽2.1% and ⩽-1.92. Curcumin degraded in emulsion under acid, alkali and UV light. In conclusion, the stability-indicating method could be employed to determine curcumin in bulk and emulsions. Copyright © 2014 Elsevier Ltd. All rights reserved.

  12. 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.

  13. Next-generation fiber lasers enabled by high-performance components

    NASA Astrophysics Data System (ADS)

    Kliner, D. A. V.; Victor, B.; Rivera, C.; Fanning, G.; Balsley, D.; Farrow, R. L.; Kennedy, K.; Hampton, S.; Hawke, R.; Soukup, E.; Reynolds, M.; Hodges, A.; Emery, J.; Brown, A.; Almonte, K.; Nelson, M.; Foley, B.; Dawson, D.; Hemenway, D. M.; Urbanek, W.; DeVito, M.; Bao, L.; Koponen, J.; Gross, K.

    2018-02-01

    Next-generation industrial fiber lasers enable challenging applications that cannot be addressed with legacy fiber lasers. Key features of next-generation fiber lasers include robust back-reflection protection, high power stability, wide power tunability, high-speed modulation and waveform generation, and facile field serviceability. These capabilities are enabled by high-performance components, particularly pump diodes and optical fibers, and by advanced fiber laser designs. We summarize the performance and reliability of nLIGHT diodes, fibers, and next-generation industrial fiber lasers at power levels of 500 W - 8 kW. We show back-reflection studies with up to 1 kW of back-reflected power, power-stability measurements in cw and modulated operation exhibiting sub-1% stability over a 5 - 100% power range, and high-speed modulation (100 kHz) and waveform generation with a bandwidth 20x higher than standard fiber lasers. We show results from representative applications, including cutting and welding of highly reflective metals (Cu and Al) for production of Li-ion battery modules and processing of carbon fiber reinforced polymers.

  14. The Predictive Validity of CBM Writing Indices for Eighth-Grade Students

    ERIC Educational Resources Information Center

    Amato, Janelle M.; Watkins, Marley W.

    2011-01-01

    Curriculum-based measurement (CBM) is an alternative to traditional assessment techniques. Technical work has begun to identify CBM writing indices that are psychometrically sound for monitoring older students' writing proficiency. This study examined the predictive validity of CBM writing indices in a sample of 447 eighth-grade students.…

  15. 3D printed high performance strain sensors for high temperature applications

    NASA Astrophysics Data System (ADS)

    Rahman, Md Taibur; Moser, Russell; Zbib, Hussein M.; Ramana, C. V.; Panat, Rahul

    2018-01-01

    Realization of high temperature physical measurement sensors, which are needed in many of the current and emerging technologies, is challenging due to the degradation of their electrical stability by drift currents, material oxidation, thermal strain, and creep. In this paper, for the first time, we demonstrate that 3D printed sensors show a metamaterial-like behavior, resulting in superior performance such as high sensitivity, low thermal strain, and enhanced thermal stability. The sensors were fabricated using silver (Ag) nanoparticles (NPs), using an advanced Aerosol Jet based additive printing method followed by thermal sintering. The sensors were tested under cyclic strain up to a temperature of 500 °C and showed a gauge factor of 3.15 ± 0.086, which is about 57% higher than that of those available commercially. The sensor thermal strain was also an order of magnitude lower than that of commercial gages for operation up to a temperature of 500 °C. An analytical model was developed to account for the enhanced performance of such printed sensors based on enhanced lateral contraction of the NP films due to the porosity, a behavior akin to cellular metamaterials. The results demonstrate the potential of 3D printing technology as a pathway to realize highly stable and high-performance sensors for high temperature applications.

  16. Game Indicators Determining Sports Performance in the NBA

    PubMed Central

    Mikołajec, Kazimierz; Maszczyk, Adam; Zając, Tomasz

    The main goal of the present study was to identify basketball game performance indicators which best determine sports level in the National Basketball Association (NBA) league. The research material consisted of all NBA game statistics at the turn of eight seasons (2003–11) and included 52 performance variables. Through detailed analysis the variables with high influence on game effectiveness were selected for final procedures. It has been proven that a limited number of factors, mostly offensive, determines sports performance in the NBA. The most critical indicators are: Win%, Offensive EFF, 3rd Quarter PPG, Win% CG, Avg Fauls and Avg Steals. In practical applications these results connected with top teams and elite players may help coaches to design better training programs. PMID:24146715

  17. Game Indicators Determining Sports Performance in the NBA.

    PubMed

    Mikołajec, Kazimierz; Maszczyk, Adam; Zając, Tomasz

    2013-01-01

    The main goal of the present study was to identify basketball game performance indicators which best determine sports level in the National Basketball Association (NBA) league. The research material consisted of all NBA game statistics at the turn of eight seasons (2003-11) and included 52 performance variables. Through detailed analysis the variables with high influence on game effectiveness were selected for final procedures. It has been proven that a limited number of factors, mostly offensive, determines sports performance in the NBA. The most critical indicators are: Win%, Offensive EFF, 3rd Quarter PPG, Win% CG, Avg Fauls and Avg Steals. In practical applications these results connected with top teams and elite players may help coaches to design better training programs.

  18. Study of the seismic performance of hybrid A-frame micropile/MSE (mechanically stabilized earth) wall

    NASA Astrophysics Data System (ADS)

    Chen, Yumin; Zhang, Zhichao; Liu, Hanlong

    2017-04-01

    The Hybrid A-Frame Micropile/MSE (mechanically stabilized earth) Wall suitable for mountain roadways is put forward in this study: a pair of vertical and inclined micropiles goes through the backfill region of a highway MSE Wall from the road surface and are then anchored into the foundation. The pile cap and grade beam are placed on the pile tops, and then a road barrier is connected to the grade beam by connecting pieces. The MSE wall's global stability, local stability and impact resistance of the road barrier can be enhanced simultaneously by this design. In order to validate the serviceability of the hybrid A-frame micropile/MSE wall and the reliability of the numerical method, scale model tests and a corresponding numerical simulation were conducted. Then, the seismic performance of the MSE walls before and after reinforcement with micropiles was studied comparatively through numerical methods. The results indicate that the hybrid A-frame micropile/MSE wall can effectively control earthquake-induced deformation, differential settlement at the road surface, bearing pressure on the bottom and acceleration by means of a rigid-soft combination of micropiles and MSE. The accumulated displacement under earthquakes with amplitude of 0.1‒0.5 g is reduced by 36.3%‒46.5%, and the acceleration amplification factor on the top of the wall is reduced by 13.4%, 15.7% and 19.3% based on 0.1, 0.3 and 0.5 g input earthquake loading, respectively. In addition, the earthquake-induced failure mode of the MSE wall in steep terrain is the sliding of the MSE region along the backslope, while the micropiles effectively control the sliding trend. The maximum earthquake-induced pile bending moment is in the interface between MSE and slope foundation, so it is necessary to strengthen the reinforcement of the pile body in the interface. Hence, it is proven that the hybrid A-frame micropile/MSE wall system has good seismic performance.

  19. Anion control as a strategy to achieve high-mobility and high-stability oxide thin-film transistors.

    PubMed

    Kim, Hyun-Suk; Jeon, Sang Ho; Park, Joon Seok; Kim, Tae Sang; Son, Kyoung Seok; Seon, Jong-Baek; Seo, Seok-Jun; Kim, Sun-Jae; Lee, Eunha; Chung, Jae Gwan; Lee, Hyungik; Han, Seungwu; Ryu, Myungkwan; Lee, Sang Yoon; Kim, Kinam

    2013-01-01

    Ultra-definition, large-area displays with three-dimensional visual effects represent megatrend in the current/future display industry. On the hardware level, such a "dream" display requires faster pixel switching and higher driving current, which in turn necessitate thin-film transistors (TFTs) with high mobility. Amorphous oxide semiconductors (AOS) such as In-Ga-Zn-O are poised to enable such TFTs, but the trade-off between device performance and stability under illumination critically limits their usability, which is related to the hampered electron-hole recombination caused by the oxygen vacancies. Here we have improved the illumination stability by substituting oxygen with nitrogen in ZnO, which may deactivate oxygen vacancies by raising valence bands above the defect levels. Indeed, the stability under illumination and electrical bias is superior to that of previous AOS-based TFTs. By achieving both mobility and stability, it is highly expected that the present ZnON TFTs will be extensively deployed in next-generation flat-panel displays.

  20. Anion control as a strategy to achieve high-mobility and high-stability oxide thin-film transistors

    PubMed Central

    Kim, Hyun-Suk; Jeon, Sang Ho; Park, Joon Seok; Kim, Tae Sang; Son, Kyoung Seok; Seon, Jong-Baek; Seo, Seok-Jun; Kim, Sun-Jae; Lee, Eunha; Chung, Jae Gwan; Lee, Hyungik; Han, Seungwu; Ryu, Myungkwan; Lee, Sang Yoon; Kim, Kinam

    2013-01-01

    Ultra-definition, large-area displays with three-dimensional visual effects represent megatrend in the current/future display industry. On the hardware level, such a “dream” display requires faster pixel switching and higher driving current, which in turn necessitate thin-film transistors (TFTs) with high mobility. Amorphous oxide semiconductors (AOS) such as In-Ga-Zn-O are poised to enable such TFTs, but the trade-off between device performance and stability under illumination critically limits their usability, which is related to the hampered electron-hole recombination caused by the oxygen vacancies. Here we have improved the illumination stability by substituting oxygen with nitrogen in ZnO, which may deactivate oxygen vacancies by raising valence bands above the defect levels. Indeed, the stability under illumination and electrical bias is superior to that of previous AOS-based TFTs. By achieving both mobility and stability, it is highly expected that the present ZnON TFTs will be extensively deployed in next-generation flat-panel displays. PMID:23492854

  1. Rotordynamic Instability Problems in High-Performance Turbomachinery, 1986

    NASA Technical Reports Server (NTRS)

    1987-01-01

    The first rotordynamics workshop proceedings (NASA CP-2133, 1980) emphasized a feeling of uncertainty in predicting the stability of characteristics of high-performance turbomachinery. In the second workshop proceedings (NASA CP-2250, 1982) these uncertainities were reduced through programs established to systematically resolve problems, with emphasis on experimental validiation of the forces that influence rotordynamics. In third proceedings (NASA CP-2338, 1984) 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. The present workshop proceedings illustrates a continued trend toward a more unified view of rotordynamic instability problems and several encouraging new analytical developments.

  2. 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.

  3. Assessing stability and performance of a digitally enabled supply chain: Retrospective of a pilot in Uttar Pradesh, India.

    PubMed

    Gilbert, Sarah Skye; Thakare, Neeraj; Ramanujapuram, Arun; Akkihal, Anup

    2017-04-19

    Immunization supply chains in low resource settings do not always reach children with necessary vaccines. Digital information systems can enable real time visibility of inventory and improve vaccine availability. In 2014, a digital, mobile/web-based information system was implemented in two districts of Uttar Pradesh, India. This retrospective investigates improvements and stabilization of supply chain performance following introduction of the digital information system. All data were collected via the digital information system between March 2014 and September 2015. Data included metadata and transaction logs providing information about users, facilities, and vaccines. Metrics evaluated include adoption (system access, timeliness and completeness), data quality (error rates), and performance (stock availability on immunization session days, replenishment response duration, rate of zero stock events). Stability was defined as the phase in which quality and performance metrics achieved equilibrium rates with minimal volatility. The analysis compared performance across different facilities and vaccines. Adoption appeared sufficiently high from the onset to commence stability measures of data quality and supply chain performance. Data quality stabilized from month 3 onwards, and supply chain performance stabilized from month 13 onwards. For data quality, error rates reduced by two thirds post stabilization. Although vaccine availability remained high throughout the pilot, the three lowest-performing facilities improved from 91.05% pre-stability to 98.70% post-stability (p<0.01; t-test). Average replenishment duration (as a corrective response to stock-out events) decreased 52.3% from 4.93days to 2.35days (p<0.01; t-test). Diphtheria-tetanus-pertussis vaccine was significantly less likely to be stocked out than any other material. The results suggest that given sufficient adoption, stability is sequentially achieved, beginning with data quality, and then performance

  4. Idealized gas turbine combustor for performance research and validation of large eddy simulations.

    PubMed

    Williams, Timothy C; Schefer, Robert W; Oefelein, Joseph C; Shaddix, Christopher R

    2007-03-01

    This paper details the design of a premixed, swirl-stabilized combustor that was designed and built for the express purpose of obtaining validation-quality data for the development of large eddy simulations (LES) of gas turbine combustors. The combustor features nonambiguous boundary conditions, a geometrically simple design that retains the essential fluid dynamics and thermochemical processes that occur in actual gas turbine combustors, and unrestrictive access for laser and optical diagnostic measurements. After discussing the design detail, a preliminary investigation of the performance and operating envelope of the combustor is presented. With the combustor operating on premixed methane/air, both the equivalence ratio and the inlet velocity were systematically varied and the flame structure was recorded via digital photography. Interesting lean flame blowout and resonance characteristics were observed. In addition, the combustor exhibited a large region of stable, acoustically clean combustion that is suitable for preliminary validation of LES models.

  5. Conceptual Design Optimization of an Augmented Stability Aircraft Incorporating Dynamic Response Performance Constraints

    NASA Technical Reports Server (NTRS)

    Welstead, Jason

    2014-01-01

    This research focused on incorporating stability and control into a multidisciplinary de- sign optimization on a Boeing 737-class advanced concept called the D8.2b. A new method of evaluating the aircraft handling performance using quantitative evaluation of the sys- tem to disturbances, including perturbations, continuous turbulence, and discrete gusts, is presented. A multidisciplinary design optimization was performed using the D8.2b transport air- craft concept. The con guration was optimized for minimum fuel burn using a design range of 3,000 nautical miles. Optimization cases were run using xed tail volume coecients, static trim constraints, and static trim and dynamic response constraints. A Cessna 182T model was used to test the various dynamic analysis components, ensuring the analysis was behaving as expected. Results of the optimizations show that including stability and con- trol in the design process drastically alters the optimal design, indicating that stability and control should be included in conceptual design to avoid system level penalties later in the design process.

  6. Delivering Quality and Choice. How Performance Indicators Help and How Performance Indicators Hinder. Research Report

    ERIC Educational Resources Information Center

    Perry, Adrian; Simpson, Matthew

    2006-01-01

    This document reports on a research project held in 2005, which looked to see how performance indicators related to area needs. It shows the results of research across four Learning and Skills Council (LSC) areas, with contributions also from national stakeholders and other witnesses. Findings include: (1) Performance indicators are regarded as…

  7. 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.

  8. AOCS Performance and Stability Validation for a 160-m Solar Sail with Control-Structure Interactions

    NASA Technical Reports Server (NTRS)

    Wie, Bong; Murphy, David

    2005-01-01

    Future solar sail missions, such as NASA's Solar Polar Imager Vision, will require sails with dimensions on the order of 50-500 m. We are examining a square sail design with moving mass (trim control mass, TCM) and quadrant rotation primary actuators plus pulsed plasma thrusters (PPTs) at the mast tips for backup attitude control. Quadrant rotation is achieved via roll stabilizer bars (RSB) at the mast tips. At these sizes, given the gossamer nature of the sail supporting structures, flexible modes may be low enough to interact with the control system, especially as these actuators are located on the flexible structure itself and not on the rigid core. This paper develops a practical analysis of the flexible interactions using state-space systems and modal data from finite element models of the system. Torsion and bending of the masts during maneuvers could significantly affect the function of the actuators while activation of the membrane modes could adversely affect the thrust vector direction and magnitude. Analysis of the RSB and TCM dynamics for developing high-fidelity simulations is included. For control analysis of the flexible system, standard finite-element models of the flexible sail body are loaded and the modal data is used to create a modal coordinate state-space system. Key parameters include which modes to include, which nodes are of interest for force inputs and displacement outputs, connecting nodes through which external forces and torques are applied from the flex body to the core, any nominal momentum in the system, and any steady rates. The system is linearized about the nominal attitude and rate. The state-space plant can then be analyzed with a state-space controller, and Bode, Nyquist, step and impulse responses generated. The approach is general for any rigid core with a flexible appendage. This paper develops a compensator for a simple two-mass flex system and extrapolates the results to the solar sail. A finite element model of the 20 m

  9. Validation of key indicators in cattle farms at high risk of animal welfare problems: a qualitative case-control study.

    PubMed

    Kelly, P C; More, S J; Blake, M; Higgins, I; Clegg, T; Hanlon, A

    2013-03-23

    The objective of this study was to validate four key farmer performance indicators (KFPI), identified in a previous study, as indicators of on-farm cattle welfare incidents in Ireland, through comparison of the distribution of these KPFIs in the national herd (n=109,925) and in case herds (n=18), where welfare incidents were previously studied. The KFPIs identified were late registrations, and exits from the herd by on-farm burial, by moves to knackeries and by moves to 'herd unknown'. Data were extracted from two Department of Agriculture, Food and the Marine databases for the national herd and the case herds. All four KFPIs differed significantly between the case herds and the national herd, and one further KFPI was identified, namely moves to factories. The data for these KFPIs are routinely stored on national databases, which were established in order to comply with Regulation (EC) 1760/2000. Based on the results obtained in this study, it may be possible in the future to use routine data capture to improve strategy towards on-farm animal welfare. At this point, however, based on calculated specificities and sensitivities, none of these five KFPIs, at the cut-offs investigated and using several combinations, are able to distinguish herds with and without on-farm animal welfare problems at an accuracy suitable for routine national use in Ireland.

  10. Double-tilt in situ TEM holder with ultra-high stability.

    PubMed

    Xu, Mingjie; Dai, Sheng; Blum, Thomas; Li, Linze; Pan, Xiaoqing

    2018-05-06

    A double tilting holder with high stability is essential for acquiring atomic-scale information by transmission electron microscopy (TEM), but the availability of such holders for in situ TEM studies under various external stimuli is limited. Here, we report a unique design of seal-bearing components that provides ultra-high stability and multifunctionality (including double tilting) in an in situ TEM holder. The seal-bearing subsystem provides superior vibration damping and electrical insulation while maintaining excellent vacuum sealing and small form factor. A wide variety of in situ TEM applications including electrical measurement, STM mapping, photovoltaic studies, and CL spectroscopy can be performed on this platform with high spatial resolution imaging and electrical sensitivity at the pA scale. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. 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

  12. 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

  13. Validating the Assessment for Measuring Indonesian Secondary School Students Performance in Ecology

    NASA Astrophysics Data System (ADS)

    Rachmatullah, A.; Roshayanti, F.; Ha, M.

    2017-09-01

    The aims of this current study are validating the American Association for the Advancement of Science (AAAS) Ecology assessment and examining the performance of Indonesian secondary school students on the assessment. A total of 611 Indonesian secondary school students (218 middle school students and 393 high school students) participated in the study. Forty-five items of AAAS assessment in the topic of Interdependence in Ecosystems were divided into two versions which every version has 21 similar items. Linking item method was used as the method to combine those two versions of assessment and further Rasch analyses were utilized to validate the instrument. Independent sample t-test was also run to compare the performance of Indonesian students and American students based on the mean of item difficulty. We found that from the total of 45 items, three items were identified as misfitting items. Later on, we also found that both Indonesian middle and high school students were significantly lower performance with very large and medium effect size compared to American students. We will discuss our findings in the regard of validation issue and the connection to Indonesian student’s science literacy.

  14. High temperature deformation behavior, thermal stability and irradiation performance in Grade 92 steel

    NASA Astrophysics Data System (ADS)

    Alsagabi, Sultan

    The 9Cr-2W ferritic-martensitic steel (i.e. Grade 92 steel) possesses excellent mechanical and thermophysical properties; therefore, it has been considered to suit more challenging applications where high temperature strength and creep-rupture properties are required. The high temperature deformation mechanism was investigated through a set of tensile testing at elevated temperatures. Hence, the threshold stress concept was applied to elucidate the operating high temperature deformation mechanism. It was identified as the high temperature climb of edge dislocations due to the particle-dislocation interactions and the appropriate constitutive equation was developed. In addition, the microstructural evolution at room and elevated temperatures was investigated. For instance, the microstructural evolution under loading was more pronounced and carbide precipitation showed more coarsening tendency. The growth of these carbide precipitates, by removing W and Mo from matrix, significantly deteriorates the solid solution strengthening. The MX type carbonitrides exhibited better coarsening resistance. To better understand the thermal microstructural stability, long tempering schedules up to 1000 hours was conducted at 560, 660 and 760°C after normalizing the steel. Still, the coarsening rate of M23C 6 carbides was higher than the MX-type particles. Moreover, the Laves phase particles were detected after tempering the steel for long periods before they dissolve back into the matrix at high temperature (i.e. 720°C). The influence of the tempering temperature and time was studied for Grade 92 steel via Hollomon-Jaffe parameter. Finally, the irradiation performance of Grade 92 steel was evaluated to examine the feasibility of its eventual reactor use. To that end, Grade 92 steel was irradiated with iron (Fe2+) ions to 10, 50 and 100 dpa at 30 and 500°C. Overall, the irradiated samples showed some irradiation-induced hardening which was more noticeable at 30°C. Additionally

  15. Development of key performance indicators for prehospital emergency care.

    PubMed

    Murphy, Adrian; Wakai, Abel; Walsh, Cathal; Cummins, Fergal; O'Sullivan, Ronan

    2016-04-01

    Key performance indicators (KPIs) are used to monitor and evaluate critical areas of clinical and support functions that influence patient outcome. Traditional prehospital emergency care performance monitoring has focused solely on response time metrics. The landscape of emergency care delivery in Ireland is in the process of significant national reconfiguration. The development of KPIs is therefore considered one of the key priorities in prehospital research. The aim of this study was to develop a suite of KPIs for prehospital emergency care in Ireland. A systematic literature review of prehospital care performance measurement was undertaken followed by a three-round Delphi consensus process facilitated by a broad-based multidisciplinary group of panellists. The consensus process was conducted between June 2012 and October 2013. Each candidate indicator on the Delphi survey questionnaire was rated using a 5-point Likert-type rating scale. Agreement was defined as at least 70% of responders rating an indicator as 'agree' or 'strongly agree' on the rating scale. Data were analysed using descriptive statistics. Sensitivity of the ratings was examined for robustness by bootstrapping the original sample. Of the 78 citations identified by the systematic review, 5 relevant publications were used to select candidate indicators for the Delphi round 1 questionnaire. Response rates in Delphi rounds 1 and 2 were 89% and 83%, respectively. Following the consensus development conference, 101 KPIs reached consensus. Based on the Donabedian framework for quality-of-care indicators, 7 of the KPIs which reached agreement were structure KPIs, 74 were process KPIs and 20 were outcome KPIs. The highest ranked indicator was a process KPI ('Direct transport of ST-elevation myocardial infarction patients to a primary percutaneous intervention (PCI)-capable facility for ECG to PCI time <90 min'). Improving the quality of prehospital care requires the development and implementation of

  16. 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

  17. 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.

  18. 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.; hide

    2017-01-01

    The James Webb Space Telescope (JWST) is a large (6.5 m) cryogenic segmented aperture telescope with science instruments that cover the near- and mid-infrared from 0.6-27 microns. The large aperture not only provides high photometric sensitivity, but it also enables high angular resolution across the bandpass, with a diffraction limited point spread function (PSF) at wavelengths longer than 2 microns. The JWST PSF quality and stability are intimately tied to the science capabilities as it is convolved with the astrophysical scene. However, the PSF evolves at a variety of timescales based on telescope jitter and thermal distortion as the observatory attitude is varied. We present the image quality and stability requirements, recent predictions from integrated modeling, measurements made during ground-based testing, and performance characterization activities that will be carried out as part of the commissioning process.

  19. High-performance liquid chromatography of oligoguanylates at high pH

    NASA Technical Reports Server (NTRS)

    Stribling, R.; Deamer, D. (Principal Investigator)

    1991-01-01

    Because of the stable self-structures formed by oligomers of guanosine, standard high-performance liquid chromatography techniques for oligonucleotide fractionation are not applicable. Previously, oligoguanylate separations have been carried out at pH 12 using RPC-5 as the packing material. While RPC-5 provides excellent separations, there are several limitations, including the lack of a commercially available source. This report describes a new anion-exchange high-performance liquid chromatography method using HEMA-IEC BIO Q, which successfully separates different forms of the guanosine monomer as well as longer oligoguanylates. The reproducibility and stability at high pH suggests a versatile role for this material.

  20. 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.

  1. Validating the BISON fuel performance code to integral LWR experiments

    DOE PAGES

    Williamson, R. L.; Gamble, K. A.; Perez, D. M.; ...

    2016-03-24

    BISON is a modern finite element-based nuclear fuel performance code that has been under development at the Idaho National Laboratory (INL) since 2009. The code is applicable to both steady and transient fuel behavior and has been used to analyze a variety of fuel forms in 1D spherical, 2D axisymmetric, or 3D geometries. Code validation is underway and is the subject of this study. A brief overview of BISON’s computational framework, governing equations, and general material and behavioral models is provided. BISON code and solution verification procedures are described, followed by a summary of the experimental data used to datemore » for validation of Light Water Reactor (LWR) fuel. Validation comparisons focus on fuel centerline temperature, fission gas release, and rod diameter both before and following fuel-clad mechanical contact. Comparisons for 35 LWR rods are consolidated to provide an overall view of how the code is predicting physical behavior, with a few select validation cases discussed in greater detail. Our results demonstrate that 1) fuel centerline temperature comparisons through all phases of fuel life are very reasonable with deviations between predictions and experimental data within ±10% for early life through high burnup fuel and only slightly out of these bounds for power ramp experiments, 2) accuracy in predicting fission gas release appears to be consistent with state-of-the-art modeling and with the involved uncertainties and 3) comparison of rod diameter results indicates a tendency to overpredict clad diameter reduction early in life, when clad creepdown dominates, and more significantly overpredict the diameter increase late in life, when fuel expansion controls the mechanical response. In the initial rod diameter comparisons they were unsatisfactory and have lead to consideration of additional separate effects experiments to better understand and predict clad and fuel mechanical behavior. Results from this study are being used to

  2. Scale indicators of social exchange relationships: a comparison of relative content validity.

    PubMed

    Colquitt, Jason A; Baer, Michael D; Long, David M; Halvorsen-Ganepola, Marie D K

    2014-07-01

    Although social exchange theory has become one of the most oft-evoked theories in industrial and organizational psychology, there remains no consensus about how to measure its key mechanism: social exchange relationships (Blau, 1964). Drawing on Cropanzano and Byrne's (2000) review of contemporary social exchange theorizing, we examined the content validity of perceived support, exchange quality, affective commitment, trust, and psychological contract fulfillment as indicators of social exchange relationships. We used Hinkin and Tracey's (1999) quantitative approach to content validation, which asks participants to rate the correspondence between scale items and definitions of intended (and unintended) constructs. Our results revealed that some of the most frequently utilized indicators of social exchange relationships--perceived support and exchange quality--were significantly less content valid than rarely used options like affect-based trust. Our results also revealed that 2 direct measures--Bernerth, Armenakis, Feild, Giles, and Walker's (2007) scale and a scale created for this study--were content valid. We discuss the implications of these results for future applications of social exchange theory.

  3. “Thermal Stabilization Effect” of Al2O3 nano-dopants improves the high-temperature dielectric performance of polyimide

    PubMed Central

    Yang, Yang; He, Jinliang; Wu, Guangning; Hu, Jun

    2015-01-01

    Insulation performance of the dielectrics under extreme conditions always attracts widespread attention in electrical and electronic field. How to improve the high-temperature dielectric properties of insulation materials is one of the key issues in insulation system design of electrical devices. This paper studies the temperature-dependent corona resistance of polyimide (PI)/Al2O3 nanocomposite films under high-frequency square-wave pulse conditions. Extended corona resistant lifetime under high-temperature conditions is experimentally observed in the 2 wt% nanocomposite samples. The “thermal stabilization effect” is proposed to explain this phenomenon which attributes to a new kind of trap band caused by nanoparticles. This effect brings about superior space charge characteristics and corona resistance under high temperature with certain nano-doping concentration. The proposed theory is experimentally demonstrated by space charge analysis and thermally stimulated current (TSC) tests. This discovered effect is of profound significance on improving high-temperature dielectric properties of nanocomposites towards various applications. PMID:26597981

  4. A high stability and repeatability electrochemical scanning tunneling microscope.

    PubMed

    Xia, Zhigang; Wang, Jihao; Hou, Yubin; Lu, Qingyou

    2014-12-01

    We present a home built electrochemical scanning tunneling microscope (ECSTM) with very high stability and repeatability. Its coarse approach is driven by a closely stacked piezo motor of GeckoDrive type with four rigid clamping points, which enhances the rigidity, compactness, and stability greatly. It can give high clarity atomic resolution images without sound and vibration isolations. Its drifting rates in XY and Z directions in solution are as low as 84 pm/min and 59 pm/min, respectively. In addition, repeatable coarse approaches in solution within 2 mm travel distance show a lateral deviation less than 50 nm. The gas environment can be well controlled to lower the evaporation rate of the cell, thus reducing the contamination and elongating the measurement time. Atomically resolved SO4(2-) image on Au (111) work electrode is demonstrated to show the performance of the ECSTM.

  5. Optimization and validation of high-performance liquid chromatography method for analyzing 25-desacetyl rifampicin in human urine

    NASA Astrophysics Data System (ADS)

    Lily; Laila, L.; Prasetyo, B. E.

    2018-03-01

    A selective, reproducibility, effective, sensitive, simple and fast High-Performance Liquid Chromatography (HPLC) was developed, optimized and validated to analyze 25-Desacetyl Rifampicin (25-DR) in human urine which is from tuberculosis patient. The separation was performed by HPLC Agilent Technologies with column Agilent Eclipse XDB- Ci8 and amobile phase of 65:35 v/v methanol: 0.01 M sodium phosphate buffer pH 5.2, at 254 nm and flow rate of 0.8ml/min. The mean retention time was 3.016minutes. The method was linear from 2–10μg/ml 25-DR with a correlation coefficient of 0.9978. Standard deviation, relative standard deviation and coefficient variation of 2, 6, 10μg/ml 25-DR were 0-0.0829, 03.1752, 0-0.0317%, respectively. The recovery of 5, 7, 9μg/ml25-DR was 80.8661, 91.3480 and 111.1457%, respectively. Limits of detection (LoD) and quantification (LoQ) were 0.51 and 1.7μg/ml, respectively. The method has fulfilled the validity guidelines of the International Conference on Harmonization (ICH) bioanalytical method which includes parameters of specificity, linearity, precision, accuracy, LoD, and LoQ. The developed method is suitable for pharmacokinetic analysis of various concentrations of 25-DR in human urine.

  6. A Stability Indicating HPLC Method for the Determination of Fluvoxamine in Pharmaceutical Dosage Forms.

    PubMed

    Souri, Effat; Donyayi, Hassan; Khaniha, Reza Ahmad; Barazandeh Tehrani, Maliheh

    2015-01-01

    Fluvoxamine maleate is a selective serotonin reuptake inhibitor, which is used for the treatment of different types of depressive disorders. In the present study, a stability indicating HPLC method was developed and validated for the determination of fluvoxamine maleate. The chromatographic separation was carried out using a Nova-Pak CN column and a mixture of K2HPO4 50 mM (pH 7.0) and acetonitrile (60: 40, v/v) as the mobile phase. Target compounds were detected using a UV detector set at 235 nm. The developed method was linear over the concentration range of 1-80 μg/ml with acceptable precision (CV values < 2.0%) and accuracy (error values < 1.6%). The degradation studies showed that fluvoxamine maleate is relatively unstable under acidic, basic and oxidative conditions and also when exposed to UV radiation. On the other hand, the bulk powder of fluvoxamine maleate was relatively stable when exposed to visible light or heat. The proposed method was successfully applied for the determination of active ingredient of fluvoxamine dosage form without any interference from tablet excipients.

  7. Performance validation of the ANSER control laws for the F-18 HARV

    NASA Technical Reports Server (NTRS)

    Messina, Michael D.

    1995-01-01

    The ANSER control laws were implemented in Ada by NASA Dryden for flight test on the High Alpha Research Vehicle (HARV). The Ada implementation was tested in the hardware-in-the-loop (HIL) simulation, and results were compared to those obtained with the NASA Langley batch Fortran implementation of the control laws which are considered the 'truth model.' This report documents the performance validation test results between these implementations. This report contains the ANSER performance validation test plan, HIL versus batch time-history comparisons, simulation scripts used to generate checkcases, and detailed analysis of discrepancies discovered during testing.

  8. Performance validation of the ANSER Control Laws for the F-18 HARV

    NASA Technical Reports Server (NTRS)

    Messina, Michael D.

    1995-01-01

    The ANSER control laws were implemented in Ada by NASA Dryden for flight test on the High Alpha Research Vehicle (HARV). The Ada implementation was tested in the hardware-in-the-loop (HIL) simulation, and results were compared to those obtained with the NASA Langley batch Fortran implementation of the control laws which are considered the 'truth model'. This report documents the performance validation test results between these implementations. This report contains the ANSER performance validation test plan, HIL versus batch time-history comparisons, simulation scripts used to generate checkcases, and detailed analysis of discrepancies discovered during testing.

  9. Development and validation of empirical indices to assess the insulinemic potential of diet and lifestyle

    PubMed Central

    Tabung, Fred K.; Wang, Weike; Fung, Teresa T.; Hu, Frank B.; Smith-Warner, Stephanie A.; Chavarro, Jorge E.; Fuchs, Charles S.; Willett, Walter C.; Giovannucci, Edward L.

    2017-01-01

    The glycemic and insulin indices assess postprandial glycemic and insulin response to foods respectively, which may not reflect the long-term effects of diet on insulin response. We developed and evaluated the validity of four empirical indices to assess the insulinemic potential of usual diets and lifestyles, using dietary, lifestyle and biomarker data from the Nurses’ Health Study (NHS, n=5,812 for hyperinsulinemia, n=3,929 for insulin resistance). The four indices were: the empirical dietary index for hyperinsulinemia (EDIH) and empirical lifestyle index for hyperinsulinemia (ELIH); empirical dietary index for insulin resistance (EDIR) and empirical lifestyle index for insulin resistance (ELIR). We entered 39 food frequency questionnaire-derived food groups in stepwise linear regression models and defined indices as the patterns most predictive of fasting plasma C-peptide, for the hyperinsulinemia pathway (EDIH and ELIH); and of the triglyceride/high density lipoprotein-cholesterol (TG/HDL) ratio, for the insulin resistance pathway (EDIR and ELIR). We evaluated the validity of indices in two independent samples from NHS-II and Health Professionals Follow-up Study (HPFS) using multivariable-adjusted linear regression analyses to calculate relative concentrations of biomarkers. EDIH is comprised of 18 food groups; 13 were positively associated with C-peptide, five inversely. EDIR is comprised of 18 food groups; ten were positively associated with TG/HDL and eight inversely. Lifestyle indices had fewer dietary components, and included BMI and physical activity as components. In the validation samples, all indices significantly predicted biomarker concentrations, e.g., the relative concentrations (95%CI) of the corresponding biomarkers comparing extreme index quintiles in HPFS were: EDIH, 1.29(1.22, 1.37); ELIH, 1.78(1.68, 1.88); EDIR, 1.44(1.34, 1.55); ELIR, 2.03(1.89, 2.19); all P-trend<0.0001. The robust associations of these novel hypothesis-driven indices

  10. Reference Proteome Extracts for Mass Spec Instrument Performance Validation and Method Development

    PubMed Central

    Rosenblatt, Mike; Urh, Marjeta; Saveliev, Sergei

    2014-01-01

    Biological samples of high complexity are required to test protein mass spec sample preparation procedures and validate mass spec instrument performance. Total cell protein extracts provide the needed sample complexity. However, to be compatible with mass spec applications, such extracts should meet a number of design requirements: compatibility with LC/MS (free of detergents, etc.)high protein integrity (minimal level of protein degradation and non-biological PTMs)compatibility with common sample preparation methods such as proteolysis, PTM enrichment and mass-tag labelingLot-to-lot reproducibility Here we describe total protein extracts from yeast and human cells that meet the above criteria. Two extract formats have been developed: Intact protein extracts with primary use for sample preparation method development and optimizationPre-digested extracts (peptides) with primary use for instrument validation and performance monitoring

  11. 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.

  12. Validation of a reversed phase high performance thin layer chromatographic-densitometric method for secoisolariciresinol diglucoside determination in flaxseed.

    PubMed

    Coran, Silvia A; Bartolucci, Gianluca; Bambagiotti-Alberti, Massimo

    2008-10-17

    The validation of a HPTLC-densitometric method for the determination of secoisolariciresinol diglucoside (SDG) in flaxseed was performed improving the reproducibility of a previously reported HPTLC densitometric procedure by the use of fully wettable reversed phase plates (silica gel 60 RP18W F(254S), 10cmx10cm) with MeOH:HCOOH 0.1% (40:60, v/v) mobile phase. The analysis required only the alkaline hydrolysis in aqueous medium of undefatted samples and densitometry at 282nm of HPTLC runs. The method was validated following the protocol proposed by the Société Francaise des Sciences et Techniques Pharmaceutiques (SFSTP) giving rise to a dependable and high throughput procedure well suited to routine application. SDG was quantified in the range of 321-1071ng with RSD of repeatability and intermediate precision not exceeding 3.61% and accuracy inside the acceptance limits. Flaxseed of five cultivars of different origin was elected as test-bed.

  13. 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.

  14. 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.

  15. 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

  16. Entropy as a Gene-Like Performance Indicator Promoting Thermoelectric Materials.

    PubMed

    Liu, Ruiheng; Chen, Hongyi; Zhao, Kunpeng; Qin, Yuting; Jiang, Binbin; Zhang, Tiansong; Sha, Gang; Shi, Xun; Uher, Ctirad; Zhang, Wenqing; Chen, Lidong

    2017-10-01

    High-throughput explorations of novel thermoelectric materials based on the Materials Genome Initiative paradigm only focus on digging into the structure-property space using nonglobal indicators to design materials with tunable electrical and thermal transport properties. As the genomic units, following the biogene tradition, such indicators include localized crystal structural blocks in real space or band degeneracy at certain points in reciprocal space. However, this nonglobal approach does not consider how real materials differentiate from others. Here, this study successfully develops a strategy of using entropy as the global gene-like performance indicator that shows how multicomponent thermoelectric materials with high entropy can be designed via a high-throughput screening method. Optimizing entropy works as an effective guide to greatly improve the thermoelectric performance through either a significantly depressed lattice thermal conductivity down to its theoretical minimum value and/or via enhancing the crystal structure symmetry to yield large Seebeck coefficients. The entropy engineering using multicomponent crystal structures or other possible techniques provides a new avenue for an improvement of the thermoelectric performance beyond the current methods and approaches. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Prospects for spinel-stabilized, high-capacity lithium-ion battery cathodes

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

    Croy, Jason R.; Park, Joong Sun; Shin, Youngho

    Herein we report early results on efforts to optimize the electrochemical performance of a cathode composed of a lithium- and manganese-rich “layered-layered-spinel” material for lithium-ion battery applications. Pre-pilot scale synthesis leads to improved particle properties compared with lab-scale efforts, resulting in high capacities (≳200 mAh/g) and good energy densities (>700 Wh/kg) in tests with lithium-ion cells. Subsequent surface modifications give further improvements in rate capabilities and high-voltage stability. These results bode well for advances in the performance of this class of lithium- and manganese-rich cathode materials.

  18. Prospects for spinel-stabilized, high-capacity lithium-ion battery cathodes

    DOE PAGES

    Croy, Jason R.; Park, Joong Sun; Shin, Youngho; ...

    2016-10-13

    Herein we report early results on efforts to optimize the electrochemical performance of a cathode composed of a lithium- and manganese-rich “layered-layered-spinel” material for lithium-ion battery applications. Pre-pilot scale synthesis leads to improved particle properties compared with lab-scale efforts, resulting in high capacities (≳200 mAh/g) and good energy densities (>700 Wh/kg) in tests with lithium-ion cells. Subsequent surface modifications give further improvements in rate capabilities and high-voltage stability. These results bode well for advances in the performance of this class of lithium- and manganese-rich cathode materials.

  19. Extra-analytical quality indicators and laboratory performances.

    PubMed

    Sciacovelli, Laura; Aita, Ada; Plebani, Mario

    2017-07-01

    In the last few years much progress has been made in raising the awareness of laboratory medicine professionals about the effectiveness of quality indicators (QIs) in monitoring, and improving upon, performances in the extra-analytical phases of the Total Testing Process (TTP). An effective system for management of QIs includes the implementation of an internal assessment system and participation in inter-laboratory comparison. A well-designed internal assessment system allows the identification of critical activities and their systematic monitoring. Active participation in inter-laboratory comparison provides information on the performance level of one laboratory with respect to that of other participating laboratories. In order to guarantee the use of appropriate QIs and facilitate their implementation, many laboratories have adopted the Model of Quality Indicators (MQI) proposed by Working Group "Laboratory Errors and Patient Safety" (WG-LEPS) of IFCC, since 2008, which is the result of international consensus and continuous experimentation, and updating to meet new, constantly emerging needs. Data from participating laboratories are collected monthly and reports describing the statistical results and evaluating laboratory data, utilizing the Six Sigma metric, issued regularly. Although the results demonstrate that the processes need to be improved upon, overall the comparison with data collected in 2014 shows a general stability of quality levels and that an improvement has been achieved over time for some activities. The continuous monitoring of QI data allows identification all possible improvements, thus highlighting the value of participation in the inter-laboratory program proposed by WG-LEPS. The active participation of numerous laboratories will guarantee an ever more significant State-of-the-Art, promote the reduction of errors and improve quality of the TTP, thus guaranteeing patient safety. Copyright © 2017. Published by Elsevier Inc.

  20. High Reynolds Number Effects on HSCT Stability and Control Characteristics

    NASA Technical Reports Server (NTRS)

    Elzey, Michael B.; Owens, Lewis R., Jr.; Wahls, Richard A.; Wilson, Douglas L.

    1999-01-01

    Two wind tunnel tests during 1995 in the National Transonic Facility (NTF 070 and 073) served to define Reynolds number effects on longitudinal and lateral-directional stability and control. Testing was completed at both high lift and transonic conditions. The effect of Reynolds number on the total airplane configuration, horizontal and vertical tail effectiveness, forebody chine performance, rudder control and model aeroelastics was investigated. This paper will present pertinent stability and control results from these two test entries. Note that while model aeroelastic effects are examined in this presentation, no corrections for these effects have been made to the data.

  1. High-temperature earth-storable propellant acoustic cavity technology. [for combustion stability

    NASA Technical Reports Server (NTRS)

    Oberg, C. L.; Hines, W. S.; Falk, A. Y.

    1974-01-01

    Design criteria, methods and data, were developed to permit effective design of acoustic cavities for use in regeneratively cooled OME-type engines. This information was developed experimentally from two series of motor firings with high-temperature fuel during which the engine stability was evaluated under various conditions and with various cavity configurations. Supplementary analyses and acoustic model testing were used to aid cavity design and interpretation of results. Results from this program clearly indicate that dynamic stability in regeneratively cooled OME-type engines can be ensured through the use of acoustic cavities. Moreover, multiple modes of instability were successfully suppressed with the cavity.

  2. Image quality validation of Sentinel 2 Level-1 products: performance status at the beginning of the constellation routine phase

    NASA Astrophysics Data System (ADS)

    Francesconi, Benjamin; Neveu-VanMalle, Marion; Espesset, Aude; Alhammoud, Bahjat; Bouzinac, Catherine; Clerc, Sébastien; Gascon, Ferran

    2017-09-01

    Sentinel-2 is an Earth Observation mission developed by the European Space Agency (ESA) in the frame of the Copernicus program of the European Commission. The mission is based on a constellation of 2-satellites: Sentinel-2A launched in June 2015 and Sentinel-2B launched in March 2017. It offers an unprecedented combination of systematic global coverage of land and coastal areas, a high revisit of five days at the equator and 2 days at mid-latitudes under the same viewing conditions, high spatial resolution, and a wide field of view for multispectral observations from 13 bands in the visible, near infrared and short wave infrared range of the electromagnetic spectrum. The mission performances are routinely and closely monitored by the S2 Mission Performance Centre (MPC), including a consortium of Expert Support Laboratories (ESL). This publication focuses on the Sentinel-2 Level-1 product quality validation activities performed by the MPC. It presents an up-to-date status of the Level-1 mission performances at the beginning of the constellation routine phase. Level-1 performance validations routinely performed cover Level-1 Radiometric Validation (Equalisation Validation, Absolute Radiometry Vicarious Validation, Absolute Radiometry Cross-Mission Validation, Multi-temporal Relative Radiometry Vicarious Validation and SNR Validation), and Level-1 Geometric Validation (Geolocation Uncertainty Validation, Multi-spectral Registration Uncertainty Validation and Multi-temporal Registration Uncertainty Validation). Overall, the Sentinel-2 mission is proving very successful in terms of product quality thereby fulfilling the promises of the Copernicus program.

  3. An extremely high stability cooling system for planet hunter

    NASA Astrophysics Data System (ADS)

    l'Allemand, J. L. Lizon a.; Becerril, S.; Mirabet, E.

    2017-12-01

    The detection of exoplanets is done by measuring very tiny periodical variations of the radial velocity of the parent star. Extremely stable spectrographs are required in order to enhance the wavelength variations of the spectral lines due to Doppler effect. CARMENES is the new high-resolution, high-stability spectrograph built for the 3.5 m telescope at the Calar Alto Observatory (CAHA, Almería, Spain) by a consortium formed by German and Spanish institutions. This instrument is composed of two separated spectrographs: VIS channel (550-1050 nm) and NIR channel (950-1700 nm). The NIR-channel spectrograph’s has been built under the responsibility of the Instituto de Astrofísica de Andalucía (IAA-CSIC). It has been manufactured, assembled, integrated and verified in the last two years, delivered in fall 2015 and commissioned in December 2015. Beside the various opto-mechanical challenges, the cooling system was one of the most demanding sub-systems of the NIR channel. Due to the highly demanding requirements applicable in terms of stability, this system arises as one of the core systems to provide outstanding stability to the channel at an operating temperature finally fixed at 140 K. Really at the edge of the state-of-the-art, the Cooling System is able to provide to the cold mass (˜1 Ton) better thermal stability than few hundredths of a degree over 24 hours (goal: 0.01K/day). The present paper describes the main technical approach, which has been taken in order to reach this very ambitious performance.

  4. 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.

  5. A PILOT STUDY OF CORE STABILITY AND ATHLETIC PERFORMANCE: IS THERE A RELATIONSHIP?

    PubMed Central

    Sharrock, Chris; Cropper, Jarrod; Mostad, Joel; Johnson, Matt

    2011-01-01

    Study Design: Correlation study Objectives: To objectively evaluate the relationship between core stability and athletic performance measures in male and female collegiate athletes. Background: The relationship between core stability and athletic performance has yet to be quantified in the available literature. The current literature does not demonstrate whether or not core strength relates to functional performance. Questions remain regarding the most important components of core stability, the role of sport specificity, and the measurement of core stability in relation to athletic performance. Methods: A sample of 35 volunteer student athletes from Asbury College (NAIA Division II) provided informed consent. Participants performed a series of five tests: double leg lowering (core stability test), the forty yard dash, the T-test, vertical jump, and a medicine ball throw. Participants performed three trials of each test in a randomized order. Results: Correlations between the core stability test and each of the other four performance tests were determined using a General Linear Model. Medicine ball throw negatively correlated to the core stability test (r –0.389, p=0.023). Participants that performed better on the core stability test had a stronger negative correlation to the medicine ball throw (r =–0.527). Gender was the most strongly correlated variable to core strength, males with a mean measurement of double leg lowering of 47.43 degrees compared to females having a mean of 54.75 degrees. Conclusions: There appears to be a link between a core stability test and athletic performance tests; however, more research is needed to provide a definitive answer on the nature of this relationship. Ideally, specific performance tests will be able to better define and to examine relationships to core stability. Future studies should also seek to determine if there are specific sub-categories of core stability which are most important to allow for optimal training and

  6. Using Lunar Observations to Validate Pointing Accuracy and Geolocation, Detector Sensitivity Stability and Static Point Response of the CERES Instruments

    NASA Technical Reports Server (NTRS)

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

    2014-01-01

    Validation of in-orbit instrument performance is a function of stability in both instrument and calibration source. This paper describes a method using lunar observations scanning near full moon by the Clouds and Earth Radiant Energy System (CERES) instruments. The Moon offers an external source whose signal variance is predictable and non-degrading. From 2006 to present, these 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 measurements studied are detector sensitivity stability, pointing accuracy and static detector point response function. This validation method also shows trends per CERES data channel of 0.8% per decade or less for Flight Models 1-4. Using instrument gimbal data and computed lunar position, the pointing error of each detector telescope, the accuracy and consistency of the alignment between the detectors can be determined. The maximum pointing error was 0.2 Deg. in azimuth and 0.17 Deg. in elevation which corresponds to an error in geolocation near nadir of 2.09 km. With the exception of one detector, all instruments were found to have consistent detector alignment from 2006 to present. All alignment error was within 0.1o with most detector telescopes showing a consistent alignment offset of less than 0.02 Deg.

  7. Characterizing Cognitive Performance in a Large Longitudinal Study of Aging with Computerized Semantic Indices of Verbal Fluency

    PubMed Central

    Pakhomov, Serguei VS; Eberly, Lynn; Knopman, David

    2016-01-01

    A computational approach for estimating several indices of performance on the animal category verbal fluency task was validated, and examined in a large longitudinal study of aging. The performance indices included the traditional verbal fluency score, size of semantic clusters, density of repeated words, as well as measures of semantic and lexical diversity. Change over time in these measures was modeled using mixed effects regression in several groups of participants, including those that remained cognitively normal throughout the study (CN) and those that were diagnosed with mild cognitive impairment (MCI) or Alzheimer’s disease (AD) dementia at some point subsequent to the baseline visit. The results of the study show that, with the exception of mean cluster size, the indices showed significantly greater declines in the MCI and AD dementia groups as compared to CN participants. Examination of associations between the indices and cognitive domains of memory, attention and visuospatial functioning showed that the traditional verbal fluency scores were associated with declines in all three domains, whereas semantic and lexical diversity measures were associated with declines only in the visuospatial domain. Baseline repetition density was associated with declines in memory and visuospatial domains. Examination of lexical and semantic diversity measures in subgroups with high vs. low attention scores (but normal functioning in other domains) showed that the performance of individuals with low attention was influenced more by word frequency rather than strength of semantic relatedness between words. These findings suggest that various automatically semantic indices may be used to examine various aspects of cognitive performance affected by dementia. PMID:27245645

  8. The Reliability and Validity of Protocols for the Assessment of Endurance Sports Performance: An Updated Review

    ERIC Educational Resources Information Center

    Stevens, Christopher John; Dascombe, Ben James

    2015-01-01

    Sports performance testing is one of the most common and important measures used in sport science. Performance testing protocols must have high reliability to ensure any changes are not due to measurement error or inter-individual differences. High validity is also important to ensure test performance reflects true performance. Time-trial…

  9. 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.

  10. Application of normal fluorescence and stability-indicating derivative synchronous fluorescence spectroscopy for the determination of gliquidone in presence of its fluorescent alkaline degradation product

    NASA Astrophysics Data System (ADS)

    El-ghobashy, Mohamed R.; Yehia, Ali M.; Helmy, Aya H.; Youssef, Nadia F.

    2018-01-01

    Simple, smart and sensitive normal fluorescence and stability-indicating derivative synchronous spectrofluorimetric methods have been developed and validated for the determination of gliquidone in the drug substance and drug product. Normal spectrofluorimetric method of gliquidone was established in methanol at λ excitation 225 nm and λ emission 400 nm in concentration range 0.2-3 μg/ml with LOD equal 0.028. The fluorescence quantum yield of gliquidone was calculated using quinine sulfate as a reference and found to be 0.542. Stability-indicating first and third derivative synchronous fluorescence spectroscopy were successfully utilized to overcome the overlapped spectra in normal fluorescence of gliquidone and its alkaline degradation product. Derivative synchronous methods are based on using the synchronous fluorescence of gliquidone and its degradation product in methanol at Δ λ50 nm. Peak amplitude in the first derivative of synchronous fluorescence spectra was measured at 309 nm where degradation product showed zero-crossing without interference. The peak amplitudes in the third derivative of synchronous fluorescence spectra, peak to trough were measured at 316,329 nm where degradation product showed zero-crossing. The different experimental parameters affecting the normal and synchronous fluorescence intensity of gliquidone were studied and optimized. Moreover, the cited methods have been validated as per ICH guidelines. The peak amplitude-concentration plots of the derivative synchronous fluorescence were linear over the concentration range 0.05-2 μg/ml for gliquidone. Limits of detection were 0.020 and 0.022 in first and third derivative synchronous spectra, respectively. The adopted methods were successfully applied to commercial tablets and the results demonstrated that the derivative synchronous fluorescence spectroscopy is a powerful stability-indicating method, suitable for routine use with a short analysis time. Statistical comparison between

  11. 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.

  12. Validated determination of primulasaponins in primula root by a high-performance-thin-layer-chromatography densitometric approach.

    PubMed

    Coran, Silvia A; Mulas, Stefano

    2012-11-01

    A novel HPTLC-densitometric method was developed for separation and quantitation of primulasaponin I and II in different matrices. HPTLC silica gel 60 F254(S), 20 cm × 10 cm, plates with ethyl acetate:water:formic acid (5:1:1 v/v) as the mobile phase were used. Densitometric determinations were performed in reflectance mode at 540 nm after derivatization with vanillin reagent. The method was validated giving rise to a dependable and high throughput procedure well suited to routine applications. Primulasaponins were quantified in the range of 150-450 ng with RSD of repeatability and intermediate precision between 0.8 and 1.4% and accuracy within the acceptance limits. The method was tested on commercial herbal medicinal preparations claiming to contain primula root extract. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. High-Performance Optical Frequency References for Space

    NASA Astrophysics Data System (ADS)

    Schuldt, Thilo; Döringshoff, Klaus; Milke, Alexander; Sanjuan, Josep; Gohlke, Martin; Kovalchuk, Evgeny V.; Gürlebeck, Norman; Peters, Achim; Braxmaier, Claus

    2016-06-01

    A variety of future space missions rely on the availability of high-performance optical clocks with applications in fundamental physics, geoscience, Earth observation and navigation and ranging. Examples are the gravitational wave detector eLISA (evolved Laser Interferometer Space Antenna), the Earth gravity mission NGGM (Next Generation Gravity Mission) and missions, dedicated to tests of Special Relativity, e.g. by performing a Kennedy- Thorndike experiment testing the boost dependence of the speed of light. In this context we developed optical frequency references based on Doppler-free spectroscopy of molecular iodine; compactness and mechanical and thermal stability are main design criteria. With a setup on engineering model (EM) level we demonstrated a frequency stability of about 2·10-14 at an integration time of 1 s and below 6·10-15 at integration times between 100s and 1000s, determined from a beat-note measurement with a cavity stabilized laser where a linear drift was removed from the data. A cavity-based frequency reference with focus on improved long-term frequency stability is currently under development. A specific sixfold thermal shield design based on analytical methods and numerical calculations is presented.

  14. 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)

  15. Stability of amoxicillin-clavulanate in BACTEC medium determined by high-performance liquid chromatography and bioassay.

    PubMed Central

    Moore, T D; Horton, R; Utrup, L J; Miller, L A; Poupard, J A

    1996-01-01

    The stabilities of amoxicillin (16 micrograms/ml) and clavulanate (8 micrograms/ml), alone and in combination in BACTEC medium (Middlebrook 7H12B medium), were determined by high-performance liquid chromatography (HPLC) and bioassay. By HPLC, the half-life of amoxicillin (trihydrate and sodium) in combination with clavulanate in nonradiolabelled 7H12B medium was 6.7 days, whereas the half-life of clavulanate in combination with amoxicillin was 2.0 days. By bioassay, the half-lives of amoxicillin trihydrate and clavulanate in radiolabelled 7H12B medium were comparable (7 and 2 days, respectively) to those determined by HPLC. When clavulanate was tested alone, the half-life was determined to be 1.88 days by HPLC and 1.87 days by bioassay. The relatively short half-life of clavulanate can be adjusted by a procedure of "topping up," or adding one-half the concentration of clavulanate every second day, in order to allow accurate amoxicillin-clavulanate MIC testing with the BACTEC mycobacterial susceptibility system. PMID:8727931

  16. Nitrogen-doped biomass/polymer composite porous carbons for high performance supercapacitor

    NASA Astrophysics Data System (ADS)

    Shu, Yu; Maruyama, Jun; Iwasaki, Satoshi; Maruyama, Shohei; Shen, Yehua; Uyama, Hiroshi

    2017-10-01

    Nitrogen-doped porous monolithic carbon (NDPMC) is obtained from biomass-derived activated carbon/polyacrylonitrile composite for the first time via a template-free thermally induced phase separation (TIPS) approach followed by KOH activation. The electrochemical results indicate that NDPMC possesses ultrahigh specific capacitance of 442 F g-1 at 1 A g-1, excellent rate capability with 81% retention rate from 1 to 100 A g-1 and outstanding cycling stability with 98% capacitance retention at 20 A g-1 after 5000 cycles. Furthermore, the evaluation of NDPMC on the practical symmetrical system also exhibits desired electrochemical performances. The novel composite carbon displays remarkable capacitance properties and the feasible, low-cost synthetic route demonstrates great potential for large-scale production of high-performance electrode materials for supercapacitors.

  17. Cross-cultural validity of Morningness-Eveningness Stability Scale improved (MESSi) in Iran, Spain and Germany.

    PubMed

    Rahafar, Arash; Randler, Christoph; Díaz-Morales, Juan F; Kasaeian, Ali; Heidari, Zeinab

    2017-01-01

    Morningness-Eveningness Stability Scale improved (MESSi) is a newly constructed measure to assess circadian types and amplitude. In this study, we applied this measure to participants from three different countries: Germany, Spain and Iran. Confirmatory factorial analysis (CFA) of MESSi displayed mediocre fit in the three countries. Comparing increasingly stringent models using multigroup confirmatory factor analyses indicated at least partial measurement invariance (metric invariance) by country for Morning Affect and Distinctness subscales. Age was positively related to Morning Affect (MA), and negatively related to Eveningness (EV) and Distinctness (DI). Men reported higher MA than women, whereas women reported higher DI than men. Regarding country effect, Iranian participants reported highest MA compared to Spaniards and Germans, whereas Germans reported higher DI compared to Iranians and Spaniards. As a conclusion, our study corroborated the validity and reliability of MESSi across three different countries with different geographical and cultural characteristics.

  18. Validated stability-indicating spectrofluorimetric methods for the determination of ebastine in pharmaceutical preparations

    PubMed Central

    2011-01-01

    Two sensitive, selective, economic, and validated spectrofluorimetric methods were developed for the determination of ebastine (EBS) in pharmaceutical preparations depending on reaction with its tertiary amino group. Method I involves condensation of the drug with mixed anhydrides (citric and acetic anhydrides) producing a product with intense fluorescence, which was measured at 496 nm after excitation at 388 nm. Method (IIA) describes quantitative fluorescence quenching of eosin upon addition of the studied drug where the decrease in the fluorescence intensity was directly proportional to the concentration of ebastine; the fluorescence quenching was measured at 553 nm after excitation at 457 nm. This method was extended to (Method IIB) to apply first and second derivative synchronous spectrofluorimetric method (FDSFS & SDSFS) for the simultaneous analysis of EBS in presence of its alkaline, acidic, and UV degradation products. The proposed methods were successfully applied for the determination of the studied compound in its dosage forms. The results obtained were in good agreement with those obtained by a comparison method. Both methods were utilized to investigate the kinetics of the degradation of the drug. PMID:21385439

  19. Fingerprint chromatogram analysis of Pseudostellaria heterophylla (Miq.) Pax root by high performance liquid chromatography.

    PubMed

    Han, Chao; Chen, Junhui; Chen, Bo; Lee, Frank Sen-Chun; Wang, Xiaoru

    2006-09-01

    A simple and reliable high performance liquid chromatographic (HPLC) method has been developed and validated for the fingerprinting of extracts from the root of Pseudostellaria heterophylla (Miq.) Pax. HPLC with gradient elution was performed on an authentic reference standard of powdered P. heterophylla (Miq.) Pax root and 11 plant samples of the root were collected from different geographic locations. The HPLC chromatograms have been standardized through the selection and identification of reference peaks and the normalization of retention times and peak intensities of all the common peaks. The standardized HPLC fingerprints show high stability and reproducibility, and thus can be used effectively for the screening analysis or quality assessment of the root or its derived products. Similarity index calculations based on cosine angle values or correlation methods have been performed on the HPLC fingerprints. As a group, the fingerprints of the P. heterophylla (Miq.) Pax samples studied are highly correlated with closely similar fingerprints. Within the group, the samples can be further divided into subgroups based on hierarchical clustering analysis (HCA). Sample grouping based on HCA coincides nicely with those based on the geographical origins of the samples. The HPLC fingerprinting techniques thus have high potential in authentication or source-tracing types of applications.

  20. Mixed cation FA x PEA 1- x PbI 3 with enhanced phase and ambient stability toward high-performance perovskite solar cells

    DOE PAGES

    Li, Nan; Zhu, Zonglong; Chueh, Chu -Chen; ...

    2016-09-26

    In this study, different from the commonly explored strategy of incorporating a smaller cation, MA + and Cs + into FAPbI 3 lattice to improve efficiency and stability, it is revealed that the introduction of phenylethylammonium iodide (PEAI) into FAPbI 3 perovksite to form mixed cation FA xPEA 1–xPbI 3 can effectively enhance both phase and ambient stability of FAPbI 3 as well as the resulting performance of the derived devices. From our experimental and theoretical calculation results, it is proposed that the larger PEA cation is capable of assembling on both the lattice surface and grain boundaries to formmore » quais-3D perovskite structures. The surrounding of PEA + ions at the crystal grain boundaries not only can serve as molecular locks to tighten FAPbI 3 domains but also passivate the surface defects to improve both phase and moisture stablity. Consequently, a high-performance (PCE:17.7%) and ambient stable FAPbI 3 solar cell could be developed« less

  1. Validation of maternal reports for low birthweight and preterm birth indicators in rural Nepal.

    PubMed

    Chang, Karen T; Mullany, Luke C; Khatry, Subarna K; LeClerq, Steven C; Munos, Melinda K; Katz, Joanne

    2018-06-01

    Tracking progress towards global newborn health targets depends largely on maternal reported data collected through large, nationally representative surveys. We evaluated the validity, across a range of recall period lengths (1 to 24 months post-delivery), of maternal report of birthweight, birth size and length of pregnancy. We compared maternal reports to reference standards of birthweights measured within 72 hours of delivery and gestational age generated from reported first day of the last menstrual period (LMP) prospectively collected as part of a population-based study (n = 1502). We calculated sensitivity, specificity, area the under the receiver operating curve (AUC) as a measure of individual-level accuracy, and the inflation factor (IF) to quantify population-level bias for each indicator. We assessed if length of recall period modified accuracy by stratifying measurements across time bins and using a modified Poisson regression with robust error variance to estimate the relative risk (RR) of correctly classifying newborns as low birthweight (LBW) or preterm, adjusting for child sex, place of delivery, maternal age, maternal education, parity, and ethnicity. The LBW indicator using maternally reported birthweight in grams had low individual-level accuracy (AUC = 0.69) and high population-level bias (inflation factor IF = 0.62). LBW using maternally reported birth size and the preterm birth indicator had lower individual-level accuracy (AUC = 0.58 and 0.56, respectively) and higher population-level bias (IF = 0.28 and 0.35, respectively) up to 24 months following birth. Length of recall time did not affect accuracy of LBW indicators. For the preterm birth indicator, accuracy did not change with length of recall up to 20 months after birth and improved slightly beyond 20 months. The use of maternal reports may underestimate and bias indicators for LBW and preterm birth. In settings with high prevalence of LBW and preterm births, these

  2. Validity and reliability of a novel measure of activity performance and participation.

    PubMed

    Murgatroyd, Phil; Karimi, Leila

    2016-01-01

    To develop and evaluate an innovative clinician-rated measure, which produces global numerical ratings of activity performance and participation. Repeated measures study with 48 community-dwelling participants investigating clinical sensibility, comprehensiveness, practicality, inter-rater reliability, responsiveness, sensitivity and concurrent validity with Barthel Index. Important clinimetric characteristics including comprehensiveness and ease of use were rated >8/10 by clinicians. Inter-rater reliability was excellent on the summary scores (intraclass correlation of 0.95-0.98). There was good evidence that the new outcome measure distinguished between known high and low functional scoring groups, including both responsiveness to change and sensitivity at the same time point in numerous tests. Concurrent validity with the Barthel Index was fair to high (Spearman Rank Order Correlation 0.32-0.85, p > 0.05). The new measure's summary scores were nearly twice as responsive to change compared with the Barthel Index. Other more detailed data could also be generated by the new measure. The Activity Performance Measure is an innovative outcome instrument that showed good clinimetric qualities in this initial study. Some of the results were strong, given the sample size, and further trial and evaluation is appropriate. Implications for Rehabilitation The Activity Performance Measure is an innovative outcome measure covering activity performance and participation. In an initial evaluation, it showed good clinimetric qualities including responsiveness to change, sensitivity, practicality, clinical sensibility, item coverage, inter-rater reliability and concurrent validity with the Barthel Index. Further trial and evaluation is appropriate.

  3. 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.…

  4. 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.

  5. High-rate synthesis of phosphine-stabilized undecagold nanoclusters using a multilayered micromixer.

    PubMed

    Jin, Hyung Dae; Garrison, Anna; Tseng, T; Paul, Brian K; Chang, Chih-Hung

    2010-11-05

    Growth in the potential applications of nanomaterials has led to a focus on the development of new manufacturing approaches for these materials. In particular, an increased demand due to the unique properties of nanomaterials requires a substantial yield of high-performance materials and a simultaneous reduction in the environmental impact of these processes. In this paper, a high-rate production of phosphine-stabilized undecagold nanoclusters was achieved using a layer-up strategy which involves the use of microlamination architectures; the patterning and bonding of thin layers of material (laminae) to create a multilayered micromixer in the range of 25-250 µm thick was used to step up the production of phosphine-stabilized undecagold nanoclusters. The continuous production of highly monodispersed phosphine-stabilized undecagold nanoclusters at a rate of about 11.8 (mg s(-1)) was achieved using a microreactor with a size of 1.687 cm(3). This result is about 500 times over conventional batch syntheses based on the production rate per reactor volume.

  6. High-rate synthesis of phosphine-stabilized undecagold nanoclusters using a multilayered micromixer

    NASA Astrophysics Data System (ADS)

    Jin, Hyung Dae; Garrison, Anna; Tseng, T.; Paul, Brian K.; Chang, Chih-Hung

    2010-11-01

    Growth in the potential applications of nanomaterials has led to a focus on the development of new manufacturing approaches for these materials. In particular, an increased demand due to the unique properties of nanomaterials requires a substantial yield of high-performance materials and a simultaneous reduction in the environmental impact of these processes. In this paper, a high-rate production of phosphine-stabilized undecagold nanoclusters was achieved using a layer-up strategy which involves the use of microlamination architectures; the patterning and bonding of thin layers of material (laminae) to create a multilayered micromixer in the range of 25-250 µm thick was used to step up the production of phosphine-stabilized undecagold nanoclusters. The continuous production of highly monodispersed phosphine-stabilized undecagold nanoclusters at a rate of about 11.8 (mg s - 1) was achieved using a microreactor with a size of 1.687 cm3. This result is about 500 times over conventional batch syntheses based on the production rate per reactor volume.

  7. Stability and performance tradeoffs in bi-lateral telemanipulation

    NASA Technical Reports Server (NTRS)

    Hannaford, Blake

    1989-01-01

    Kinesthetic force feedback provides measurable increase in remote manipulation system performance. Intensive computation time requirements or operation under conditions of time delay can cause serious stability problems in control-system design. Here, a simplified linear analysis of this stability problem is presented for the forward-flow generalized architecture, applying the hybrid two-port representation to express the loop gain of the traditional master-slave architecture, which can be subjected to similar analysis. The hybrid two-port representation is also used to express the effects on the fidelity of manipulation or feel of one design approach used to stabilize the forward-flow architecture. The results suggest that, when local force feedback at the slave side is used to reduce manipulator stability problems, a price is paid in terms of telemanipulation fidelity.

  8. Stability of Colistin and Colistin Methanesulfonate in Aqueous Media and Plasma as Determined by High-Performance Liquid Chromatography

    PubMed Central

    Li, Jian; Milne, Robert W.; Nation, Roger L.; Turnidge, John D.; Coulthard, Kingsley

    2003-01-01

    The stabilities of colistin and colistin methanesulfonate (CMS) in different aqueous media were studied by specific high-performance liquid chromatography (HPLC) methods. Colistin was stable in water at 4 and 37°C for up to 60 days and 120 h, respectively. However, degradation was observed when colistin was stored in isotonic phosphate buffer (0.067 M, pH 7.4) and human plasma at 37°C. The stability of CMS from three different sources in water was explored by strong-anion-exchange (SAX) HPLC for CMS and by measuring the concentrations of colistin formed from the hydrolysis of CMS. The peaks of CMS in SAX HPLC disappeared almost completely after 12 h at 37°C, but appeared to remain intact for up to 2 days at 4°C. Over the same period, there was no formation of colistin at 4°C. In water, phosphate buffer, and plasma, there was rapid formation of colistin within 24 to 48 h at 37°C from the three sources of CMS. The hydrolysis products were assumed to be a complex mixture of many different sulfomethyl derivatives, including colistin. The stability of a fourth source of CMS in Mueller-Hinton broth examined during 30 min at 37°C revealed no formation of colistin. Along with previous microbiological studies, this suggested that different sulfomethyl CMSs possess intrinsic antibacterial activity. These results will be helpful for understanding the pharmacokinetics and pharmacodynamics of colistin and CMS in humans and animals. PMID:12654671

  9. New factors in the design, operation and performance of waste-stabilization ponds

    PubMed Central

    Marais, G. v. R.

    1966-01-01

    In the developing countries, the unit costs of waste-stabilization ponds are generally low. Moreover, in the tropics and subtropics, the environmental conditions are conducive to a high level of pond performance. In view of this, the theory, operation and performance of such ponds under these conditions have been studied. It is shown that the Hermann & Gloyna and Marais & Shaw theories of the degradation action in oxidation ponds can be integrated, and that account can be taken of the effect of the sludge layer. In Lusaka, Zambia, anaerobic conditions are much more likely to occur in summer than in winter, because of intense stratification. It is confirmed that a series of maturation or oxidation ponds is more efficient than a single pond of equivalent volume. When aqua privies and septic tanks are used as anaerobic pretreatment units, the area of the primary oxidation ponds can be reduced and there is less likelihood that anaerobic conditions will develop in them in summer. The use of self-topping aqua privies, discharging through sewers to oxidation ponds, has made possible the economic installation of water-carriage systems of waste disposal in low-cost high-density housing areas. In the oxidation ponds, typhoid bacteria appear to be more resistant than indicator organisms; helminths, cysts and ova settle out; there are no snails and, if peripheral vegetation is removed, mosquitos will not breed. PMID:5296235

  10. Influence of storage conditions on the stability of monomeric anthocyanins studied by reversed-phase high-performance liquid chromatography.

    PubMed

    Morais, Helena; Ramos, Cristina; Forgács, Esther; Cserháti, Tibor; Oliviera, José

    2002-04-25

    The effect of light, storage time and temperature on the decomposition rate of monomeric anthocyanin pigments extracted from skins of grape (Vitis vinifera var. Red globe) was determined by reversed-phase high-performance liquid chromatography (RP-HPLC). The impact of various storage conditions on the pigment stability was assessed by stepwise regression analysis. RP-HPLC separated well the five anthocyanins identified and proved the presence of other unidentified pigments at lower concentrations. Stepwise regression analysis confirmed that the overall decomposition rate of monomeric anthocyanins, peonidin-3-glucoside and malvidin-3-glucoside significantly depended on the time and temperature of storage, the effect of storage time being the most important. The presence or absence of light exerted a negligible impact on the decomposition rate.

  11. Concurrent Validation of the Clinical Opiate Withdrawal Scale (COWS) and Single-Item Indices against the Clinical Institute Narcotic Assessment (CINA) Opioid Withdrawal Instrument

    PubMed Central

    Tompkins, D. Andrew; Bigelow, George E.; Harrison, Joseph A.; Johnson, Rolley E.; Fudala, Paul J.; Strain, Eric C.

    2009-01-01

    Introduction The Clinical Opiate Withdrawal Scale (COWS) is an 11-item clinician-administered scale assessing opioid withdrawal. Though commonly used in clinical practice, it has not been systematically validated. The present study validated the COWS in comparison to the validated Clinical Institute Narcotic Assessment (CINA) scale. Method Opioid-dependent volunteers were enrolled in a residential trial and stabilized on morphine 30 mg given subcutaneously four times daily. Subjects then underwent double-blind, randomized challenges of intramuscularly administered placebo and naloxone (0.4 mg) on separate days, during which the COWS, CINA, and visual analog scale (VAS) assessments were concurrently obtained. Subjects completing both challenges were included (N=46). Correlations between mean peak COWS and CINA scores as well as self-report VAS questions were calculated. Results Mean peak COWS and CINA scores of 7.6 and 24.4, respectively, occurred on average 30 minutes post-injection of naloxone. Mean COWS and CINA scores 30 minutes after placebo injection were 1.3 and 18.9, respectively. The Pearson correlation coefficient for peak COWS and CINA scores during the naloxone challenge session was 0.85 (p<0.001). Peak COWS scores also correlated well with peak VAS self-report scores of bad drug effect (r=0.57, p<0.001) and feeling sick (r=0.57, p<0.001), providing additional evidence of concurrent validity. Placebo was not associated with any significant elevation of COWS, CINA, or VAS scores, indicating discriminant validity. Cronbach’s alpha for the COWS was 0.78, indicating good internal consistency (reliability). Discussion COWS, CINA, and certain VAS items are all valid measurement tools for acute opiate withdrawal. PMID:19647958

  12. QTL validation and stability for volatile organic compounds (VOCs) in apple.

    PubMed

    Costa, Fabrizio; Cappellin, Luca; Zini, Elena; Patocchi, Andrea; Kellerhals, Markus; Komjanc, Matteo; Gessler, Cesare; Biasioli, Franco

    2013-10-01

    The aroma trait in apple is a key factor for fruit quality strongly affecting the consumer appreciation, and its detection and analysis is often an extremely laborious and time consuming procedure. Molecular markers associated to this trait can to date represent a valuable selection tool to overcome these limitations. QTL mapping is the first step in the process of targeting valuable molecular markers to be employed in marker-assisted breeding programmes (MAB). However, a validation step is usually required before a newly identified molecular marker can be implemented in marker-assisted selection. In this work the position of a set of QTLs associated to volatile organic compounds (VOCs) was confirmed and validated in three different environments in Switzerland, namely Wädenswil, Conthey and Cadenazzo, where the progeny 'Fiesta×Discovery' was replicated. For both QTL identification and validation, the phenotypic data were represented by VOCs produced by mature apple fruit and assessed with a Proton Transfer Reaction-Mass Spectrometer (PTR-MS) instrument. The QTL-VOC combined analysis performed among these three locations validated the presence of important QTLs in three specific genomic regions, two located in the linkage group 2 and one in linkage group 15, respectively, for compounds related to esters (m/z 43, 61 and 131) and to the hormone ethylene (m/z 28). The QTL set presented here confirmed that in apple some compounds are highly genetically regulated and stable across environments. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

  13. Cross-Validation of Predictor Equations for Armor Crewman Performance

    DTIC Science & Technology

    1980-01-01

    Technical Report 447 CROSS-VALIDATION OF PREDICTOR EQUATIONS FOR ARMOR CREWMAN PERFORMANCE Anthony J. Maitland , Newell K. Eaton, and Janet F. Neft...ORG. REPORT NUMBER Anthony J/ Maitland . Newell K/EatorV. and B OTATO RN UBR. 9- PERFORMING ORGANIZATION NAME AND ADDRESS I0. PROGRAM ELEMENT, PROJECT...Technical Report 447 CROSS-VALIDATION OF PREDICTOR EQUATIONS FOR ARMOR CREWMAN PERFORMANCE Anthony J. Maitland , Newell K. Eaton, Accession For and

  14. 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.

  15. Identification of sorghum hybrids with high phenotypic stability using GGE biplot methodology.

    PubMed

    Teodoro, P E; Almeida Filho, J E; Daher, R F; Menezes, C B; Cardoso, M J; Godinho, V P C; Torres, F E; Tardin, F D

    2016-06-10

    The aim of this study was to identify sorghum hybrids that have both high yield and phenotypic stability in Brazilian environments. Seven trials were conducted between February and March 2011. The experimental design was a randomized complete block with 25 treatments and three replicates. The treatments consisted of 20 simple pre-commercial hybrids and five witnesses of grain sorghum. Sorghum genotypes were analyzed by the genotype main effects + genotype environment interaction (GGE) biplot method if significant genotype x environment interaction, adaptability, and phenotypic stability were detected. GGE biplot methodology identified two groups of environments, the first composed of Água Comprida-MG, Montividiu-GO, and Vilhena- RO and the second of Guaíra-SP and Sete Lagoas-MG. The BRS 308 and 1G282 genotypes were found to have high grain yield, adaptability, and phenotypic stability and are thus indicated for cultivation in the first and second groups of environments, respectively.

  16. Assessment of environmental stability of agroserous soil according to indicator of energy potential of organic substances

    NASA Astrophysics Data System (ADS)

    Murtazina, S. G.; Gaffarova, L. G.; Murtazin, MG

    2018-01-01

    Studies of the group and fractional composition of humus have determineded that the long-term use of soil (for 20 years) without the use of fertilizers (control) leads to a decrease in the content of humic acids and fulvic acids relative to the initial soil, which indicates an increase in mineralization of the soil humus. Under the influence of a long application of high doses of mineral fertilizers, the content of mobile fractions of humic and fulvic acids in the field rotation increases in the humus content. In systems of agriculture that are not balanced by organic matter, which are predominant in most farms of the Republic of Tatarstan, the use of very high doses of potassium fertilizers is not justified energetically. To compensate for losses of humus and its energy potential in calculating organic fertilizers on backgrounds with high doses of mineral fertilizers, the humification coefficients of organic residues should be increased by 30-40% during the rotational period of 5-6 years, which will reduce the loss of energy reserves and thereby improve the ecological stability of soils and the stability of agricultural landscapes

  17. 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.

  18. 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

  19. High thermal stability fluorene-based hole-injecting material for organic light-emitting devices

    NASA Astrophysics Data System (ADS)

    Li, Lu; Jiao, Bo; Li, Sanfeng; Ma, Lin; Yu, Yue; Wu, Zhaoxin

    2016-03-01

    Novel N1,N3,N5-tris(9,9-diphenyl-9H-fluroen-2-yl)-N1,N3,N5-triphenylbenzene-1,3,5-triamine (TFADB) was synthesized and characterized as a hole-injecting material (HIM) for organic light-emitting devices (OLEDs). By incorporating fluorene group TFADB shows a high glass-transition temperature Tg > 168 °C, indicative of excellent thermal stability. TFADB-based devices exhibited the highest performance in terms of the maximum current efficiency (6.0 cd/A), maximum power efficiency (4.0 lm/W), which is improved than that of the standard device based on 4-4‧-4″Tris(N-(naphthalene-2-yl)-N-phenyl-amino)triphenylamine (2T-NATA) (5.2 cd/A, 3.6 lm/W). This material could be a promising hole-injecting material, especially for the high temperature applications of OLEDs and other organic electronic devices.

  20. Oxygen stabilization induced enhancement in superconducting characteristics of high-Tc oxides

    NASA Technical Reports Server (NTRS)

    Wu, M. K.; Chen, J. T.; Huang, C. Y.

    1991-01-01

    In an attempt to enhance the electrical and mechanical properties of the high temperature superconducting oxides, high T(sub c) composites were prepared composed of the 123 compounds and AgO. The presence of extra oxygen due to the decomposition of AgO at high temperature is found to stabilize the superconducting 123 phase. Ag is found to serve as clean flux for grain growth and precipitates as pinning center. Consequently, almost two orders of magnitude enhancement in critical current densities were also observed in these composites. In addition, these composites also show much improvement in workability and shape formation. On the other hand, proper oxygen treatment of Y5Ba6Cu11Oy was found to possibly stabilize superconducting phase with T(sub c) near 250 K. I-V, ac susceptibility, and electrical resistivity measurements indicate the existence of this ultra high T(sub c) phase in this compound. Detailed structure, microstructure, electrical, magnetic and thermal studies of the superconducting composites and the ultra high T(sub c) compound are presented and discussed.

  1. High Stability Engine Control (HISTEC): Flight Demonstration Results

    NASA Technical Reports Server (NTRS)

    Delaat, John C.; Southwick, Robert D.; Gallops, George W.; Orme, John S.

    1998-01-01

    Future aircraft turbine engines, both commercial and military, must be able to accommodate expected increased levels of steady-state and dynamic engine-face distortion. The current approach of incorporating sufficient design stall margin to tolerate these increased levels of distortion would significantly reduce performance. The High Stability Engine Control (HISTEC) program has developed technologies for an advanced, integrated engine control system that uses measurement- based 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/or decrease in fuel burn. The HISTEC concept was successfully flight demonstrated on the F-15 ACTIVE aircraft during the summer of 1997. The flight demonstration was planned and carried out in two parts, the first to show distortion estimation, and the second to show distortion accommodation. Post-flight analysis shows that the HISTEC technologies are able to successfully estimate and accommodate distortion, transiently setting the stall margin requirement on-line and in real-time. Flight demonstration of the HISTEC technologies has significantly reduced the risk of transitioning the technology to tactical and commercial engines.

  2. [Validation and adhesion to GESIDA quality indicators in patients with HIV infection].

    PubMed

    Riera, Melchor; Esteban, Herminia; Suarez, Ignacio; Palacios, Rosario; Lozano, Fernando; Blanco, Jose R; Valencia, Eulalia; Ocampo, Antonio; Amador, Concha; Frontera, Guillem; vonWichmann-de Miguel, Miguel Angel

    2016-01-01

    The objective of the study is to validate the relevant GESIDA quality indicators for HIV infection, assessing the reliability, feasibility and adherence to them. The reliability was evaluated using the reproducibility of 6 indicators in peer review, with the second observer being an outsider. The feasibility and measurement of the level of adherence to the 22 indicators was conducted with annual fragmented retrospective collection of information from specific databases or the clinical charts of the nine participating hospitals. Reliability was very high, with interobserver agreement levels higher than 95% in 5 of the 6 indicators. The median time to achieve the indicators ranged between 5 and 600minutes, but could be achieved progressively from specific databases, enabling obtaining them automatically. As regards adherence to the indicators related with the initial evaluation of the patients, instructions and suitability of the guidelines for ART, adherence to ART, follow-up in clinics, and achieve an undetectable HIV by PCR at week 48 of the ART. Indicators of quality related to the prevention of opportunistic infections and control of comorbidities, the standards set were not achieved, and significant heterogeneity was observed between hospitals. The GESIDA quality indicators of HIV infection enabled the relevant indicators to be feasibly and reliably measured, and should be collected in all the units that care for patients with HIV infection. Copyright © 2015 Elsevier España, S.L.U. and Sociedad Española de Enfermedades Infecciosas y Microbiología Clínica. All rights reserved.

  3. Highly precise stabilization of intracavity prism-based Er:fiber frequency comb using optical-microwave phase detector.

    PubMed

    Zhang, Shuangyou; Wu, Jiutao; Leng, Jianxiao; Lai, Shunnan; Zhao, Jianye

    2014-11-15

    In this Letter, we demonstrate a fully stabilized Er:fiber frequency comb by using a fiber-based, high-precision optical-microwave phase detector. To achieve high-precision and long-term phase locking of the repetition rate to a microwave reference, frequency control techniques (tuning pump power and cavity length) are combined together as its feedback. Since the pump power has been used for stabilization of the repetition rate, we introduce a pair of intracavity prisms as a regulator for carrier-envelope offset frequency, thereby phase locking one mode of the comb to the rubidium saturated absorption transition line. The stabilized comb performs the same high stability as the reference for the repetition rate and provides a residual frequency instability of 3.6×10(-13) for each comb mode. The demonstrated stabilization scheme could provide a high-precision comb for optical communication, direct frequency comb spectroscopy.

  4. 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.

  5. Developing a performance measurement framework and indicators for community health service facilities in urban China.

    PubMed

    Wong, Sabrina T; Yin, Delu; Bhattacharyya, Onil; Wang, Bin; Liu, Liqun; Chen, Bowen

    2010-11-18

    China has had no effective and systematic information system to provide guidance for strengthening PHC (Primary Health Care) or account to citizens on progress. We report on the development of the China results-based Logic Model for Community Health Facilities and Stations (CHS) and a set of relevant PHC indicators intended to measure CHS priorities. We adapted the PHC Results Based Logic Model developed in Canada and current work conducted in the community health system in China to create the China CHS Logic Model framework. We used a staged approach by first constructing the framework and indicators and then validating their content through an interactive process involving policy analysis, critical review of relevant literature and multiple stakeholder consultation. The China CHS Logic Model includes inputs, activities, outputs and outcomes with a total of 287 detailed performance indicators. In these indicators, 31 indicators measure inputs, 64 measure activities, 105 measure outputs, and 87 measure immediate (n = 65), intermediate (n = 15), or final (n = 7) outcomes. A Logic Model framework can be useful in planning, implementation, analysis and evaluation of PHC at a system and service level. The development and content validation of the China CHS Logic Model and subsequent indicators provides a means for stronger accountability and a clearer sense of overall direction and purpose needed to renew and strengthen the PHC system in China. Moreover, this work will be useful in moving towards developing a PHC information system and performance measurement across districts in urban China, and guiding the pursuit of quality in PHC.

  6. Developing a Performance Measurement Framework and Indicators for Community Health Service Facilities in Urban China

    PubMed Central

    2010-01-01

    Background China has had no effective and systematic information system to provide guidance for strengthening PHC (Primary Health Care) or account to citizens on progress. We report on the development of the China results-based Logic Model for Community Health Facilities and Stations (CHS) and a set of relevant PHC indicators intended to measure CHS priorities. Methods We adapted the PHC Results Based Logic Model developed in Canada and current work conducted in the community health system in China to create the China CHS Logic Model framework. We used a staged approach by first constructing the framework and indicators and then validating their content through an interactive process involving policy analysis, critical review of relevant literature and multiple stakeholder consultation. Results The China CHS Logic Model includes inputs, activities, outputs and outcomes with a total of 287 detailed performance indicators. In these indicators, 31 indicators measure inputs, 64 measure activities, 105 measure outputs, and 87 measure immediate (n = 65), intermediate (n = 15), or final (n = 7) outcomes. Conclusion A Logic Model framework can be useful in planning, implementation, analysis and evaluation of PHC at a system and service level. The development and content validation of the China CHS Logic Model and subsequent indicators provides a means for stronger accountability and a clearer sense of overall direction and purpose needed to renew and strengthen the PHC system in China. Moreover, this work will be useful in moving towards developing a PHC information system and performance measurement across districts in urban China, and guiding the pursuit of quality in PHC. PMID:21087516

  7. Validity And Practicality of Experiment Integrated Guided Inquiry-Based Module on Topic of Colloidal Chemistry for Senior High School Learning

    NASA Astrophysics Data System (ADS)

    Andromeda, A.; Lufri; Festiyed; Ellizar, E.; Iryani, I.; Guspatni, G.; Fitri, L.

    2018-04-01

    This Research & Development study aims to produce a valid and practical experiment integrated guided inquiry based module on topic of colloidal chemistry. 4D instructional design model was selected in this study. Limited trial of the product was conducted at SMAN 7 Padang. Instruments used were validity and practicality questionnaires. Validity and practicality data were analyzed using Kappa moment. Analysis of the data shows that Kappa moment for validity was 0.88 indicating a very high degree of validity. Kappa moments for the practicality from students and teachers were 0.89 and 0.95 respectively indicating high degree of practicality. Analysis on the module filled in by students shows that 91.37% students could correctly answer critical thinking, exercise, prelab, postlab and worksheet questions asked in the module. These findings indicate that the integrated guided inquiry based module on topic of colloidal chemistry was valid and practical for chemistry learning in senior high school.

  8. Measuring individual work performance: identifying and selecting indicators.

    PubMed

    Koopmans, Linda; Bernaards, Claire M; Hildebrandt, Vincent H; de Vet, Henrica C W; van der Beek, Allard J

    2014-01-01

    Theoretically, individual work performance (IWP) can be divided into four dimensions: task performance, contextual performance, adaptive performance, and counterproductive work behavior. However, there is no consensus on the indicators used to measure these dimensions. This study was designed to (1) identify indicators for each dimension, (2) select the most relevant indicators, and (3) determine the relative weight of each dimension in ratings of work performance. IWP indicators were identified from multiple research disciplines, via literature, existing questionnaires, and expert interviews. Subsequently, experts selected the most relevant indicators per dimension and scored the relative weight of each dimension in ratings of IWP. In total, 128 unique indicators were identified. Twenty-three of these indicators were selected by experts as most relevant for measuring IWP. Task performance determined 36% of the work performance rating, while the other three dimensions respectively determined 22%, 20% and 21% of the rating. Notable consensus was found on relevant indicators of IWP, reducing the number from 128 to 23 relevant indicators. This provides an important step towards the development of a standardized, generic and short measurement instrument for assessing IWP.

  9. Validating the performance of one-time decomposition for fMRI analysis using ICA with automatic target generation process.

    PubMed

    Yao, Shengnan; Zeng, Weiming; Wang, Nizhuan; Chen, Lei

    2013-07-01

    Independent component analysis (ICA) has been proven to be effective for functional magnetic resonance imaging (fMRI) data analysis. However, ICA decomposition requires to optimize the unmixing matrix iteratively whose initial values are generated randomly. Thus the randomness of the initialization leads to different ICA decomposition results. Therefore, just one-time decomposition for fMRI data analysis is not usually reliable. Under this circumstance, several methods about repeated decompositions with ICA (RDICA) were proposed to reveal the stability of ICA decomposition. Although utilizing RDICA has achieved satisfying results in validating the performance of ICA decomposition, RDICA cost much computing time. To mitigate the problem, in this paper, we propose a method, named ATGP-ICA, to do the fMRI data analysis. This method generates fixed initial values with automatic target generation process (ATGP) instead of being produced randomly. We performed experimental tests on both hybrid data and fMRI data to indicate the effectiveness of the new method and made a performance comparison of the traditional one-time decomposition with ICA (ODICA), RDICA and ATGP-ICA. The proposed method demonstrated that it not only could eliminate the randomness of ICA decomposition, but also could save much computing time compared to RDICA. Furthermore, the ROC (Receiver Operating Characteristic) power analysis also denoted the better signal reconstruction performance of ATGP-ICA than that of RDICA. Copyright © 2013 Elsevier Inc. All rights reserved.

  10. Validation of the solar heating and cooling high speed performance (HISPER) computer code

    NASA Technical Reports Server (NTRS)

    Wallace, D. B.

    1980-01-01

    Developed to give a quick and accurate predictions HISPER, a simplification of the TRNSYS program, achieves its computational speed by not simulating detailed system operations or performing detailed load computations. In order to validate the HISPER computer for air systems the simulation was compared to the actual performance of an operational test site. Solar insolation, ambient temperature, water usage rate, and water main temperatures from the data tapes for an office building in Huntsville, Alabama were used as input. The HISPER program was found to predict the heating loads and solar fraction of the loads with errors of less than ten percent. Good correlation was found on both a seasonal basis and a monthly basis. Several parameters (such as infiltration rate and the outside ambient temperature above which heating is not required) were found to require careful selection for accurate simulation.

  11. 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

  12. EFFECTIVE INDICES FOR MONITORING MENTAL WORKLOAD WHILE PERFORMING MULTIPLE TASKS.

    PubMed

    Hsu, Bin-Wei; Wang, Mao-Jiun J; Chen, Chi-Yuan; Chen, Fang

    2015-08-01

    This study identified several physiological indices that can accurately monitor mental workload while participants performed multiple tasks with the strategy of maintaining stable performance and maximizing accuracy. Thirty male participants completed three 10-min. simulated multitasks: MATB (Multi-Attribute Task Battery) with three workload levels. Twenty-five commonly used mental workload measures were collected, including heart rate, 12 HRV (heart rate variability), 10 EEG (electroencephalography) indices (α, β, θ, α/θ, θ/β from O1-O2 and F4-C4), and two subjective measures. Analyses of index sensitivity showed that two EEG indices, θ and α/θ (F4-C4), one time-domain HRV-SDNN (standard deviation of inter-beat intervals), and four frequency-domain HRV: VLF (very low frequency), LF (low frequency), %HF (percentage of high frequency), and LF/HF were sensitive to differentiate high workload. EEG α/θ (F4-C4) and LF/HF were most effective for monitoring high mental workload. LF/HF showed the highest correlations with other physiological indices. EEG α/θ (F4-C4) showed strong correlations with subjective measures across different mental workload levels. Operation strategy would affect the sensitivity of EEG α (F4-C4) and HF.

  13. Stability Analysis of High-Speed Boundary-Layer Flow with Gas Injection

    DTIC Science & Technology

    2014-06-01

    Vitaly G. Soudakov; Ivett A Leyva 5e. TASK NUMBER 5f. WORK UNIT NUMBER Q0AF 7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES) 8. PERFORMING...cases of low injection rates in which the N -factors in the near field region are below the critical level, shaping can produce a significant...distribution unlimited Stability analysis of high-speed boundary-layer flow with gas injection Alexander V. Fedorov* and Vitaly G. Soudakov

  14. Characterizing cognitive performance in a large longitudinal study of aging with computerized semantic indices of verbal fluency.

    PubMed

    Pakhomov, Serguei V S; Eberly, Lynn; Knopman, David

    2016-08-01

    A computational approach for estimating several indices of performance on the animal category verbal fluency task was validated, and examined in a large longitudinal study of aging. The performance indices included the traditional verbal fluency score, size of semantic clusters, density of repeated words, as well as measures of semantic and lexical diversity. Change over time in these measures was modeled using mixed effects regression in several groups of participants, including those that remained cognitively normal throughout the study (CN) and those that were diagnosed with mild cognitive impairment (MCI) or Alzheimer's disease (AD) dementia at some point subsequent to the baseline visit. The results of the study show that, with the exception of mean cluster size, the indices showed significantly greater declines in the MCI and AD dementia groups as compared to CN participants. Examination of associations between the indices and cognitive domains of memory, attention and visuospatial functioning showed that the traditional verbal fluency scores were associated with declines in all three domains, whereas semantic and lexical diversity measures were associated with declines only in the visuospatial domain. Baseline repetition density was associated with declines in memory and visuospatial domains. Examination of lexical and semantic diversity measures in subgroups with high vs. low attention scores (but normal functioning in other domains) showed that the performance of individuals with low attention was influenced more by word frequency rather than strength of semantic relatedness between words. These findings suggest that various automatically semantic indices may be used to examine various aspects of cognitive performance affected by dementia. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. Improved confinement in highly powered high performance scenarios on DIII-D

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

    Petrie, Thomas W.; Osborne, Thomas; Fenstermacher, Max E.

    DIII-D has recently demonstrated improved energy confinement by injecting neutral deuterium gas into high performance near-double null divertor (DND) plasmas during high power operation. Representative parameters for these plasmas are: q 95 = 6, P IN up to 15 MW, H 98 = 1.4–1.8, and β N = 2.5–4.0. The ion B xmore » $$\\triangledown$$B direction is away from the primary X-point. While plasma conditions at lower to moderate power input (e.g., 11 MW) are shown to be favorable to successful puff-and-pump radiating divertor applications, particularly when using argon seeds, plasma behavior at higher powers (e.g., ≥14 MW) may make successful puff-and-pump operation more problematic. In contrast to lower powered high performance plasmas, both $$\\tau$$ E and β N in the high power cases (≥14 MW) increased and ELM frequency decreased, as density was raised by deuterium gas injection. Improved performance in the higher power plasmas was tied to higher pedestal pressure, which according to peeling-ballooning mode stability analysis using the ELITE code could increase with density along the kink/peeling stability threshold, while the pedestal pressure gradient in the lower power discharges were limited by the ballooning threshold. This resulted in improved fueling efficiency and ≈10% higher $$\\tau$$ E and β N than is normally observed in comparable high performance plasmas on DIII-D. Applying the puff-and-pump radiating divertor approach at moderate versus high power input is shown to result in a much different evolution in core and pedestal plasma behavior. In conclusion, we find that injecting deuterium gas into these highly powered DND plasmas may open up a new avenue for achieving elevated plasma performance, including better fueling, but the resulting higher density may also complicate application of a radiating divertor approach to heat flux reduction in present-day tokamaks, if scenarios involving second-harmonic electron cyclotron heating are used.« less

  16. Improved confinement in highly powered high performance scenarios on DIII-D

    DOE PAGES

    Petrie, Thomas W.; Osborne, Thomas; Fenstermacher, Max E.; ...

    2017-06-09

    DIII-D has recently demonstrated improved energy confinement by injecting neutral deuterium gas into high performance near-double null divertor (DND) plasmas during high power operation. Representative parameters for these plasmas are: q 95 = 6, P IN up to 15 MW, H 98 = 1.4–1.8, and β N = 2.5–4.0. The ion B xmore » $$\\triangledown$$B direction is away from the primary X-point. While plasma conditions at lower to moderate power input (e.g., 11 MW) are shown to be favorable to successful puff-and-pump radiating divertor applications, particularly when using argon seeds, plasma behavior at higher powers (e.g., ≥14 MW) may make successful puff-and-pump operation more problematic. In contrast to lower powered high performance plasmas, both $$\\tau$$ E and β N in the high power cases (≥14 MW) increased and ELM frequency decreased, as density was raised by deuterium gas injection. Improved performance in the higher power plasmas was tied to higher pedestal pressure, which according to peeling-ballooning mode stability analysis using the ELITE code could increase with density along the kink/peeling stability threshold, while the pedestal pressure gradient in the lower power discharges were limited by the ballooning threshold. This resulted in improved fueling efficiency and ≈10% higher $$\\tau$$ E and β N than is normally observed in comparable high performance plasmas on DIII-D. Applying the puff-and-pump radiating divertor approach at moderate versus high power input is shown to result in a much different evolution in core and pedestal plasma behavior. In conclusion, we find that injecting deuterium gas into these highly powered DND plasmas may open up a new avenue for achieving elevated plasma performance, including better fueling, but the resulting higher density may also complicate application of a radiating divertor approach to heat flux reduction in present-day tokamaks, if scenarios involving second-harmonic electron cyclotron heating are used.« less

  17. 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.

  18. Relative operational performance of geosynthetics used as subgrade stabilization.

    DOT National Transportation Integrated Search

    2014-05-01

    Full-scale test sections were constructed, trafficked and monitored to compare the relative operational : performance of geosynthetics used as subgrade stabilization as well as determine which material properties are : most related to performance. Se...

  19. Review and evaluation of performance measures for survival prediction models in external validation settings.

    PubMed

    Rahman, M Shafiqur; Ambler, Gareth; Choodari-Oskooei, Babak; Omar, Rumana Z

    2017-04-18

    When developing a prediction model for survival data it is essential to validate its performance in external validation settings using appropriate performance measures. Although a number of such measures have been proposed, there is only limited guidance regarding their use in the context of model validation. This paper reviewed and evaluated a wide range of performance measures to provide some guidelines for their use in practice. An extensive simulation study based on two clinical datasets was conducted to investigate the performance of the measures in external validation settings. Measures were selected from categories that assess the overall performance, discrimination and calibration of a survival prediction model. Some of these have been modified to allow their use with validation data, and a case study is provided to describe how these measures can be estimated in practice. The measures were evaluated with respect to their robustness to censoring and ease of interpretation. All measures are implemented, or are straightforward to implement, in statistical software. Most of the performance measures were reasonably robust to moderate levels of censoring. One exception was Harrell's concordance measure which tended to increase as censoring increased. We recommend that Uno's concordance measure is used to quantify concordance when there are moderate levels of censoring. Alternatively, Gönen and Heller's measure could be considered, especially if censoring is very high, but we suggest that the prediction model is re-calibrated first. We also recommend that Royston's D is routinely reported to assess discrimination since it has an appealing interpretation. The calibration slope is useful for both internal and external validation settings and recommended to report routinely. Our recommendation would be to use any of the predictive accuracy measures and provide the corresponding predictive accuracy curves. In addition, we recommend to investigate the characteristics

  20. Performance Ratings: Designs for Evaluating Their Validity and Accuracy.

    DTIC Science & Technology

    1986-07-01

    ratees with substantial validity and with little bias due to the ethod for rating. Convergent validity and discriminant validity account for approximately...The expanded research design suggests that purpose for the ratings has little influence on the multitrait-multimethod properties of the ratings...Convergent and discriminant validity again account for substantial differences in the ratings of performance. Little method bias is present; both methods of

  1. Construct Validity of Three Clerkship Performance Assessments

    ERIC Educational Resources Information Center

    Lee, Ming; Wimmers, Paul F.

    2010-01-01

    This study examined construct validity of three commonly used clerkship performance assessments: preceptors' evaluations, OSCE-type clinical performance measures, and the NBME [National Board of Medical Examiners] medicine subject examination. Six hundred and eighty-six students taking the inpatient medicine clerkship from 2003 to 2007…

  2. 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.

  3. Exploratory study on performance measures as indicators of IS effectiveness

    NASA Technical Reports Server (NTRS)

    Bishop, Peter C.; Yoes, Cissy

    1992-01-01

    The Information Systems Directorate at JSC/NASA has undertaken the reevaluation of its performance measures process and measures. Under the direction of a quality approach it is essential to identify an external perspective of how well an organization is performing. This study was conducted with two major objectives: (1) survey and summarize the academic literature on performance measures as indicators of information systems (IS) effectiveness; and (2) survey organizations for their experience in measuring for IS effectiveness. Four approaches to measuring the effectiveness of IS performance were identified: (1) listen to the customer for the things they need; (2) align with corporate goals; (3) benchmark against well-respected organizations; and (4) ask yourself what critical factors lead to success. The list of known methods for soliciting customer feedback are as follows: (1) executive visit; (2) survey, interview, and focus group; (3) complaints and compliments; and (4) service level agreements. A common set of characteristics that satisfy customers was identified from the literature. The list includes elements such as the following: accuracy, timeliness, relevance, understandability, reliability, and completeness. Future research in this topic area should prove beneficial to determine the metrics for external validity.

  4. 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.

  5. High-throughput screening and stability optimization of anti-streptavidin IgG1 and IgG2 formulations.

    PubMed

    Alekseychyk, Larysa; Su, Cheng; Becker, Gerald W; Treuheit, Michael J; Razinkov, Vladimir I

    2014-10-01

    Selection of a suitable formulation that provides adequate product stability is an important aspect of the development of biopharmaceutical products. Stability of proteins includes not only resistance to chemical modifications but also conformational and colloidal stabilities. While chemical degradation of antibodies is relatively easy to detect and control, propensity for conformational changes and/or aggregation during manufacturing or long-term storage is difficult to predict. In many cases, the formulation factors that increase one type of stability may significantly decrease another type under the same or different conditions. Often compromise is necessary to minimize the adverse effects of an antibody formulation by careful optimization of multiple factors responsible for overall stability. In this study, high-throughput stress and characterization techniques were applied to 96 formulations of anti-streptavidin antibodies (an IgG1 and an IgG2) to choose optimal formulations. Stress and analytical methods applied in this study were 96-well plate based using an automated liquid handling system to prepare the different formulations and sample plates. Aggregation and clipping propensity were evaluated by temperature and mechanical stresses. Multivariate regression analysis of high-throughput data was performed to find statistically significant formulation factors that alter measured parameters such as monomer percentage or unfolding temperature. The results of the regression models were used to maximize the stabilities of antibodies under different formulations and to find the optimal formulation space for each molecule. Comparison of the IgG1 and IgG2 data indicated an overall greater stability of the IgG1 molecule under the conditions studied. The described method can easily be applied to both initial preformulation screening and late-stage formulation development of biopharmaceutical products. © 2014 Society for Laboratory Automation and Screening.

  6. Improving stability and curving passing performance for railway vehicles with a variable stiffness MRF rubber joint

    NASA Astrophysics Data System (ADS)

    Harris, B. J.; Sun, S. S.; Li, W. H.

    2017-03-01

    With the growing need for effective intercity transport, the need for more advanced rail vehicle technology has never been greater. The conflicting primary longitudinal suspension requirements of high speed stability and curving performance limit the development of rail vehicle technology. This paper presents a novel magnetorheological fluid based joint with variable stiffness characteristics for the purpose of overcoming this parameter conflict. Firstly, the joint design and working principle is developed. Following this, a prototype is tested by MTS to characterize its variable stiffness properties under a range of conditions. Lastly, the performance of the proposed MRF rubber joint with regard to improving train stability and curving performance is numerically evaluated.

  7. Concurrent and convergent validity of the mobility- and multidimensional-hierarchical disability categorization models with physical performance in community older adults.

    PubMed

    Hu, Ming-Hsia; Yeh, Chih-Jun; Chen, Tou-Rong; Wang, Ching-Yi

    2014-01-01

    A valid, time-efficient and easy-to-use instrument is important for busy clinical settings, large scale surveys, or community screening use. The purpose of this study was to validate the mobility hierarchical disability categorization model (an abbreviated model) by investigating its concurrent validity with the multidimensional hierarchical disability categorization model (a comprehensive model) and triangulating both models with physical performance measures in older adults. 604 community-dwelling older adults of at least 60 years in age volunteered to participate. Self-reported function on mobility, instrumental activities of daily living (IADL) and activities of daily living (ADL) domains were recorded and then the disability status determined based on both the multidimensional hierarchical categorization model and the mobility hierarchical categorization model. The physical performance measures, consisting of grip strength and usual and fastest gait speeds (UGS, FGS), were collected on the same day. Both categorization models showed high correlation (γs = 0.92, p < 0.001) and agreement (kappa = 0.61, p < 0.0001). Physical performance measures demonstrated significant different group means among the disability subgroups based on both categorization models. The results of multiple regression analysis indicated that both models individually explain similar amount of variance on all physical performances, with adjustments for age, sex, and number of comorbidities. Our results found that the mobility hierarchical disability categorization model is a valid and time efficient tool for large survey or screening use.

  8. 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.

  9. 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.

  10. Simultaneous Quantification of Syringic Acid and Kaempferol in Extracts of Bergenia Species Using Validated High-Performance Thin-Layer Chromatographic-Densitometric Method.

    PubMed

    Srivastava, Nishi; Srivastava, Amit; Srivastava, Sharad; Rawat, Ajay Kumar Singh; Khan, Abdul Rahman

    2016-03-01

    A rapid, sensitive, selective and robust quantitative densitometric high-performance thin-layer chromatographic method was developed and validated for separation and quantification of syringic acid (SYA) and kaempferol (KML) in the hydrolyzed extracts of Bergenia ciliata and Bergenia stracheyi. The separation was performed on silica gel 60F254 high-performance thin-layer chromatography plates using toluene : ethyl acetate : formic acid (5 : 4: 1, v/v/v) as the mobile phase. The quantification of SYA and KML was carried out using a densitometric reflection/absorption mode at 290 nm. A dense spot of SYA and KML appeared on the developed plate at a retention factor value of 0.61 ± 0.02 and 0.70 ± 0.01. A precise and accurate quantification was performed using linear regression analysis by plotting the peak area vs concentration 100-600 ng/band (correlation coefficient: r = 0.997, regression coefficient: R(2) = 0.996) for SYA and 100-600 ng/band (correlation coefficient: r = 0.995, regression coefficient: R(2) = 0.991) for KML. The developed method was validated in terms of accuracy, recovery and inter- and intraday study as per International Conference on Harmonisation guidelines. The limit of detection and limit of quantification of SYA and KML were determined, respectively, as 91.63, 142.26 and 277.67, 431.09 ng. The statistical data analysis showed that the method is reproducible and selective for the estimation of SYA and KML in extracts of B. ciliata and B. stracheyi. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  11. Construct validity of the Groningen Frailty Indicator established in a large sample of home-dwelling elderly persons: Evidence of stability across age and gender.

    PubMed

    Peters, L L; Boter, H; Burgerhof, J G M; Slaets, J P J; Buskens, E

    2015-09-01

    The primary objective of the present study was to evaluate the validity of the Groningen Frailty Indicator (GFI) in a sample of Dutch elderly persons participating in LifeLines, a large population-based cohort study. Additional aims were to assess differences between frail and non-frail elderly and examine which individual characteristics were associated with frailty. By December 2012, 5712 elderly persons were enrolled in LifeLines and complied with the inclusion criteria of the present study. Mann-Whitney U or Kruskal-Wallis tests were used to assess the variability of GFI-scores among elderly subgroups that differed in demographic characteristics, morbidity, obesity, and healthcare utilization. Within subgroups Kruskal-Wallis tests were also used to examine differences in GFI-scores across age groups. Multivariate logistic regression analyses were performed to assess associations between individual characteristics and frailty. The GFI discriminated between subgroups: statistically significantly higher GFI-median scores (interquartile range) were found in e.g. males (1 [0-2]), the oldest old (2 [1-3]), in elderly who were single (1 [0-2]), with lower socio economic status (1 [0-3]), with increasing co-morbidity (2 [1-3]), who were obese (2 [1-3]), and used more healthcare (2 [1-4]). Overall age had an independent and statistically significant association with GFI scores. Compared with the non-frail, frail elderly persons experienced statistically significantly more chronic stress and more social/psychological related problems. In the multivariate logistic regression model, psychological morbidity had the strongest association with frailty. The present study supports the construct validity of the GFI and provides an insight in the characteristics of (non)frail community-dwelling elderly persons participating in LifeLines. Copyright © 2015 Elsevier Inc. All rights reserved.

  12. High-Performance and Self-Powered Deep UV Photodetectors Based on High Quality 2D Boron Nitride Nanosheets

    PubMed Central

    Rivera, Manuel; Rahaman, Mostafizur; Zhou, Andrew F.; Mohammed Alzuraiqi, Waleed; Feng, Peter

    2017-01-01

    High-quality two-dimensional (2D) crystalline boron nitride nanosheets (BNNSs) were grown on silicon wafers by using pulsed plasma beam deposition techniques. Self-powered deep ultraviolet (DUV) photodetectors (PDs) based on BNNSs with Schottky contact structures are designed and fabricated. By connecting the fabricated DUV photodetector to an ammeter, the response strength, response time and recovery time to different DUV wavelengths at different intensities have been characterized using the output short circuit photocurrent without a power supply. Furthermore, effects of temperature and plasma treatment on the induced photocurrent response of detectors have also been investigated. The experimental data clearly indicate that plasma treatment would significantly improve both induced photocurrent and response time. The BNNS-based DUV photodetector is demonstrated to possess excellent performance at a temperature up to 400 °C, including high sensitivity, high signal-to-noise ratio, high spectral selectivity, high speed, and high stability, which is better than almost all reported semiconducting nanomaterial-based self-powered photodetectors. PMID:29257098

  13. The stability cycle—A universal pathway for the stability of films over topography

    NASA Astrophysics Data System (ADS)

    Schörner, Mario; Aksel, Nuri

    2018-01-01

    In the present study on the linear stability of gravity-driven Newtonian films flowing over inclined topographies, we consider a fundamental question: Is there a universal principle, being valid to describe the parametric evolution of the flow's stability chart for variations of different system parameters? For this sake, we first screened all experimental and numerical stability charts available in the literature. In a second step, we performed experiments to fill the gaps which remained. Variations of the fluid's viscosity and the topography's specific shape, amplitude, wavelength, tip width, and inclination were considered. That way, we identified a set of six characteristic patterns of stability charts to be sufficient to describe and unify all results on the linear stability of Newtonian films flowing over undulated inclines. We unveiled a universal pathway—the stability cycle—along which the linear stability charts of all considered Newtonian films flowing down periodically corrugated inclines evolved when the system parameters were changed.

  14. Highly Stable Bimetallic AuIr/TiO₂ Catalyst: Physical Origins of the Intrinsic High Stability against Sintering.

    PubMed

    Han, Chang Wan; Majumdar, Paulami; Marinero, Ernesto E; Aguilar-Tapia, Antonio; Zanella, Rodolfo; Greeley, Jeffrey; Ortalan, Volkan

    2015-12-09

    It has been a long-lived research topic in the field of heterogeneous catalysts to find a way of stabilizing supported gold catalyst against sintering. Herein, we report highly stable AuIr bimetallic nanoparticles on TiO2 synthesized by sequential deposition-precipitation. To reveal the physical origin of the high stability of AuIr/TiO2, we used aberration-corrected scanning transmission electron microscopy (STEM), STEM-tomography, and density functional theory (DFT) calculations. Three-dimensional structures of AuIr/TiO2 obtained by STEM-tomography indicate that AuIr nanoparticles on TiO2 have intrinsically lower free energy and less driving force for sintering than Au nanoparticles. DFT calculations on segregation behavior of AuIr slabs on TiO2 showed that the presence of Ir near the TiO2 surface increases the adhesion energy of the bimetallic slabs to the TiO2 and the attractive interactions between Ir and TiO2 lead to higher stability of AuIr nanoparticles as compared to Au nanoparticles.

  15. Porous Ni-Co-Mn oxides prisms for high performance electrochemical energy storage

    NASA Astrophysics Data System (ADS)

    Zhao, Jianbo; Li, Man; Li, Junru; Wei, Chengzhen; He, Yuyue; Huang, Yixuan; Li, Qiaoling

    2017-12-01

    Porous Ni-Co-Mn oxides prisms have been successfully synthesized via a facile route. The process involves the preparation of nickel-cobalt-manganese acetate hydroxide by a simple co-precipitation method and subsequently the thermal treatment. The as-synthesized Ni-Co-Mn oxides prisms had a large surface area (96.53 m2 g-1) and porous structure. As electrode materials for supercapacitors, porous Ni-Co-Mn oxides prisms showed a high specific capacitance of 1623.5 F g-1 at 1.0 A g-1. Moreover, the porous Ni-Co-Mn oxides prisms were also employed as positive electrode materials to assemble flexible solid-state asymmetric supercapacitors. The resulting flexible device had a maximum volumetric energy density (0.885 mW h cm-3) and power density (48.9 mW cm-3). Encouragingly, the flexible device exhibited good cycling stability with only about 2.2% loss after 5000 charge-discharge cycles and excellent mechanical stability. These results indicate that porous Ni-Co-Mn oxides prisms have the promising application in high performance electrochemical energy storage.

  16. Validation of MCNP6 Version 1.0 with the ENDF/B-VII.1 Cross Section Library for Plutonium Metals, Oxides, and Solutions on the High Performance Computing Platform Moonlight

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

    Chapman, Bryan Scott; Gough, Sean T.

    This report documents a validation of the MCNP6 Version 1.0 computer code on the high performance computing platform Moonlight, for operations at Los Alamos National Laboratory (LANL) that involve plutonium metals, oxides, and solutions. The validation is conducted using the ENDF/B-VII.1 continuous energy group cross section library at room temperature. The results are for use by nuclear criticality safety personnel in performing analysis and evaluation of various facility activities involving plutonium materials.

  17. Hierarchy stability moderates the effect of status on stress and performance in humans

    PubMed Central

    Knight, Erik L.; Mehta, Pranjal H.

    2017-01-01

    High social status reduces stress responses in numerous species, but the stress-buffering effect of status may dissipate or even reverse during times of hierarchical instability. In an experimental test of this hypothesis, 118 participants (57.3% female) were randomly assigned to a high- or low-status position in a stable or unstable hierarchy and were then exposed to a social-evaluative stressor (a mock job interview). High status in a stable hierarchy buffered stress responses and improved interview performance, but high status in an unstable hierarchy boosted stress responses and did not lead to better performance. This general pattern of effects was observed across endocrine (cortisol and testosterone), psychological (feeling in control), and behavioral (competence, dominance, and warmth) responses to the stressor. The joint influence of status and hierarchy stability on interview performance was explained by feelings of control and testosterone reactivity. Greater feelings of control predicted enhanced interview performance, whereas increased testosterone reactivity predicted worse performance. These results provide direct causal evidence that high status confers adaptive benefits for stress reduction and performance only when the social hierarchy is stable. When the hierarchy is unstable, high status actually exacerbates stress responses. PMID:27994160

  18. Hierarchy stability moderates the effect of status on stress and performance in humans.

    PubMed

    Knight, Erik L; Mehta, Pranjal H

    2017-01-03

    High social status reduces stress responses in numerous species, but the stress-buffering effect of status may dissipate or even reverse during times of hierarchical instability. In an experimental test of this hypothesis, 118 participants (57.3% female) were randomly assigned to a high- or low-status position in a stable or unstable hierarchy and were then exposed to a social-evaluative stressor (a mock job interview). High status in a stable hierarchy buffered stress responses and improved interview performance, but high status in an unstable hierarchy boosted stress responses and did not lead to better performance. This general pattern of effects was observed across endocrine (cortisol and testosterone), psychological (feeling in control), and behavioral (competence, dominance, and warmth) responses to the stressor. The joint influence of status and hierarchy stability on interview performance was explained by feelings of control and testosterone reactivity. Greater feelings of control predicted enhanced interview performance, whereas increased testosterone reactivity predicted worse performance. These results provide direct causal evidence that high status confers adaptive benefits for stress reduction and performance only when the social hierarchy is stable. When the hierarchy is unstable, high status actually exacerbates stress responses.

  19. Relating indices of knowledge structure coherence and accuracy to skill-based performance: Is there utility in using a combination of indices?

    PubMed

    Schuelke, Matthew J; Day, Eric Anthony; McEntire, Lauren E; Boatman, Jazmine Espejo; Wang, Xiaoqian; Kowollik, Vanessa; Boatman, Paul R

    2009-07-01

    The authors examined the relative criterion-related validity of knowledge structure coherence and two accuracy-based indices (closeness and correlation) as well as the utility of using a combination of knowledge structure indices in the prediction of skill acquisition and transfer. Findings from an aggregation of 5 independent samples (N = 958) whose participants underwent training on a complex computer simulation indicated that coherence and the accuracy-based indices yielded comparable zero-order predictive validities. Support for the incremental validity of using a combination of indices was mixed; the most, albeit small, gain came in pairing coherence and closeness when predicting transfer. After controlling for baseline skill, general mental ability, and declarative knowledge, only coherence explained a statistically significant amount of unique variance in transfer. Overall, the results suggested that the different indices largely overlap in their representation of knowledge organization, but that coherence better reflects adaptable aspects of knowledge organization important to skill transfer.

  20. High performance quantum cascade lasers: Loss, beam stability, and gain engineering

    NASA Astrophysics Data System (ADS)

    Bouzi, Pierre Michel

    Quantum Cascade (QC) lasers are semiconductor devices emitting in the mid-infrared (3-30 micron) and terahertz (30-300 micron) regions of the electromagnetic spectrum. Since their first demonstration by Jerome Faist et. al. in 1994, they have evolved very quickly into high performance devices and given rise to many applications such as trace-gas sensing, medical diagnosis, free-space communication, and light detection and ranging (LIDAR). In this thesis, we investigate a further increase of the performance of QC devices and, through meticulous device modeling and characterizations, gain a deeper understanding of several of their unique characteristics, especially their carrier transport and lifetime, their characteristic temperature, their waveguide loss and modal gain, their leakage current, and their transverse mode profile. First, in our quest to achieve higher performance, we investigate the effect of growth asymmetries on device transport characteristics. This investigation stems from recent studies on the role of interface roughness on intersubband scattering and device performance. Through a symmetric active core design, we find that interface roughness and ionized impurity scattering induced by dopant migration play a significant role in carrier transport through the device. Understanding how interface roughness affects intersubband scattering, in turn, we engineer the gain in QC devices by placing monolayer barriers at specific locations within the device band structure. These strategically placed additional thin barrier layers introduce roughness scattering into the device active region, thereby selectively decreasing the lower laser state lifetime and increasing population inversion necessary for laser action. Preliminary measurement results from modified devices reveal a 50% decrease in the emission broadening compared to the control structures, which should lead to a two-fold increase in gain. A special class of so-called "strong coupling" QC lasers

  1. 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.

  2. Key Performance Indicators for Primary Schools.

    ERIC Educational Resources Information Center

    Strand, Steve

    Focusing mostly on their application for primary schools, this document describes the educational key performance indicators (KPI) employed by the Wendsworth, England, Local Educational Authority (LEA). Indicators are divided into 3 areas, educational context, resource development, and outcomes. Contextual indicators include pupil mobility, home…

  3. 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.

  4. EEG-neurofeedback for optimising performance. II: creativity, the performing arts and ecological validity.

    PubMed

    Gruzelier, John H

    2014-07-01

    As a continuation of a review of evidence of the validity of cognitive/affective gains following neurofeedback in healthy participants, including correlations in support of the gains being mediated by feedback learning (Gruzelier, 2014a), the focus here is on the impact on creativity, especially in the performing arts including music, dance and acting. The majority of research involves alpha/theta (A/T), sensory-motor rhythm (SMR) and heart rate variability (HRV) protocols. There is evidence of reliable benefits from A/T training with advanced musicians especially for creative performance, and reliable benefits from both A/T and SMR training for novice music performance in adults and in a school study with children with impact on creativity, communication/presentation and technique. Making the SMR ratio training context ecologically relevant for actors enhanced creativity in stage performance, with added benefits from the more immersive training context. A/T and HRV training have benefitted dancers. The neurofeedback evidence adds to the rapidly accumulating validation of neurofeedback, while performing arts studies offer an opportunity for ecological validity in creativity research for both creative process and product. Copyright © 2013 Elsevier Ltd. All rights reserved.

  5. Quality assurance and stability reference (QUASAR) monitoring concept for calibration/validation

    NASA Astrophysics Data System (ADS)

    Teillet, Philippe M.; Horler, D. N.; O'Neill, Norman T.

    1997-12-01

    The paper introduces the concept that calibration/validation (cal/val) can play an essential role in bringing remote sensing to mainstream consumers in an information-based society, provided that cal/val is an integral part of a quality-assurance strategy. A market model for remote sensing is introduced and used to demonstrate that quality assurance is the key to bridging the gap between early adopters of technology and mainstream markets. The paper goes on to propose the semi-continuous monitoring of quality assurance and stability reference (QUASAR) sites as an important first step towards a cal/val infrastructure beneficial to mainstream users. Prospective QUASAR test sites are described.

  6. Oxidative degradation stability and hydrogen sulfide removal performance of dual-ligand iron chelate of Fe-EDTA/CA.

    PubMed

    Miao, Xinmei; Ma, Yiwen; Chen, Zezhi; Gong, Huijuan

    2017-09-05

    Catalytic oxidation desulfurization using chelated iron catalyst is an effective method to remove H 2 S from various gas streams including biogas. However, the ligand of ethylenediaminetetraacetic acid (EDTA), which is usually adopted to prepare chelated iron catalyst, is liable to be oxidative degraded, and leads to the loss of desulfurization performance. In order to improve the degradation stability of the iron chelate, a series of iron chelates composed of two ligands including citric acid (CA) and EDTA were prepared and the oxidative degradation stability as well as desulfurization performance of these chelated iron catalysts were studied. Results show that the iron chelate of Fe-CA is more stable than Fe-EDTA, while for the desulfurization performance, the situation is converse. For the dual-ligand iron chelates of Fe-EDTA/CA, with the increase of mol ratio of CA to EDTA in the iron chelate solution, the oxidative degradation stability increased while the desulfurization performance decreased. The results of this work showed that Fe-EDTA/CA with a mol ratio of CA:EDTA = 1:1 presents a relative high oxidative degradation stability and an acceptable desulfurization performance with over 90% of H 2 S removal efficiency.

  7. Aligned carbon nanotube/zinc oxide nanowire hybrids as high performance electrodes for supercapacitor applications

    NASA Astrophysics Data System (ADS)

    Al-Asadi, Ahmed S.; Henley, Luke Alexander; Wasala, Milinda; Muchharla, Baleeswaraiah; Perea-Lopez, Nestor; Carozo, Victor; Lin, Zhong; Terrones, Mauricio; Mondal, Kanchan; Kordas, Krisztian; Talapatra, Saikat

    2017-03-01

    Carbon nanotube/metal oxide based hybrids are envisioned as high performance electrochemical energy storage electrodes since these systems can provide improved performances utilizing an electric double layer coupled with fast faradaic pseudocapacitive charge storage mechanisms. In this work, we show that high performance supercapacitor electrodes with a specific capacitance of ˜192 F/g along with a maximum energy density of ˜3.8 W h/kg and a power density of ˜ 28 kW/kg can be achieved by synthesizing zinc oxide nanowires (ZnO NWs) directly on top of aligned multi-walled carbon nanotubes (MWCNTs). In comparison to pristine MWCNTs, these constitute a 12-fold of increase in specific capacitance as well as corresponding power and energy density values. These electrodes also possess high cycling stability and were able to retain ˜99% of their specific capacitance value over 2000 charging discharging cycles. These findings indicate potential use of a MWCNT/ZnO NW hybrid material for future electrochemical energy storage applications.

  8. Effect of high hydrostatic pressure and high dynamic pressure on stability and rheological properties of model oil-in-water emulsions

    NASA Astrophysics Data System (ADS)

    Bigikocin, Erman; Mert, Behic; Alpas, Hami

    2011-09-01

    Both static and dynamic high pressure applications provide interesting modifications in food structures which lead to new product formulations. In this study, the effects of two different treatments, high hydrostatic pressure (HHP) and high dynamic pressure (HDP), on oil-in-water emulsions were identified and compared. Microfluidization was selected from among the HDP homogenization techniques. The performance of each process was analyzed in terms of rheological modifications and emulsion stability improvements compared with the coarse emulsions. The stability of the emulsions was determined comparatively by using an analytical photo-centrifuge device employing novel analysis technology. Whey protein isolate (WPI) in combination with a food polysaccharide (xanthan gum, guar gum or locust bean gum) were used as emulsifying and stabilizing ingredients. The effective disruption of oil droplets and the degradation of polysaccharides by the shear forces under high pressure in HDP microfluidization yielded finer emulsions with lower viscosities, leading to distinctive improvements in emulsion stability. On the other hand, improvements in stability obtained with HHP treatment were due to the thickening of the emulsions mainly induced by protein unfolding. The corresponding increases in viscosity were intensified in emulsion formulations containing higher oil content. Apart from these, HHP treatment was found to be relatively more contributive to the enhancements in viscoelastic properties.

  9. Performance Indicators in Education.

    ERIC Educational Resources Information Center

    Irvine, David J.

    Evaluation of education involves assessing the effectiveness of schools and trying to determine how best to improve them. Since evaluation often deals only with the question of effectiveness, performance indicators in education are designed to make evaluation more complete. They are a set of statistical models which relate several important…

  10. 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

  11. Crucial aspects of high performance thin layer chromatography quantitative validation. The case of determination of rosmarinic acid in different matrices.

    PubMed

    Coran, Silvia A; Mulas, Stefano; Mulinacci, Nadia

    2012-01-13

    A new HPTLC method was envisaged to determine rosmarinic acid (RA) in different matrices with the aim of testing the influence of optimizing the main HPTLC operative parameters in view of a more stringent validation process. HPTLC LiChrospher silica gel 60 F254s, 20 cm × 10 cm, plates with toluene:ethyl formate:formic acid (6:4:1, v/v) as the mobile phase were used. Densitometric determinations were performed in reflectance mode at 330 nm. The method was validated giving rise to a dependable and high throughput procedure well suited to routine applications. RA was quantified in the range of 132-660 ng with RSD of repeatability and intermediate precision not exceeding 2.0% and accuracy within the acceptance limits. The method was tested on several commercial preparations containing RA in different amounts. Copyright © 2011 Elsevier B.V. All rights reserved.

  12. A simple, rapid and validated high-performance liquid chromatography method suitable for clinical measurements of human mercaptalbumin and non-mercaptalbumin.

    PubMed

    Yasukawa, Keiko; Shimosawa, Tatsuo; Okubo, Shigeo; Yatomi, Yutaka

    2018-01-01

    Background Human mercaptalbumin and human non-mercaptalbumin have been reported as markers for various pathological conditions, such as kidney and liver diseases. These markers play important roles in redox regulations throughout the body. Despite the recognition of these markers in various pathophysiologic conditions, the measurements of human mercaptalbumin and non-mercaptalbumin have not been popular because of the technical complexity and long measurement time of conventional methods. Methods Based on previous reports, we explored the optimal analytical conditions for a high-performance liquid chromatography method using an anion-exchange column packed with a hydrophilic polyvinyl alcohol gel. The method was then validated using performance tests as well as measurements of various patients' serum samples. Results We successfully established a reliable high-performance liquid chromatography method with an analytical time of only 12 min per test. The repeatability (within-day variability) and reproducibility (day-to-day variability) were 0.30% and 0.27% (CV), respectively. A very good correlation was obtained with the results of the conventional method. Conclusions A practical method for the clinical measurement of human mercaptalbumin and non-mercaptalbumin was established. This high-performance liquid chromatography method is expected to be a powerful tool enabling the expansion of clinical usefulness and ensuring the elucidation of the roles of albumin in redox reactions throughout the human body.

  13. Validation of high throughput sequencing and microbial forensics applications

    PubMed Central

    2014-01-01

    High throughput sequencing (HTS) generates large amounts of high quality sequence data for microbial genomics. The value of HTS for microbial forensics is the speed at which evidence can be collected and the power to characterize microbial-related evidence to solve biocrimes and bioterrorist events. As HTS technologies continue to improve, they provide increasingly powerful sets of tools to support the entire field of microbial forensics. Accurate, credible results allow analysis and interpretation, significantly influencing the course and/or focus of an investigation, and can impact the response of the government to an attack having individual, political, economic or military consequences. Interpretation of the results of microbial forensic analyses relies on understanding the performance and limitations of HTS methods, including analytical processes, assays and data interpretation. The utility of HTS must be defined carefully within established operating conditions and tolerances. Validation is essential in the development and implementation of microbial forensics methods used for formulating investigative leads attribution. HTS strategies vary, requiring guiding principles for HTS system validation. Three initial aspects of HTS, irrespective of chemistry, instrumentation or software are: 1) sample preparation, 2) sequencing, and 3) data analysis. Criteria that should be considered for HTS validation for microbial forensics are presented here. Validation should be defined in terms of specific application and the criteria described here comprise a foundation for investigators to establish, validate and implement HTS as a tool in microbial forensics, enhancing public safety and national security. PMID:25101166

  14. Validation of high throughput sequencing and microbial forensics applications.

    PubMed

    Budowle, Bruce; Connell, Nancy D; Bielecka-Oder, Anna; Colwell, Rita R; Corbett, Cindi R; Fletcher, Jacqueline; Forsman, Mats; Kadavy, Dana R; Markotic, Alemka; Morse, Stephen A; Murch, Randall S; Sajantila, Antti; Schmedes, Sarah E; Ternus, Krista L; Turner, Stephen D; Minot, Samuel

    2014-01-01

    High throughput sequencing (HTS) generates large amounts of high quality sequence data for microbial genomics. The value of HTS for microbial forensics is the speed at which evidence can be collected and the power to characterize microbial-related evidence to solve biocrimes and bioterrorist events. As HTS technologies continue to improve, they provide increasingly powerful sets of tools to support the entire field of microbial forensics. Accurate, credible results allow analysis and interpretation, significantly influencing the course and/or focus of an investigation, and can impact the response of the government to an attack having individual, political, economic or military consequences. Interpretation of the results of microbial forensic analyses relies on understanding the performance and limitations of HTS methods, including analytical processes, assays and data interpretation. The utility of HTS must be defined carefully within established operating conditions and tolerances. Validation is essential in the development and implementation of microbial forensics methods used for formulating investigative leads attribution. HTS strategies vary, requiring guiding principles for HTS system validation. Three initial aspects of HTS, irrespective of chemistry, instrumentation or software are: 1) sample preparation, 2) sequencing, and 3) data analysis. Criteria that should be considered for HTS validation for microbial forensics are presented here. Validation should be defined in terms of specific application and the criteria described here comprise a foundation for investigators to establish, validate and implement HTS as a tool in microbial forensics, enhancing public safety and national security.

  15. Policy and Validity Prospects for Performance-Based Assessment.

    ERIC Educational Resources Information Center

    Baker, Eva L.; And Others

    1994-01-01

    This article describes performance-based assessment as expounded by its proponents, comments on these conceptions, reviews evidence regarding the technical quality of performance-based assessment, and considers its validity under various policy options. (JDD)

  16. Tough, High-Performance, Thermoplastic Addition Polymers

    NASA Technical Reports Server (NTRS)

    Pater, Ruth H.; Proctor, K. Mason; Gleason, John; Morgan, Cassandra; Partos, Richard

    1991-01-01

    Series of addition-type thermoplastics (ATT's) exhibit useful properties. Because of their addition curing and linear structure, ATT polymers have toughness, like thermoplastics, and easily processed, like thermosets. Work undertaken to develop chemical reaction forming stable aromatic rings in backbone of ATT polymer, combining high-temperature performance and thermo-oxidative stability with toughness and easy processibility, and minimizing or eliminating necessity for tradeoffs among properties often observed in conventional polymer syntheses.

  17. Development of side-chain NLO polymer materials with high electro-optic activity and long-term stability

    NASA Astrophysics Data System (ADS)

    Huang, Diyun; Parker, Timothy; Guan, Hann Wen; Cong, Shuxin; Jin, Danliang; Dinu, Raluca; Chen, Baoquan; Tolstedt, Don; Wolf, Nick; Condon, Stephen

    2005-01-01

    The electro-optic coefficient and long-term dipole alignment stability are two major factors in the development of high performance NLO materials for the application of high-speed EO devices. We have developed a high performance non-linear organic chromophore and incorporated it into a crosslinkable side-chain polyimide system. The polymer was synthesized through stepwise grafting of the crosslinker followed by the chromophore onto the polyimide backbone via esterification. Different chromophore loading levels were achieved by adjusting the crosslinker/chromophore feeding ratio. The polyimides films were contact-poled with second-harmonic generation monitoring. A large EO coefficient value was obtained and good long-term thermal stability at 85°C was observed.

  18. 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.

  19. 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

  20. Performance indicators and indices of sludge management in urban wastewater treatment plants.

    PubMed

    Silva, C; Saldanha Matos, J; Rosa, M J

    2016-12-15

    Sludge (or biosolids) management is highly complex and has a significant cost associated with the biosolids disposal, as well as with the energy and flocculant consumption in the sludge processing units. The sludge management performance indicators (PIs) and indices (PXs) are thus core measures of the performance assessment system developed for urban wastewater treatment plants (WWTPs). The key PIs proposed cover the sludge unit production and dry solids concentration (DS), disposal/beneficial use, quality compliance for agricultural use and costs, whereas the complementary PIs assess the plant reliability and the chemical reagents' use. A key PI was also developed for assessing the phosphorus reclamation, namely through the beneficial use of the biosolids and the reclaimed water in agriculture. The results of a field study with 17 Portuguese urban WWTPs in a 5-year period were used to derive the PI reference values which are neither inherent to the PI formulation nor literature-based. Clusters by sludge type (primary, activated, trickling filter and mixed sludge) and by digestion and dewatering processes were analysed and the reference values for sludge production and dry solids were proposed for two clusters: activated sludge or biofilter WWTPs with primary sedimentation, sludge anaerobic digestion and centrifuge dewatering; activated sludge WWTPs without primary sedimentation and anaerobic digestion and with centrifuge dewatering. The key PXs are computed for the DS after each processing unit and the complementary PXs for the energy consumption and the operating conditions DS-determining. The PX reference values are treatment specific and literature based. The PI and PX system was applied to a WWTP and the results demonstrate that it diagnosis the situation and indicates opportunities and measures for improving the WWTP performance in sludge management. Copyright © 2016 Elsevier Ltd. All rights reserved.