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…

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

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.

Theoretical optimum of implant positional index design.

PubMed

Semper, W; Kraft, S; Krüger, T; Nelson, K

2009-08-01

Rotational freedom of the implant-abutment connection influences its screw joint stability; for optimization, influential factors need to be evaluated based on a previously developed closed formula. The underlying hypothesis is that the manufacturing tolerances, geometric pattern, and dimensions of the index do not influence positional stability. We used the dimensions of 5 commonly used implant systems with a clearance of 20 microm to calculate the extent of rotational freedom; a 3D simulation (SolidWorks) validated the analytical findings. Polygonal positional indices showed the highest degrees of rotational freedom. The polygonal profile displayed higher positional stability than the polygons, but less positional accuracy than the cam-groove connection. Features of a maximal rotation-safe positional index were determined. The analytical calculation of rotational freedom of implant positional indices is possible. Rotational freedom is dependent on the geometric design of the index and may be decreased by incorporating specific aspects into the positional index design.

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.

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

PubMed

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

2017-03-01

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

Development and validation of a 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.

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.

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.

Development and validation of a disease-specific scale to assess psychosocial well-being of patients living with unruptured intracranial aneurysm.

PubMed

Fujishima-Hachiya, Asami; Inoue, Tomoko

2012-12-01

Although the detection rate for unruptured intracranial aneurysm (UIA) has improved since the 1990s, the quality of life and psychosocial status of patients living with UIA have been negatively affected. However, a comprehensive assessment tool for UIA patients is still awaited. This study aimed to develop and validate a disease-specific scale to assess UIA patients' psychosocial well-being in their daily lives. On the basis of previous qualitative research, 52 items on a six-dimension scale were generated. After a pilot study, statistical analysis was conducted to examine construct validity-including convergent validity, discriminant and known-group validity, and internal reliability. Between 2010 and 2011, 124 patients across three hospitals in Japan were tested using a tentative scale. As a result of exploratory factor analysis, we identified 25 items based on five conceptually derived dimensions (psychological stability, trust in healthcare resources, satisfaction with the decision-making process, positive perception of self-management, and confidence in UIA knowledge) as a final psychosocial well-being scale for UIA patients (UIA-PW scale). Cronbach's alpha coefficients for each subscale ranged between .76 and .90, with .83 for the total score, which indicated satisfactory internal consistency. The total score for the UIA-PW scale correlated significantly with the existing quality of life and mental health scales, but it is important to note that psychological stability and positive perception of self-management were negatively correlated. Although additional investigation is needed, the UIA-PW scale shows reasonable validity and reliability in assessing psychosocial well-being of patients living with UIA.

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

PubMed Central

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

2018-01-01

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

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

PubMed

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

2018-01-01

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

Stability-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.

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.

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.

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

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

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.

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.

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%).

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.

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

PubMed

Barry, Adam E; Goodson, Patricia

2011-01-01

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

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.

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.

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

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

NASA Astrophysics Data System (ADS)

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

2017-11-01

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

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.

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.

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.

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).

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.

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.

[Reliability and validity of depression scales of Chinese version: a systematic review].

PubMed

Sun, X Y; Li, Y X; Yu, C Q; Li, L M

2017-01-10

Objective: Through systematically reviewing the reliability and validity of depression scales of Chinese version in adults in China to evaluate the psychometric properties of depression scales for different groups. Methods: Eligible studies published before 6 May 2016 were retrieved from the following database: CNKI, Wanfang, PubMed and Embase. The HSROC model of the diagnostic test accuracy (DTA) for Meta-analysis was used to calculate the pooled sensitivity and specificity of the PHQ-9. Results: A total of 44 papers evaluating the performance of depression scales were included. Results showed that the reliability and validity of the common depression scales were eligible, including the Beck depression inventory (BDI), the Hamilton depression scale (HAMD), the center epidemiological studies depression scale (CES-D), the patient health questionnaire (PHQ) and the Geriatric depression scale (GDS). The Cronbach' s coefficient of most tools were larger than 0.8, while the test-retest reliability and split-half reliability were larger than 0.7, indicating good internal consistency and stability. The criterion validity, convergent validity, discrimination validity and screening validity were acceptable though different cut-off points were recommended by different studies. The pooled sensitivity of the 11 studies evaluating PHQ-9 was 0.88 (95 %CI : 0.85-0.91) while the pooled specificity was 0.89 (95 %CI : 0.82-0.94), which demonstrated the applicability of PHQ-9 in screening depression. Conclusion: The reliability and validity of different depression scales of Chinese version are acceptable. The characteristics of different tools and study population should be taken into consideration when choosing a specific scale.

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.

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.

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.

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.

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.

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.

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

Mean Length of Utterance in Children with Specific Language Impairment and in Younger Control Children Shows Concurrent Validity and Stable and Parallel Growth Trajectories

ERIC Educational Resources Information Center

Rice, Mabel L.; Redmond, Sean M.; Hoffman, Lesa

2006-01-01

Purpose: Although mean length of utterance (MLU) is a useful benchmark in studies of children with specific language impairment (SLI), some empirical and interpretive issues are unresolved. The authors report on 2 studies examining, respectively, the concurrent validity and temporal stability of MLU equivalency between children with SLI and…

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 rights reserved.

Fractional Stability of Trunk Acceleration Dynamics of Daily-Life Walking: Toward a Unified Concept of Gait Stability

PubMed Central

Ihlen, Espen A. F.; van Schooten, Kimberley S.; Bruijn, Sjoerd M.; Pijnappels, Mirjam; van Dieën, Jaap H.

2017-01-01

Over the last decades, various measures have been introduced to assess stability during walking. All of these measures assume that gait stability may be equated with exponential stability, where dynamic stability is quantified by a Floquet multiplier or Lyapunov exponent. These specific constructs of dynamic stability assume that the gait dynamics are time independent and without phase transitions. In this case the temporal change in distance, d(t), between neighboring trajectories in state space is assumed to be an exponential function of time. However, results from walking models and empirical studies show that the assumptions of exponential stability break down in the vicinity of phase transitions that are present in each step cycle. Here we apply a general non-exponential construct of gait stability, called fractional stability, which can define dynamic stability in the presence of phase transitions. Fractional stability employs the fractional indices, α and β, of differential operator which allow modeling of singularities in d(t) that cannot be captured by exponential stability. The fractional stability provided an improved fit of d(t) compared to exponential stability when applied to trunk accelerations during daily-life walking in community-dwelling older adults. Moreover, using multivariate empirical mode decomposition surrogates, we found that the singularities in d(t), which were well modeled by fractional stability, are created by phase-dependent modulation of gait. The new construct of fractional stability may represent a physiologically more valid concept of stability in vicinity of phase transitions and may thus pave the way for a more unified concept of gait stability. PMID:28900400

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

PubMed

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

2006-09-28

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

Laboratory sample stability. Is it possible to define a consensus stability function? An example of five blood magnitudes.

PubMed

Gómez Rioja, Rubén; Martínez Espartosa, Débora; Segovia, Marta; Ibarz, Mercedes; Llopis, María Antonia; Bauça, Josep Miquel; Marzana, Itziar; Barba, Nuria; Ventura, Monserrat; García Del Pino, Isabel; Puente, Juan José; Caballero, Andrea; Gómez, Carolina; García Álvarez, Ana; Alsina, María Jesús; Álvarez, Virtudes

2018-05-05

The stability limit of an analyte in a biological sample can be defined as the time required until a measured property acquires a bias higher than a defined specification. Many studies assessing stability and presenting recommendations of stability limits are available, but differences among them are frequent. The aim of this study was to classify and to grade a set of bibliographic studies on the stability of five common blood measurands and subsequently generate a consensus stability function. First, a bibliographic search was made for stability studies for five analytes in blood: alanine aminotransferase (ALT), glucose, phosphorus, potassium and prostate specific antigen (PSA). The quality of every study was evaluated using an in-house grading tool. Second, the different conditions of stability were uniformly defined and the percent deviation (PD%) over time for each analyte and condition were scattered while unifying studies with similar conditions. From the 37 articles considered as valid, up to 130 experiments were evaluated and 629 PD% data were included (106 for ALT, 180 for glucose, 113 for phosphorus, 145 for potassium and 85 for PSA). Consensus stability equations were established for glucose, potassium, phosphorus and PSA, but not for ALT. Time is the main variable affecting stability in medical laboratory samples. Bibliographic studies differ in recommedations of stability limits mainly because of different specifications for maximum allowable error. Definition of a consensus stability function in specific conditions can help laboratories define stability limits using their own quality specifications.

Caught in the struggle with food craving: Development and validation of a new cognitive fusion measure.

PubMed

Duarte, Cristiana; Pinto-Gouveia, José; Ferreira, Cláudia; Silva, Bárbara

2016-06-01

Cognitive fusion has been related to the development and maintenance of a series of mental health difficulties. Specifically, growing research on eating psychopathology has been demonstrating the important role of cognitive fusion related to body image in these disorders. Nonetheless, cognitive fusion specifically focused on eating remained to be investigated. The current study aimed at developing and validating the Cognitive Fusion Questionnaire-Food Craving, a measure assessing the extent to which an individual is fused with food-craving undesirable and disturbing thoughts and urges. This study was conducted with distinct samples comprising men and women from the student and general population. A principal component analysis was conducted to assess the scale's structure, which was further examined in a confirmatory factor analysis. The scale's reliability and validities were also analysed. Results indicated that the CFQ-FC presented a one-dimensional structure with 7 items, accounting for 66.14% of the variance. A CFA confirmed the plausibility of the measurement model, which was found to be invariant in both sexes. The CFQ-FC also revealed very good internal consistency, construct reliability, temporal stability, and convergent and divergent validity, being positively associated with similar constructs and with indicators of eating and general psychopathology. CFQ-FC also discriminated individuals with clinically significant symptoms of binge eating from participants with no symptoms. Finally, the CFQ-FC presents incremental validity over a global measure of cognitive fusion in predicting eating psychopathology, namely binge eating. The CFQ-FC is a psychometrically sound measure that allows for a brief and reliable assessment of eating-related cognitive fusion. This is a novel measure that may significantly contribute for the assessment of this specific dimension of cognitive fusion and for the understanding of its role in eating psychopathology. Copyright © 2016 Elsevier Ltd. All rights reserved.

Longitudinal Validation of General and Specific Structural Features of Personality Pathology

PubMed Central

Wright, Aidan G.C.; Hopwood, Christopher J.; Skodol, Andrew E.; Morey, Leslie C.

2016-01-01

Theorists have long argued that personality disorder (PD) is best understood in terms of general impairments shared across the disorders as well as more specific instantiations of pathology. A model based on this theoretical structure was proposed as part of the DSM-5 revision process. However, only recently has this structure been subjected to formal quantitative evaluation, with little in the way of validation efforts via external correlates or prospective longitudinal prediction. We used the Collaborative Longitudinal Study of Personality Disorders dataset to: (1) estimate structural models that parse general from specific variance in personality disorder features, (2) examine patterns of growth in general and specific features over the course of 10 years, and (3) establish concurrent and dynamic longitudinal associations in PD features and a host of external validators including basic personality traits and psychosocial functioning scales. We found that general PD exhibited much lower absolute stability and was most strongly related to broad markers of psychosocial functioning, concurrently and longitudinally, whereas specific features had much higher mean stability and exhibited more circumscribed associations with functioning. However, both general and specific factors showed recognizable associations with normative and pathological traits. These results can inform efforts to refine the conceptualization and diagnosis of personality pathology. PMID:27819472

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.

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

PubMed Central

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

2014-01-01

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

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

PubMed

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

2014-01-01

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

Development and validation of 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.

Stability-Indicating HPLC Determination of Gemcitabine in Pharmaceutical Formulations

PubMed Central

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

2015-01-01

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

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

PubMed Central

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

2014-01-01

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

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

PubMed

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

2011-04-01

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

The Italian version of the Inventory of Interpersonal Problems Personality Disorders Scales (IIP-47): psychometric properties and clinical usefulness as a screening measure.

PubMed

Ubbiali, Alessandro; Chiorri, Carlo; Donati, Deborah

2011-08-01

The Inventory of Interpersonal Problems-47 (IIP-47) is a brief and valid self-report measure for screening Personality Disorders (PDs). This study examined internal consistency, factor structure, criterion validity, temporal stability, and operating characteristics of the Italian version of the IIP-47 in two independent samples: PD subjects (n = 120) and nonclinical subjects (n = 475). Alpha coefficients ranged from .70 to .90. Multiple-Group Confirmatory Factor Analyses showed that the five-correlated-factor model reported in literature had the highest measurement invariance across the two groups. Criterion validity was supported by correlations among IIP-47 scale scores and scores on established measures of personality dimensions and pathology. Test-retest indices ranged from .71 to .95. PD subjects scored significantly higher than nonclinical subjects on all IIP-47 scales and cut-off scores for different levels of specificity and sensibility are reported. It is concluded that the psychometric properties of the original IIP-47 were preserved in its Italian version.

Length of stay after reaching clinical stability drives hospital costs associated with adult community-acquired pneumonia.

PubMed

Cortoos, Pieter-Jan; Gilissen, Christa; Laekeman, Gert; Peetermans, Willy E; Leenaers, Hilde; Vandorpe, Luc; Simoens, Steven

2013-03-01

Community-acquired pneumonia (CAP) has a considerable clinical and economic impact. The aim of this study was to identify drivers of hospital costs associated with CAP in 2 Belgian hospitals. Specifically, the influence of patient characteristics, quality indicators, and other treatment aspects on hospital costs was explored. The following were registered for patients admitted with a confirmed diagnosis of CAP in a large university hospital (Universitaire Ziekenhuizen Leuven, UZL) and a medium-sized secondary care hospital (Ziekenhuis Oost-Limburg, ZOL) in Belgium: the pneumonia severity index (PSI), time to clinical stability, length of stay, antibiotic therapy, outcomes, compliance with validated quality indicators, and the different costs (pharmacy, laboratory, and radiology, and total). Regression analysis was used to identify influential variables. Between October 2007 and June 2010, 803 patients were included, with a median total cost of €4794.57. The length of stay after clinical stability and time to clinical stability had the highest influence on the total cost (+6.3% and +4.9% per additional day, respectively; p < 0.0001). Other important drivers of higher costs were total therapy duration, PSI score, age, and admission to intensive care. Patients treated with moxifloxacin had significantly, but limited, lower costs. Quality indicator compliance, including guideline-compliant antibiotic treatment and therapy streamlining, had little influence. The most important driver of hospital costs associated with CAP was the time between clinical stability and actual hospital discharge. In order to substantially decrease the costs of CAP treatment, this period should be rigorously evaluated for possible intervention targets that would allow costs in CAP treatment to be decreased in a substantial manner.

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

PubMed

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

2014-08-01

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

Development and validation of a mass casualty conceptual model.

PubMed

Culley, Joan M; Effken, Judith A

2010-03-01

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

Letter to the Editor: On "Advantages and disadvantages of stiffness instructions when studying postural control" by C.T. Bonnet: You just can't win: Advantages and disadvantages of the postural stability requirement.

PubMed

Lajoie, Y; Richer, N; Jehu, D A; Polskaia, N; Saunders, D

2016-05-01

In the examination of postural control, instructions to stand as still as possible are common and promote a relatively unnatural sway pattern. The validity of the stability requirement is discussed in the present commentary in response to the discussion initiated by Cedrick T. Bonnet. The advantages of using the stability requirement include: evaluating unbiased postural control, reducing variability in postural sway, manipulating focus of attention, examining the ability to maintain an upright stance, and ecological validity of testing. The disadvantages include: constraining natural postural sway, increasing the complexity of the control condition, promoting an internal focus of attention, and reducing the ability to detect exploratory behaviour. After evaluating the aforementioned advantages and disadvantages, the present commentary suggests that researchers should strive to provide specific instructions to maintain feet, arm and eye position without specifically requiring participants to reduce their postural sway. Copyright © 2015 Elsevier B.V. All rights reserved.

Transcriptome Wide Annotation of Eukaryotic RNase III Reactivity and Degradation Signals

PubMed Central

Gagnon, Jules; Lavoie, Mathieu; Catala, Mathieu; Malenfant, Francis; Elela, Sherif Abou

2015-01-01

Detection and validation of the RNA degradation signals controlling transcriptome stability are essential steps for understanding how cells regulate gene expression. Here we present complete genomic and biochemical annotations of the signals required for RNA degradation by the dsRNA specific ribonuclease III (Rnt1p) and examine its impact on transcriptome expression. Rnt1p cleavage signals are randomly distributed in the yeast genome, and encompass a wide variety of sequences, indicating that transcriptome stability is not determined by the recurrence of a fixed cleavage motif. Instead, RNA reactivity is defined by the sequence and structural context in which the cleavage sites are located. Reactive signals are often associated with transiently expressed genes, and their impact on RNA expression is linked to growth conditions. Together, the data suggest that Rnt1p reactivity is triggered by malleable RNA degradation signals that permit dynamic response to changes in growth conditions. PMID:25680180

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

ERIC Educational Resources Information Center

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

2013-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2014-09-01

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

Development and Validation of 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

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

PubMed

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

2005-09-01

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

Fuzzy Logic Controller Stability Analysis Using a Satisfiability Modulo Theories Approach

NASA Technical Reports Server (NTRS)

Arnett, Timothy; Cook, Brandon; Clark, Matthew A.; Rattan, Kuldip

2017-01-01

While many widely accepted methods and techniques exist for validation and verification of traditional controllers, at this time no solutions have been accepted for Fuzzy Logic Controllers (FLCs). Due to the highly nonlinear nature of such systems, and the fact that developing a valid FLC does not require a mathematical model of the system, it is quite difficult to use conventional techniques to prove controller stability. Since safety-critical systems must be tested and verified to work as expected for all possible circumstances, the fact that FLC controllers cannot be tested to achieve such requirements poses limitations on the applications for such technology. Therefore, alternative methods for verification and validation of FLCs needs to be explored. In this study, a novel approach using formal verification methods to ensure the stability of a FLC is proposed. Main research challenges include specification of requirements for a complex system, conversion of a traditional FLC to a piecewise polynomial representation, and using a formal verification tool in a nonlinear solution space. Using the proposed architecture, the Fuzzy Logic Controller was found to always generate negative feedback, but inconclusive for Lyapunov stability.

Recent Advances in Heliogyro Solar Sail Structural Dynamics, Stability, and Control Research

NASA Technical Reports Server (NTRS)

Wilkie, W. Keats; Warren, Jerry E.; Horta, Lucas G.; Lyle, Karen H.; Juang, Jer-Nan; Gibbs, S. Chad; Dowell, Earl H.; Guerrant, Daniel V.; Lawrence, Dale

2015-01-01

Results from recent NASA sponsored research on the structural dynamics, stability, and control characteristics of heliogyro solar sails are summarized. Specific areas under investigation include coupled nonlinear finite element analysis of heliogyro membrane blade with solar radiation pressure effects, system identification of spinning membrane structures, and solarelastic stability analysis of heliogyro solar sails, including stability during blade deployment. Recent results from terrestrial 1-g blade dynamics and control experiments on "rope ladder" membrane blade analogs, and small-scale in vacuo system identification experiments with hanging and spinning high-aspect ratio membranes will also be presented. A low-cost, rideshare payload heliogyro technology demonstration mission concept is used as a mission context for these heliogyro structural dynamics and solarelasticity investigations, and is also described. Blade torsional dynamic response and control are also shown to be significantly improved through the use of edge stiffening structural features or inclusion of modest tip masses to increase centrifugal stiffening of the blade structure. An output-only system identification procedure suitable for on-orbit blade dynamics investigations is also developed and validated using ground tests of spinning sub-scale heliogyro blade models. Overall, analytical and experimental investigations to date indicate no intractable stability or control issues for the heliogyro solar sail concept.

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 to drug concentration, with an activation energy of 25.5 Kcal mol(-1) and a t(1/2)=10,830 h, in 0.1N HCl at 38 degrees C.

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.

Gene expression studies of reference genes for quantitative real-time PCR: an overview in insects.

PubMed

Shakeel, Muhammad; Rodriguez, Alicia; Tahir, Urfa Bin; Jin, Fengliang

2018-02-01

Whenever gene expression is being examined, it is essential that a normalization process is carried out to eliminate non-biological variations. The use of reference genes, such as glyceraldehyde-3-phosphate dehydrogenase, actin, and ribosomal protein genes, is the usual method of choice for normalizing gene expression. Although reference genes are used to normalize target gene expression, a major problem is that the stability of these genes differs among tissues, developmental stages, species, and responses to abiotic factors. Therefore, the use and validation of multiple reference genes are required. This review discusses the reasons that why RT-qPCR has become the preferred method for validating results of gene expression profiles, the use of specific and non-specific dyes and the importance of use of primers and probes for qPCR as well as to discuss several statistical algorithms developed to help the validation of potential reference genes. The conflicts arising in the use of classical reference genes in gene normalization and their replacement with novel references are also discussed by citing the high stability and low stability of classical and novel reference genes under various biotic and abiotic experimental conditions by employing various methods applied for the reference genes amplification.

Stable White Coatings

NASA Technical Reports Server (NTRS)

Zerlaut, Gene A.; Gilligan, J. E.; Harada, Y.

1965-01-01

In a previous research program for the Jet Propulsion- Laboratory, extensive studies led to the development and specifications of three zinc oxide-pigmented thermal-control coatings. The principal objectives of this program are: improvement of the three paints (as engineering materials), determination of the validity of our accelerated space-simulation testing, and continuation of the zinc oxide photolysis studies begun in the preceding program. Specific tasks that are discussed include: improvement of potassium silicate coatings as engineering materials and elucidation of their storage and handling problems; improvement of methyl silicone coatings as engineering materials; studies of zinc oxide photolysis to establish reasons for the observed stability of zinc oxide; and determination of space-simulation parameters such as long-term stability (to 8000 ESH), effect of coating surface temperature on the rate of degradation, and validity of accelerated testing (by reciprocity and wavelength dependency studies).

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

PubMed

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

2015-10-01

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

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

ERIC Educational Resources Information Center

Lowe, Patricia A.; Reynolds, Cecil R.

2006-01-01

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

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

Treesearch

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

2013-01-01

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

A systematic plan for the continued study of dimensional stability of metallic alloys considered for the fabrication of cryogenic wind tunnel models

NASA Technical Reports Server (NTRS)

Wigley, D. A.

1985-01-01

Interrelated research and development activities, phased development of stepped specimen program are documented and a sequence for a specific program of machining, validation and heat treatment cycles for one material are described. Proposed work for the next phase of dimensional stability research is presented and further technology development activities are proposed.

Evaluating the validity of self-reported smoking in Mexican adolescents

PubMed Central

Valladolid-López, María del Carmen; Barrientos-Gutiérrez, Tonatiuh; Reynales-Shigematsu, Luz Myriam; Thrasher, James F; Peláez-Ballestas, Ingris; Lazcano-Ponce, Eduardo; Hernández-Ávila, Mauricio

2015-01-01

Objectives We aimed to evaluate the validity of the self-reported smoking indicator used in the Global Youth Tobacco Survey (GYTS). Setting 43 middle and high-school classrooms from 26 schools were selected from Mexico City and Cuernavaca, Morelos. Participants A total of 1257 students provided both a questionnaire and a urine sample. Primary and secondary outcome Sensitivity and specificity of self-reported smoking compared to urinary cotinine. Validity indices were evaluated by subgroups of gender, social acceptability of smoking (ie, smoking parents or friends) and smoking frequency. Results Sensitivity and specificity for current smoking were 93.2% and 81.7%, respectively. Validity indices remained stable across gender. Parental smoking status moderated the validity of self-report, which had lower sensitivity in adolescents with non-smoking parents (86.7%) than in adolescents with smoking parents (96.6%). Sensitivity and specificity increased with smoking frequency. Conclusions This first validation study of self-reported current smoking used in the GYTS among Mexican adolescents suggests that self-reported smoking in the past 30 days is a valid and stable indicator of current smoking behaviour. This measure appears suitable for public health research and surveillance. PMID:26453588

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.

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.

Facultative Stabilization Pond: Measuring Biological Oxygen Demand using Mathematical Approaches

NASA Astrophysics Data System (ADS)

Wira S, Ihsan; Sunarsih, Sunarsih

2018-02-01

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

Development and psychometric evaluation of a cardiovascular risk and disease management knowledge assessment tool.

PubMed

Rosneck, James S; Hughes, Joel; Gunstad, John; Josephson, Richard; Noe, Donald A; Waechter, Donna

2014-01-01

This article describes the systematic construction and psychometric analysis of a knowledge assessment instrument for phase II cardiac rehabilitation (CR) patients measuring risk modification disease management knowledge and behavioral outcomes derived from national standards relevant to secondary prevention and management of cardiovascular disease. First, using adult curriculum based on disease-specific learning outcomes and competencies, a systematic test item development process was completed by clinical staff. Second, a panel of educational and clinical experts used an iterative process to identify test content domain and arrive at consensus in selecting items meeting criteria. Third, the resulting 31-question instrument, the Cardiac Knowledge Assessment Tool (CKAT), was piloted in CR patients to ensure use of application. Validity and reliability analyses were performed on 3638 adults before test administrations with additional focused analyses on 1999 individuals completing both pretreatment and posttreatment administrations within 6 months. Evidence of CKAT content validity was substantiated, with 85% agreement among content experts. Evidence of construct validity was demonstrated via factor analysis identifying key underlying factors. Estimates of internal consistency, for example, Cronbach's α = .852 and Spearman-Brown split-half reliability = 0.817 on pretesting, support test reliability. Item analysis, using point biserial correlation, measured relationships between performance on single items and total score (P < .01). Analyses using item difficulty and item discrimination indices further verified item stability and validity of the CKAT. A knowledge instrument specifically designed for an adult CR population was systematically developed and tested in a large representative patient population, satisfying psychometric parameters, including validity and reliability.

11th GCC Closed Forum: cumulative stability; matrix stability; immunogenicity assays; laboratory manuals; biosimilars; chiral methods; hybrid LBA/LCMS assays; fit-for-purpose validation; China Food and Drug Administration bioanalytical method validation.

PubMed

Islam, Rafiq; Briscoe, Chad; Bower, Joseph; Cape, Stephanie; Arnold, Mark; Hayes, Roger; Warren, Mark; Karnik, Shane; Stouffer, Bruce; Xiao, Yi Qun; van der Strate, Barry; Sikkema, Daniel; Fang, Xinping; Tudoroniu, Ariana; Tayyem, Rabab; Brant, Ashley; Spriggs, Franklin; Barry, Colin; Khan, Masood; Keyhani, Anahita; Zimmer, Jennifer; Caturla, Maria Cruz; Couerbe, Philippe; Khadang, Ardeshir; Bourdage, James; Datin, Jim; Zemo, Jennifer; Hughes, Nicola; Fatmi, Saadya; Sheldon, Curtis; Fountain, Scott; Satterwhite, Christina; Colletti, Kelly; Vija, Jenifer; Yu, Mathilde; Stamatopoulos, John; Lin, Jenny; Wilfahrt, Jim; Dinan, Andrew; Ohorodnik, Susan; Hulse, James; Patel, Vimal; Garofolo, Wei; Savoie, Natasha; Brown, Michael; Papac, Damon; Buonarati, Mike; Hristopoulos, George; Beaver, Chris; Boudreau, Nadine; Williard, Clark; Liu, Yansheng; Ray, Gene; Warrino, Dominic; Xu, Allan; Green, Rachel; Hayward-Sewell, Joanne; Marcelletti, John; Sanchez, Christina; Kennedy, Michael; Charles, Jessica St; Bouhajib, Mohammed; Nehls, Corey; Tabler, Edward; Tu, Jing; Joyce, Philip; Iordachescu, Adriana; DuBey, Ira; Lindsay, John; Yamashita, Jim; Wells, Edward

2018-04-01

The 11th Global CRO Council Closed Forum was held in Universal City, CA, USA on 3 April 2017. Representatives from international CRO members offering bioanalytical services were in attendance in order to discuss scientific and regulatory issues specific to bioanalysis. The second CRO-Pharma Scientific Interchange Meeting was held on 7 April 2017, which included Pharma representatives' sharing perspectives on the topics discussed earlier in the week with the CRO members. The issues discussed at the meetings included cumulative stability evaluations, matrix stability evaluations, the 2016 US FDA Immunogenicity Guidance and recent and unexpected FDA Form 483s on immunogenicity assays, the bioanalytical laboratory's role in writing PK sample collection instructions, biosimilars, CRO perspectives on the use of chiral versus achiral methods, hybrid LBA/LCMS assays, applications of fit-for-purpose validation and, at the Global CRO Council Closed Forum only, the status and trend of current regulated bioanalytical practice in China under CFDA's new BMV policy. Conclusions from discussions of these topics at both meetings are included in this report.

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

ERIC Educational Resources Information Center

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

2008-01-01

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

Validation of the World Health Organization Enzyme-Linked Immunosorbent Assay for the Quantitation of Immunoglobulin G Serotype-Specific Anti-Pneumococcal Antibodies in Human Serum

PubMed Central

2017-01-01

The World Health Organization (WHO) enzyme-linked immunosorbent assay (ELISA) guideline is currently accepted as the gold standard for the evaluation of immunoglobulin G (IgG) antibodies specific to pneumococcal capsular polysaccharide. We conducted validation of the WHO ELISA for 7 pneumococcal serotypes (4, 6B, 9V, 14, 18C, 19F, and 23F) by evaluating its specificity, precision (reproducibility and intermediate precision), accuracy, spiking recovery test, lower limit of quantification (LLOQ), and stability at the Ewha Center for Vaccine Evaluation and Study, Seoul, Korea. We found that the specificity, reproducibility, and intermediate precision were within acceptance ranges (reproducibility, coefficient of variability [CV] ≤ 15%; intermediate precision, CV ≤ 20%) for all serotypes. Comparisons between the provisional assignments of calibration sera and the results from this laboratory showed a high correlation > 94% for all 7 serotypes, supporting the accuracy of the ELISA. The spiking recovery test also fell within an acceptable range. The quantification limit, calculated using the LLOQ, for each of the serotypes was 0.05–0.093 μg/mL. The freeze-thaw stability and the short-term temperature stability were also within an acceptable range. In conclusion, we showed good performance using the standardized WHO ELISA for the evaluation of serotype-specific anti-pneumococcal IgG antibodies; the WHO ELISA can evaluate the immune response against pneumococcal vaccines with consistency and accuracy. PMID:28875600

Validation of the World Health Organization Enzyme-Linked Immunosorbent Assay for the Quantitation of Immunoglobulin G Serotype-Specific Anti-Pneumococcal Antibodies in Human Serum.

PubMed

Lee, Hyunju; Lim, Soo Young; Kim, Kyung Hyo

2017-10-01

The World Health Organization (WHO) enzyme-linked immunosorbent assay (ELISA) guideline is currently accepted as the gold standard for the evaluation of immunoglobulin G (IgG) antibodies specific to pneumococcal capsular polysaccharide. We conducted validation of the WHO ELISA for 7 pneumococcal serotypes (4, 6B, 9V, 14, 18C, 19F, and 23F) by evaluating its specificity, precision (reproducibility and intermediate precision), accuracy, spiking recovery test, lower limit of quantification (LLOQ), and stability at the Ewha Center for Vaccine Evaluation and Study, Seoul, Korea. We found that the specificity, reproducibility, and intermediate precision were within acceptance ranges (reproducibility, coefficient of variability [CV] ≤ 15%; intermediate precision, CV ≤ 20%) for all serotypes. Comparisons between the provisional assignments of calibration sera and the results from this laboratory showed a high correlation > 94% for all 7 serotypes, supporting the accuracy of the ELISA. The spiking recovery test also fell within an acceptable range. The quantification limit, calculated using the LLOQ, for each of the serotypes was 0.05-0.093 μg/mL. The freeze-thaw stability and the short-term temperature stability were also within an acceptable range. In conclusion, we showed good performance using the standardized WHO ELISA for the evaluation of serotype-specific anti-pneumococcal IgG antibodies; the WHO ELISA can evaluate the immune response against pneumococcal vaccines with consistency and accuracy. © 2017 The Korean Academy of Medical Sciences.

Driving-forces model on individual behavior in scenarios considering moving threat agents

NASA Astrophysics Data System (ADS)

Li, Shuying; Zhuang, Jun; Shen, Shifei; Wang, Jia

2017-09-01

The individual behavior model is a contributory factor to improve the accuracy of agent-based simulation in different scenarios. However, few studies have considered moving threat agents, which often occur in terrorist attacks caused by attackers with close-range weapons (e.g., sword, stick). At the same time, many existing behavior models lack validation from cases or experiments. This paper builds a new individual behavior model based on seven behavioral hypotheses. The driving-forces model is an extension of the classical social force model considering scenarios including moving threat agents. An experiment was conducted to validate the key components of the model. Then the model is compared with an advanced Elliptical Specification II social force model, by calculating the fitting errors between the simulated and experimental trajectories, and being applied to simulate a specific circumstance. Our results show that the driving-forces model reduced the fitting error by an average of 33.9% and the standard deviation by an average of 44.5%, which indicates the accuracy and stability of the model in the studied situation. The new driving-forces model could be used to simulate individual behavior when analyzing the risk of specific scenarios using agent-based simulation methods, such as risk analysis of close-range terrorist attacks in public places.

Development and validation of a new condition-specific instrument for evaluation of smile esthetics-related quality of life.

PubMed

Saltovic, Ema; Lajnert, Vlatka; Saltovic, Sabina; Kovacevic Pavicic, Daniela; Pavlic, Andrej; Spalj, Stjepan

2018-03-01

Orofacial esthetics raises psychosocial issues. The purpose was to create and validate new short instrument for psychosocial impacts of altered smile esthetics. A team of an orthodontist, two prosthodontists, psychologist, and a dental student generated items that could draw up specific hypothetical psychosocial dimensions (69 items initially, 39 in final analysis). The sample consisted of 261 Caucasian subjects attending local high schools and university (26% male) aged 14 to 28 years that have self-administrated the designed questionnaire. Factorial analysis, Cronbach's alpha, Pearson correlation, paired samples t-test and analysis of variance were used for analyses of internal consistency, construct validity, responsiveness, and test-retest. Three dimensions of psychosocial impacts of altered smile esthetics were identified: dental self-consciousness, dental self-confidence and social contacts that can be best fitted by 12 items, 4 items in each dimension. Internal consistency was good (α in range 0.85-0.89). Good stability in test-retest was confirmed. In responsiveness testing, tooth whitening induced increase in dental self-confidence (P = 0.002), but no significant changes in other dimensions. The new instrument, Smile Esthetics-Related Quality of Life (SERQoL), is short and has proven to be a good indicator of psychosocial dimensions related to perception of smile esthetics. Smile Esthetics-Related Quality of Life questionnaire might have practical validity when applied in esthetic dental clinical procedures. © 2017 Wiley Periodicals, Inc.

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

PubMed

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

2015-05-22

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

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.

Stability-indicating spectrophotometric methods for determination of the anticoagulant drug apixaban in the presence of its hydrolytic degradation product

NASA Astrophysics Data System (ADS)

Tantawy, Mahmoud A.; El-Ragehy, Nariman A.; Hassan, Nagiba Y.; Abdelkawy, Mohamed

2016-04-01

Apixaban (a novel anticoagulant agent) was subjected to a stress stability study including acid, alkali, oxidative, photolytic, and thermal degradation. The drug was found to be only liable to acidic and alkaline hydrolysis. The degradation product was then isolated and identified by IR and GC-mass spectrometry. Four spectrophotometric methods, namely; first derivative (D1), derivative ratio (DR), ratio difference (RD) and mean centering of ratio spectra (MCR), have been suggested for the determination of apixaban in presence of its hydrolytic degradation product. The proposed methods do not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined, and the methods were validated as per ICH guidelines and the specificity was assessed by analyzing synthetic mixtures containing different percentages of the degradation product with the drug. The developed methods were successfully applied for the determination of apixaban in bulk powder and its tablet dosage form.

Stability-indicating spectrophotometric methods for determination of the anticoagulant drug apixaban in the presence of its hydrolytic degradation product.

PubMed

Tantawy, Mahmoud A; El-Ragehy, Nariman A; Hassan, Nagiba Y; Abdelkawy, Mohamed

2016-04-15

Apixaban (a novel anticoagulant agent) was subjected to a stress stability study including acid, alkali, oxidative, photolytic, and thermal degradation. The drug was found to be only liable to acidic and alkaline hydrolysis. The degradation product was then isolated and identified by IR and GC-mass spectrometry. Four spectrophotometric methods, namely; first derivative (D(1)), derivative ratio (DR), ratio difference (RD) and mean centering of ratio spectra (MCR), have been suggested for the determination of apixaban in presence of its hydrolytic degradation product. The proposed methods do not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined, and the methods were validated as per ICH guidelines and the specificity was assessed by analyzing synthetic mixtures containing different percentages of the degradation product with the drug. The developed methods were successfully applied for the determination of apixaban in bulk powder and its tablet dosage form. Copyright © 2016 Elsevier B.V. All rights reserved.

Design and Validation of a Low-Cost Portable Device to Quantify Postural Stability.

PubMed

Zhu, Yong

2017-03-18

Measurement of the displacement of the center-of-pressure (COP) is an important tool used in biomechanics to assess postural stability and human balance. The goal of this research was to design and validate a low-cost portable device that can offer a quick indication of the state of postural stability and human balance related conditions. Approximate entropy (ApEn) values reflecting the amount of irregularity hiding in COP oscillations were used to calculate the index. The prototype adopted a portable design using the measurements of the load cells located at the four corners of a low-cost force platform. The test subject was asked to stand on the device in a quiet, normal, upright stance for 30 s with eyes open and subsequently for 30 s with eyes closed. Based on the COP displacement signals, the ApEn values were calculated. The results indicated that the prototype device was capable of capturing the increase in regularity of postural control in the visual-deprivation conditions. It was also able to decipher the subtle postural control differences along anterior-posterior and medial-lateral directions. The data analysis demonstrated that the prototype would enable the quantification of postural stability and thus provide a low-cost portable device to assess many conditions related to postural stability and human balance such as aging and pathologies.

A measure of satisfaction with food-related life.

PubMed

Grunert, Klaus G; Dean, Moira; Raats, Monique M; Nielsen, Niels Asger; Lumbers, Margaret

2007-09-01

A measure of satisfaction with food-related life is developed and tested in three studies in eight European countries. Five items are retained from an original pool of seven; these items exhibit good reliability as measured by Cronbach's alpha, good temporal stability, convergent validity with two related measures, and construct validity as indicated by relationships with other indicators of quality of life, including the Satisfaction With Life and the SF-8 scales. It is concluded that this scale will be useful in studies trying to identify factors contributing to satisfaction with food-related life.

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.

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.

Psychometric Properties of a Self-Report Instrument for the Assessment of Tic Severity in Adults With Tic Disorders.

PubMed

Abramovitch, Amitai; Reese, Hannah; Woods, Douglas W; Peterson, Alan; Deckersbach, Thilo; Piacentini, John; Scahill, Lawrence; Wilhelm, Sabine

2015-11-01

The gold-standard measure of tic severity in tic disorders (TD), the Yale Global Tic Severity Scale (YGTSS), is a semistructured clinician-administered interview that can be time consuming and requires highly trained interviewers. Moreover, the YGTSS does not provide information regarding frequency and intensity of specific tics because all motor and all vocal tics are rated as a group. The aim of the present study is to describe and test the Adult Tic Questionnaire (ATQ), a measure for the assessment of tic severity in adults, and to report its preliminary psychometric properties. The ATQ is a brief self-report questionnaire that provides information regarding frequency, intensity, and severity of 27 specific tics. In addition, the ATQ produces total frequency, intensity, and severity scores for vocal and motor tics, as well as a global total tic severity score. Results showed that the ATQ demonstrated very good internal consistency and temporal stability. The total, vocal, and motor tic severity scales of the ATQ showed strong correlation with corresponding subscales of the YGTSS, indicating strong convergent validity. Weak correlations with measures of severity of obsessive-compulsive disorder and attention deficit/hyperactivity disorder, indicated strong discriminant validity. The ATQ, a promising measure for the assessment of tic severity in adults with TD, may be a valuable supplement to the current recommended assessment battery for TD. Furthermore, the ATQ enables clinicians and researchers to track changes in the frequency and intensity of specific tics, which is important given their complex and dynamic nature. Copyright © 2015. Published by Elsevier Ltd.

Psychometric Properties of a Self-Report Instrument for the Assessment of Tic Severity in Adults with Tic Disorders

PubMed Central

Abramovitch, Amitai; Reese, Hannah; Woods, Douglas W.; Peterson, Alan; Deckersbach, Thilo; Piacentini, John; Scahill, Lawrence; Wilhelm, Sabine

2017-01-01

The gold-standard measure of tic severity in Tic Disorders (TD), the Yale Global Tic Severity Scale (YGTSS), is a semi-structured clinician-administered interview that can be time consuming and requires highly trained interviewers. Moreover, the YGTSS does not provide information regarding frequency and intensity of specific tics as all motor, and all vocal tics are rated as a group. The aim of the present study is to describe and test the Adult Tic Questionnaire (ATQ), a measure for the assessment of tic severity in adults, and to report its preliminary psychometric properties. The ATQ is a brief self-report questionnaire that provides information regarding frequency, intensity, and severity of 27 specific tics. In addition, the ATQ produces total frequency, intensity, and severity scores for vocal, and motor tics, as well as a global total tic severity score. Results showed that the ATQ demonstrated very good internal consistency and temporal stability. The total, vocal, and motor tic severity scales of the ATQ showed strong correlation with corresponding subscales of the YGTSS, indicating strong convergent validity. Weak correlations with measures of severity of obsessive-compulsive disorder and attention deficit/hyperactivity disorder, indicated strong discriminant validity. The ATQ is a promising measure for the assessment of tic severity in adults with TD which may be a valuable supplement to the current recommended assessment battery for TD. Furthermore, the ATQ enables clinicians and researchers to track changes in the frequency and intensity of specific tics, which is important given their complex and dynamic nature. PMID:26520221

Efficacy validation of synthesized retinol derivatives In vitro: stability, toxicity, and activity.

PubMed

Han, Hye-Sook; Kwon, Youn-Ja; Park, Myoung-Soon; Park, Si-Ho; Cho, So-Mi Kim; Rho, Young-Soy; Kim, Jin-Wou; Sin, Hong-Sig; Um, Soo-Jong

2003-08-15

Retinol (vitamin A) is used as an antiwrinkle agent in the cosmetics industry. However, its photo-instability makes it unsuitable for use in general cosmetic formulations. To improve the photo-stability of retinol, three derivatives (3, 4, and 5) were synthesized and their biological activities were analyzed. 1H NMR and HPLC analysis indicated that derivatives 3 and 5 were much more stable than retinol under our sunlight exposure conditions. When human adult fibroblasts were treated, the IC(50) of derivative 3 was 96 microM, which is similar to that of retinol, as determined by the MTT assay. Derivatives 4 and 5 were 2.5 and 8 times more toxic than retinol, respectively. At 1 microM treatment, like retinol, derivatives 3 and 4 were specifically active for RARalpha out of six retinoid receptors (RAR/RXRalpha, beta, gamma). Dose-dependent analysis confirmed that derivative 4 was as active as retinol and the other two derivatives were less active for RARalpha. The effect of our derivatives on the expression of collagenase, an indicator of wrinkle formation, was measured using the transient co-expression of c-Jun and RT-PCR in HaCaT cells. Collagenase promoter activity, which is increased by c-Jun expression, was reduced 42% by retinol treatment. The other derivatives inhibited collagenase promoter activity similarly. These results were further confirmed by RT-PCR analysis of the collagenase gene. Taken together, our results suggest that retinol derivative 3 is a promising antiwrinkle agent based on its higher photo-stability, lower RARalpha activity (possibly indicating reduced side effects), and similar effect on collagenase expression.

A New Rapid and Sensitive Stability-Indicating UPLC Assay Method for Tolterodine Tartrate: Application in Pharmaceuticals, Human Plasma and Urine Samples.

PubMed

Yanamandra, Ramesh; Vadla, Chandra Sekhar; Puppala, Umamaheshwar; Patro, Balaram; Murthy, Yellajyosula L N; Ramaiah, Parimi Atchuta

2012-01-01

A new rapid, simple, sensitive, selective and accurate reversed-phase stability-indicating Ultra Performance Liquid Chromatography (RP-UPLC) technique was developed for the assay of Tolterodine Tartrate in pharmaceutical dosage form, human plasma and urine samples. The developed UPLC method is superior in technology to conventional HPLC with respect to speed, solvent consumption, resolution and cost of analysis. Chromatographic run time was 6 min in reversed-phase mode and ultraviolet detection was carried out at 220 nm for quantification. Efficient separation was achieved for all the degradants of Tolterodine Tartrate on BEH C18 sub-2-μm Acquity UPLC column using Trifluoroacetic acid and acetonitrile as organic solvent in a linear gradient program. The active pharmaceutical ingredient was extracted from tablet dosage form using a mixture of acetonitrile and water as diluent. The calibration graphs were linear and the method showed excellent recoveries for bulk and tablet dosage form. The test solution was found to be stable for 40 days when stored in the refrigerator between 2 and 8 °C. The developed UPLC method was validated and meets the requirements delineated by the International Conference on Harmonization (ICH) guidelines with respect to linearity, accuracy, precision, specificity and robustness. The intra-day and inter-day variation was found be less than 1%. The method was reproducible and selective for the estimation of Tolterodine Tartrate. Because the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating one.

A New Rapid and Sensitive Stability-Indicating UPLC Assay Method for Tolterodine Tartrate: Application in Pharmaceuticals, Human Plasma and Urine Samples

PubMed Central

Yanamandra, Ramesh; Vadla, Chandra Sekhar; Puppala, Umamaheshwar; Patro, Balaram; Murthy, Yellajyosula. L. N.; Ramaiah, Parimi Atchuta

2012-01-01

A new rapid, simple, sensitive, selective and accurate reversed-phase stability-indicating Ultra Performance Liquid Chromatography (RP-UPLC) technique was developed for the assay of Tolterodine Tartrate in pharmaceutical dosage form, human plasma and urine samples. The developed UPLC method is superior in technology to conventional HPLC with respect to speed, solvent consumption, resolution and cost of analysis. Chromatographic run time was 6 min in reversed-phase mode and ultraviolet detection was carried out at 220 nm for quantification. Efficient separation was achieved for all the degradants of Tolterodine Tartrate on BEH C18 sub-2-μm Acquity UPLC column using Trifluoroacetic acid and acetonitrile as organic solvent in a linear gradient program. The active pharmaceutical ingredient was extracted from tablet dosage form using a mixture of acetonitrile and water as diluent. The calibration graphs were linear and the method showed excellent recoveries for bulk and tablet dosage form. The test solution was found to be stable for 40 days when stored in the refrigerator between 2 and 8 °C. The developed UPLC method was validated and meets the requirements delineated by the International Conference on Harmonization (ICH) guidelines with respect to linearity, accuracy, precision, specificity and robustness. The intra-day and inter-day variation was found be less than 1%. The method was reproducible and selective for the estimation of Tolterodine Tartrate. Because the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating one. PMID:22396907

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.

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.

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

PubMed

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

2014-08-01

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

Development and Validation of RP-LC Method for the Determination of Cinnarizine/Piracetam and Cinnarizine/Heptaminol Acefyllinate in Presence of Cinnarizine Reported Degradation Products

PubMed Central

EL-Houssini, Ola M.; Zawilla, Nagwan H.; Mohammad, Mohammad A.

2013-01-01

Specific stability indicating reverse-phase liquid chromatography (RP-LC) assay method (SIAM) was developed for the determination of cinnarizine (Cinn)/piracetam (Pira) and cinnarizine (Cinn)/heptaminol acefyllinate (Hept) in the presence of the reported degradation products of Cinn. A C18 column and gradient mobile phase was applied for good resolution of all peaks. The detection was achieved at 210 nm and 254 nm for Cinn/Pira and Cinn/Hept, respectively. The responses were linear over concentration ranges of 20–200, 20–1000 and 25–1000 μgmL−1 for Cinn, Pira, and Hept respectively. The proposed method was validated for linearity, accuracy, repeatability, intermediate precision, and robustness via statistical analysis of the data. The method was shown to be precise, accurate, reproducible, sensitive, and selective for the analysis of Cinn/Pira and Cinn/Hept in laboratory prepared mixtures and in pharmaceutical formulations. PMID:24137049

Computational evaluation of load carriage effects on gait balance stability.

PubMed

Mummolo, Carlotta; Park, Sukyung; Mangialardi, Luigi; Kim, Joo H

2016-01-01

Evaluating the effects of load carriage on gait balance stability is important in various applications. However, their quantification has not been rigorously addressed in the current literature, partially due to the lack of relevant computational indices. The novel Dynamic Gait Measure (DGM) characterizes gait balance stability by quantifying the relative effects of inertia in terms of zero-moment point, ground projection of center of mass, and time-varying foot support region. In this study, the DGM is formulated in terms of the gait parameters that explicitly reflect the gait strategy of a given walking pattern and is used for computational evaluation of the distinct balance stability of loaded walking. The observed gait adaptations caused by load carriage (decreased single support duration, inertia effects, and step length) result in decreased DGM values (p < 0.0001), which indicate that loaded walking motions are more statically stable compared with the unloaded normal walking. Comparison of the DGM with other common gait stability indices (the maximum Floquet multiplier and the margin of stability) validates the unique characterization capability of the DGM, which is consistently informative of the presence of the added load.

Clinical utility of the mBIAS and NSI validity-10 to detect symptom over-reporting following mild TBI: A multicenter investigation with military service members.

PubMed

Armistead-Jehle, Patrick; Cooper, Douglas B; Grills, Chad E; Cole, Wesley R; Lippa, Sara M; Stegman, Robert L; Lange, Rael T

2018-04-01

Self-report measures are commonly relied upon in military healthcare environments to assess service members following a mild traumatic brain injury (mTBI). However, such instruments are susceptible to over-reporting and rarely include validity scales. This study evaluated the utility of the mild Brain Injury Atypical Symptoms scale (mBIAS) and the Neurobehavioral Symptom Inventory Validity-10 scale to detect symptom over-reporting. A total of 359 service members with a reported history of mTBI were separated into two symptom reporting groups based on MMPI-2-RF validity scales (i.e., non-over-reporting versus symptom over-reporting). The clinical utility of the mBIAS and Validity-10 as diagnostic indicators and screens of symptom over-reporting were evaluated by calculating sensitivity, specificity, positive test rate, positive predictive power (PPP), and negative predictive power (NPP) values. An mBIAS cut score of ≥10 was optimal as a diagnostic indicator, which resulted in high specificity and PPP; however, sensitivity was low. The utility of the mBIAS as a screening instrument was limited. A Validity-10 cut score of ≥33 was optimal as a diagnostic indicator. This resulted in very high specificity and PPP, but low sensitivity. A Validity-10 cut score of ≥7 was considered optimal as a screener, which resulted in moderate sensitivity, specificity, NPP, but relatively low PPP. Owing to low sensitivity, the current data suggests that both the mBIAS and Validity-10 are insufficient as stand-alone measures of symptom over-reporting. However, Validity-10 scores above the identified cut-off of ≥7should be taken as an indication that further evaluation to rule out symptom over-reporting is necessary.

Atmospheric stability and complex terrain: comparing measurements and CFD

NASA Astrophysics Data System (ADS)

Koblitz, T.; Bechmann, A.; Berg, J.; Sogachev, A.; Sørensen, N.; Réthoré, P.-E.

2014-12-01

For wind resource assessment, the wind industry is increasingly relying on Computational Fluid Dynamics models that focus on modeling the airflow in a neutrally stratified surface layer. So far, physical processes that are specific to the atmospheric boundary layer, for example the Coriolis force, buoyancy forces and heat transport, are mostly ignored in state-of-the-art flow solvers. In order to decrease the uncertainty of wind resource assessment, the effect of thermal stratification on the atmospheric boundary layer should be included in such models. The present work focuses on non-neutral atmospheric flow over complex terrain including physical processes like stability and Coriolis force. We examine the influence of these effects on the whole atmospheric boundary layer using the DTU Wind Energy flow solver EllipSys3D. To validate the flow solver, measurements from Benakanahalli hill, a field experiment that took place in India in early 2010, are used. The experiment was specifically designed to address the combined effects of stability and Coriolis force over complex terrain, and provides a dataset to validate flow solvers. Including those effects into EllipSys3D significantly improves the predicted flow field when compared against the measurements.

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

Validity of a New Patient Engagement Measure: The Altarum Consumer Engagement (ACE) Measure.

PubMed

Duke, Christopher C; Lynch, Wendy D; Smith, Brad; Winstanley, Julie

2015-12-01

The objective of this study was to report on the validation of new scales [called the Altarum Consumer Engagement (ACE) Measure] that are indicative of an individual's engagement in health and healthcare decisions. The instrument was created to broaden the scope of how engagement is measured and understood, and to update the concept of engagement to include modern information sources, such as online health resources and ratings of providers and patient health. Data were collected through an online survey with a US population of 2079 participants. A combination of Principal Component Analysis (PCA) and detailed Rasch analyses were conducted to identify specific subscales of engagement. Results were compared to another commonly used survey instrument, and outcomes were compared for construct validity. The PCA identified a four-factor structure composed of 21 items. The factors were named Commitment, Informed Choice, Navigation, and Ownership. Rasch analyses confirmed scale stability. Relevant outcomes were correlated in the expected direction, such as health status, lifestyle behaviors, medication adherence, and observed expected group differences. This study confirmed the validity of the new ACE Measure and its utility in screening for and finding group differences in activities related to patient engagement and health consumerism, such as using provider comparison tools and asking about medical costs.

Validation of the French version of the Burn Specific Health Scale-Brief (BSHS-B) questionnaire.

PubMed

Gandolfi, S; Auquit-Auckbur, I; Panunzi, S; Mici, E; Grolleau, J-L; Chaput, B

2016-11-01

The Burn Specific Health Scale-Brief questionnaire is a widely validated tool for estimating the health related quality of life and for assessing the best multidisciplinary management of burn patients. The aim of this study was to translate the BSHS-B into French and to investigate its reliability and validity. According to the procedure proposed by the Scientific Advisory Committee of the Medical Outcomes Trust, the Burn Specific Health Scale-Brief (BSHS-B) was translated from the English version into French. In order to test the reliability of the French version of the BSHS-B, 53 burn patients French speakers completed the BSHS-B and SF-36 questionnaires from two to four years after burn. Ten of them have been re-tested at 6 months after the first evaluation. To evaluate clinical utility of the BSHS-F, internal consistency, construct validity (using SF-36) and stability in time were assessed using Cronbach's alpha statistic, Spearman rank test, and intra-class correlation coefficient respectively. The French version of the BSHS-B Cronbach's alpha coefficient was 0.93 and was >0.80 for all the sub-domains. French version of the BSHS-B and the SF-36 were positively correlated, all the associations were statistically significant (p<0.01). Intra-class correlation coefficients for test-retest ranged between 0.95 and 0.99 for the sub-domains. The intra-class correlation coefficient (ICC) for the total score was 0.98. The French version of the BSHS-B shows a robust rate of internal consistency, construct validity and stability in time, supporting its application in routine clinical practice as well as in international studies. Copyright © 2016 Elsevier Ltd and ISBI. All rights reserved.

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.

Examining the validity of self-reports on scales measuring students' strategic processing.

PubMed

Samuelstuen, Marit S; Bråten, Ivar

2007-06-01

Self-report inventories trying to measure strategic processing at a global level have been much used in both basic and applied research. However, the validity of global strategy scores is open to question because such inventories assess strategy perceptions outside the context of specific task performance. The primary aim was to examine the criterion-related and construct validity of the global strategy data obtained with the Cross-Curricular Competencies (CCC) scale. Additionally, we wanted to compare the validity of these data with the validity of data obtained with a task-specific self-report inventory focusing on the same types of strategies. The sample included 269 10th-grade students from 12 different junior high schools. Global strategy use as assessed with the CCC was compared with task-specific strategy use reported in three different reading situations. Moreover, relationships between scores on the CCC and scores on measures of text comprehension were examined and compared with relationships between scores on the task-specific strategy measure and the same comprehension measures. The comparison between the CCC strategy scores and the task-specific strategy scores suggested only modest criterion-related validity for the data obtained with the global strategy inventory. The CCC strategy scores were also not related to the text comprehension measures, indicating poor construct validity. In contrast, the task-specific strategy scores were positively related to the comprehension measures, indicating good construct validity. Attempts to measure strategic processing at a global level seem to have limited validity and utility.

Selection and validation of reference genes for gene expression analysis in apomictic and sexual Cenchrus ciliaris

PubMed Central

2013-01-01

Background Apomixis is a naturally occurring asexual mode of seed reproduction resulting in offspring genetically identical to the maternal plant. Identifying differential gene expression patterns between apomictic and sexual plants is valuable to help deconstruct the trait. Quantitative RT-PCR (qRT-PCR) is a popular method for analyzing gene expression. Normalizing gene expression data using proper reference genes which show stable expression under investigated conditions is critical in qRT-PCR analysis. We used qRT-PCR to validate expression and stability of six potential reference genes (EF1alpha, EIF4A, UBCE, GAPDH, ACT2 and TUBA) in vegetative and reproductive tissues of B-2S and B-12-9 accessions of C. ciliaris. Findings Among tissue types evaluated, EF1alpha showed the highest level of expression while TUBA showed the lowest. When all tissue types were evaluated and compared between genotypes, EIF4A was the most stable reference gene. Gene expression stability for specific ovary stages of B-2S and B-12-9 was also determined. Except for TUBA, all other tested reference genes could be used for any stage-specific ovary tissue normalization, irrespective of the mode of reproduction. Conclusion Our gene expression stability assay using six reference genes, in sexual and apomictic accessions of C. ciliaris, suggests that EIF4A is the most stable gene across all tissue types analyzed. All other tested reference genes, with the exception of TUBA, could be used for gene expression comparison studies between sexual and apomictic ovaries over multiple developmental stages. This reference gene validation data in C. ciliaris will serve as an important base for future apomixis-related transcriptome data validation. PMID:24083672

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

PubMed

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

2018-01-01

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

Identification and characterization of stress degradants of lacosamide by LC-MS and ESI-Q-TOF-MS/MS: development and validation of a stability indicating RP-HPLC method.

PubMed

Ramisetti, Nageswara Rao; Kuntamukkala, Ramakrishna; Lakshetti, Sridhar; Sripadi, Prabhakar

2014-07-01

The current study dealt with the degradation behavior of lacosamide (LAC) under ICH prescribed stress conditions. LAC was found to be labile under acid and base hydrolytic stress conditions, while it was stable to neutral hydrolytic, oxidative, photolytic and thermal stress. In total, seven degradation products (DPs) were formed, which were separated on a C18 column using a stability-indicating method. LC-MS analyses indicated that one of the DPs had the same molecular mass as that of the drug. Structural characterization of DPs was carried out using ESI-Q-TOF-MS/MS technique. The degradation pathways and mechanisms of degradation of the drug were delineated by carrying out the degradation in different co-solvents viz. methanol, deuterated methanol, ethanol, 1-propanol and acetonitrile. The developed LC method was validated for the determination of related substances and assay of LAC as per ICH guidelines. This study demonstrates a comprehensive approach of LAC degradation studies during its development phase. Copyright © 2014. Published by Elsevier B.V.

Stability of physical assessment of older drivers over 1 year.

PubMed

Smith, Andrew; Marshall, Shawn; Porter, Michelle; Ha, Linda; Bédard, Michel; Gélinas, Isabelle; Man-Son-Hing, Malcolm; Mazer, Barbara; Rapoport, Mark; Tuokko, Holly; Vrkljan, Brenda

2013-12-01

Older adults represent the fastest-growing population of drivers with a valid driver's licence. Also common in this age group are multiple chronic medical conditions that may have an effect on physical function and driving ability. Determining the reliability of physical measures used to assess older drivers' functional ability is important to identifying those who are safe to continue driving. Most previous reliability studies of clinical physical measures of health used test-retest intervals shorter than those between patient visits with a clinician. In the present study we examined a more clinically representative interval of 1 year to determine the stability of commonly used physical measures collected during the Candrive II prospective cohort study of older drivers. Reliability statistics indicate that the sequential finger-thumb opposition, rapid pace walk and the Pelli-Robson contrast sensitivity tests have adequate stability over 1 year. Poor stability was observed for the one-legged stance and Snellen visual acuity test. Several assessments with nominal data (Marottoli method [functional neck range of motion], whispered voice test, range of motion and strength testing) lacked sufficient variability to conduct reliability analyses; however, a lack of variability between test days suggests consistency over a 1-year time frame. Our results provide evidence that specific physical measures are stable in monitoring functional ability over the course of a year. Copyright © 2013 Elsevier Ltd. All rights reserved.

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.

Recommendations for the evaluation of specimen stability for flow cytometric testing during drug development.

PubMed

Brown, Lynette; Green, Cherie L; Jones, Nicholas; Stewart, Jennifer J; Fraser, Stephanie; Howell, Kathy; Xu, Yuanxin; Hill, Carla G; Wiwi, Christopher A; White, Wendy I; O'Brien, Peter J; Litwin, Virginia

2015-03-01

The objective of this manuscript is to present an approach for evaluating specimen stability for flow cytometric methods used during drug development. While this approach specifically addresses stability assessment for assays to be used in clinical trials with centralized testing facilities, the concepts can be applied to any stability assessment for flow cytometric methods. The proposed approach is implemented during assay development and optimization, and includes suggestions for designing a stability assessment plan, data evaluation and acceptance criteria. Given that no single solution will be applicable in all scenarios, this manuscript offers the reader a roadmap for stability assessment and is intended to guide the investigator during both the method development phase and in the experimental design of the validation plan. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of RP UPLC-TOF/MS, stability indicating method for omeprazole and its related substances by applying two level factorial design; and identification and synthesis of non-pharmacopoeial impurities.

PubMed

Jadhav, Sushant Bhimrao; Kumar, C Kiran; Bandichhor, Rakeshwar; Bhosale, P N

2016-01-25

A new UPLC-TOF/MS compatible, reverse phase-stability indicating method was developed for determination of Omeprazole (OMP) and its related substances in pharmaceutical dosage forms by implementing Design of Experiment (DoE) i.e. two level full factorial Design (2(3)+3 center points=11 experiments) to understand the Critical Method Parameters (CMP) and its relation with Critical Method Attribute (CMA); to ensure robustness of the method. The separation of eleven specified impurities including conversion product of OMP related compound F (13) and G (14) i.e. Impurity-I (1), OMP related compound-I (11) and OMP 4-chloro analog (12) was achieved in a single method on Acquity BEH shield RP18 100 × 2.1 mm, 1.7 μm column, with inlet filter (0.2 μm) using gradient elution and detector wavelength at 305 nm and validated in accordance with ICH guidelines and found to be accurate, precise, reproducible, robust and specific. The drug was found to degrade extensively in heat, humidity and acidic conditions and forms unknown degradation products during stability studies. The same method was used for LC-MS analysis to identify m/z and fragmentation of maximum unknown impurities (Non-Pharmacopoeial) i.e. Impurity-I (1), Impurity-III (3), Impurity-V (5) and Impurity-VIII (9) formed during stability studies. Based on the results, degradation pathway for the drug has been proposed and synthesis of identified impurities i.e. impurities (Impurity-I (1), Impurity-III (3), Impurity-V (5) and Impurity-VIII (9)) are discussed in detail to ensure in-depth understanding of OMP and its related impurities and optimum performance during lifetime of the product. Copyright © 2015. Published by Elsevier B.V.

Validation of quality indicators for the organization of palliative care: a modified RAND Delphi study in seven European countries (the Europall project).

PubMed

Woitha, Kathrin; Van Beek, Karen; Ahmed, Nisar; Jaspers, Birgit; Mollard, Jean M; Ahmedzai, Sam H; Hasselaar, Jeroen; Menten, Johan; Vissers, Kris; Engels, Yvonne

2014-02-01

Validated quality indicators can help health-care professionals to evaluate their medical practices in a comparative manner to deliver optimal clinical care. No international set of quality indicators to measure the organizational aspects of palliative care settings exists. To develop and validate a set of structure and process indicators for palliative care settings in Europe. A two-round modified RAND Delphi process was conducted to rate clarity and usefulness of a previously developed set of 110 quality indicators. In total, 20 multi-professional palliative care teams of centers of excellence from seven European countries. In total, 56 quality indicators were rated as useful. These valid quality indicators concerned the following domains: the definition of a palliative care service (2 quality indicators), accessibility to palliative care (16 quality indicators), specific infrastructure to deliver palliative care (8 quality indicators), symptom assessment tools (1 quality indicator), specific personnel in palliative care services (9 quality indicators), documentation methodology of clinical data (14 quality indicators), evaluation of quality and safety procedures (1 quality indicator), reporting of clinical activities (1 quality indicator), and education in palliative care (4 quality indicator). The modified RAND Delphi process resulted in 56 international face-validated quality indicators to measure and compare organizational aspects of palliative care. These quality indicators, aimed to assess and improve the organization of palliative care, will be pilot tested in palliative care settings all over Europe and be used in the EU FP7 funded IMPACT project.

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

PubMed

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

2013-01-01

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

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

PubMed

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

2010-02-05

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

Development and psychometric testing of a new geriatric spiritual well-being scale.

PubMed

Dunn, Karen S

2008-09-01

Aims and objectives.  Assess the psychometric properties of a new geriatric spiritual well-being scale (GSWS), specifically designed for older adults. Background.  Religiosity and spiritual wellness must be measured as two distinct concepts to prevent confounding them as synonymous among atheist and agnostic population. Design.  A test-retest survey design was used to estimate the psychometric properties. Methods.  A convenience sample of 138 community-dwelling older adults was drawn from the inner city of Detroit. Data were collected using telephone survey interviews. Data analyses included descriptive statistics, structural equation modelling, reliability analyses, and point-biserial correlations. Results.  The factorial validity of the proposed model was not supported by the data. Fit indices were χ(2)  = 185.98, d.f. = 98, P < 0.00, goodness-of-fit index of 0.85, comparative fit index of 0.87 and root mean error of approximation of 0.08, indicating a mediocre fit. Reliability statistics for the subscales ranged from being poor (0.36) to good (0.84) with an acceptable overall scale alpha of 0.76. Participants' performance stability and criterion-related validity were also supported. Conclusions.  The GSWS is an age-specific assessment tool that was developed specifically to address a population's cultural diversity. Future research endeavors will be to test the psychometric properties of this scale in culturally diverse older adult populations for further instrument development. Relevance to clinical practice.  Nurses need to recognize that agnostics/atheists have spiritual needs that do not include religious beliefs or practices. Thus, assessing patients' religious beliefs and practices prior to assessing spiritual well-being is essential to prevent bias. © 2008 The Author. Journal compilation © 2008 Blackwell Publishing Ltd.

Stability-indicating HPLC Method for Simultaneous Determination of Terbutaline Sulphate, Bromhexine Hydrochloride and Guaifenesin

PubMed Central

Porel, A.; Haty, Sanjukta; Kundu, A.

2011-01-01

The aim of the present study was the development and subsequent validation of a simple, precise and stability-indicating reversed phase HPLC method for the simultaneous determination of guaifenesin, terbutaline sulphate and bromhexine hydrochloride in the presence of their potential impurities in a single run. The photolytic as well as hydrolytic impurities were detected as 3,5-dihydroxybenzoic acid, 3,5-dihydroxybenzaldehyde, 1-(3,5-dihydroxyphenyl)-2-[(1,1-dimethylethyl) amino]-ethanone from terbutaline, 2-methoxyphenol and an unknown impurity identified as (2RS)-3-(2-hydroxyphenoxy)-propane-1,2-diol from guaifenesin. The chromatographic separation of all the three active components and their impurities was achieved on Wakosil II column, using phosphate buffer (pH 3.0) and acetonitrile as mobile phase which was delivered initially in the ratio of 80:20 (v/v) for 18 min, then changed to 60:40 (v/v) for next 12 min, and finally equilibrated back to 80:20 (v/v) for 10 min. Other HPLC parameters were: Flow rate at 1.0 ml/min, detection wavelengths 248 and 280 nm, injection volume 10 μl. The calibration graphs plotted with five concentrations of each component were linear with a regression coefficient R2 >0.9999. The limit of detection and limit of quantitation were estimated for all the five impurities. The established method was then validated for linearity, precision, accuracy, and specificity and demonstrated to be applicable to the determination of the active ingredients in commercial and model cough syrup. No interference from the formulation excipients was observed. These results suggest that this LC method can be used for the determination of multiple active ingredients and their impurities in a cough and cold syrup. PMID:22131621

Stability-indicating HPLC Method for Simultaneous Determination of Terbutaline Sulphate, Bromhexine Hydrochloride and Guaifenesin.

PubMed

Porel, A; Haty, Sanjukta; Kundu, A

2011-01-01

The aim of the present study was the development and subsequent validation of a simple, precise and stability-indicating reversed phase HPLC method for the simultaneous determination of guaifenesin, terbutaline sulphate and bromhexine hydrochloride in the presence of their potential impurities in a single run. The photolytic as well as hydrolytic impurities were detected as 3,5-dihydroxybenzoic acid, 3,5-dihydroxybenzaldehyde, 1-(3,5-dihydroxyphenyl)-2-[(1,1-dimethylethyl) amino]-ethanone from terbutaline, 2-methoxyphenol and an unknown impurity identified as (2RS)-3-(2-hydroxyphenoxy)-propane-1,2-diol from guaifenesin. The chromatographic separation of all the three active components and their impurities was achieved on Wakosil II column, using phosphate buffer (pH 3.0) and acetonitrile as mobile phase which was delivered initially in the ratio of 80:20 (v/v) for 18 min, then changed to 60:40 (v/v) for next 12 min, and finally equilibrated back to 80:20 (v/v) for 10 min. Other HPLC parameters were: Flow rate at 1.0 ml/min, detection wavelengths 248 and 280 nm, injection volume 10 μl. The calibration graphs plotted with five concentrations of each component were linear with a regression coefficient R(2) >0.9999. The limit of detection and limit of quantitation were estimated for all the five impurities. The established method was then validated for linearity, precision, accuracy, and specificity and demonstrated to be applicable to the determination of the active ingredients in commercial and model cough syrup. No interference from the formulation excipients was observed. These results suggest that this LC method can be used for the determination of multiple active ingredients and their impurities in a cough and cold syrup.

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

PubMed

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

2016-01-01

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

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

PubMed Central

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

2016-01-01

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

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

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

Comparative Assessment of the Effect of Hyper-glycosylation on the Pattern and Kinetics of Degradation of Darbepoetin Alfa using a Stability-Indicating Orthogonal Testing Protocol.

PubMed

Moenes, Eman M; Al-Ghobashy, Medhat A; Mohamed, Abeer A; Salem, Maissa Y

2018-01-01

Darbepoetin alfa (DA); hyper-glycosylated Erythropoietin alfa (EPO) is an essential treatment of anemia in patients with chronic kidney failure and cancer. In this study, DA and EPO were subjected to physicochemical stress factors that might be encountered during production, transport and storage (pH, temperature, agitation, repeated freeze-thaw and oxidation). An orthogonal stability-indicating assay protocol comprised of SE-HPLC, RP-HPLC, ELISA and SDS-PAGE was developed and validated to investigate the effect of further glycosylation of DA on the pattern and kinetics of degradation. Results showed a relatively higher stability and lower tendency to form high molecular weight aggregates in the case of DA when compared to EPO, under equivalent stress conditions. Dimers and aggregates were formed for both drugs across the whole pH range and following incubation at temperatures higher than 2-8°C or repeated freeze/thaw. The same observation was noted upon agitation of standard samples prepared in the formulation buffers at high speed and upon oxidation with hydrogen peroxide. The agreement between SE-HPLC, supported with spectral purity data and ELISA confirmed the specificity of both techniques for the intact drugs. Results of RP-HPLC and SDS-PAGE indicated that dimerization occurred through disulfide and bi-tyrosine covalent bonds in the case of pH and oxidation, respectively. It was evident that aggregation was significantly suppressed upon increasing the glycan size and under any of the studied stress factors loss of the glycan has not been observed. These observations supported with the slow kinetics of degradation confirmed the superiority of glyco-engineering over chemical pegylation to enhance the stability of EPO. Formation of such potentially immunogenic product-related impurities at all tested stress factors confirmed the need for orthogonal testing protocols to investigate the complex pattern of degradation of such sensitive products. Copyright © 2017 Elsevier B.V. All rights reserved.

A method to determine residue-specific unfolded-state pKa values from analysis of stability changes in single mutant cycles.

PubMed

Shen, Jana K

2010-06-02

It is now widely recognized that the unfolded state of a protein in equilibrium with the native state under folding conditions may contain significant residual structures. However, due to technical difficulties residue-specific interactions in the unfolded state remain elusive. Here we introduce a method derived from the Wyman-Tanford theory to determine residue-specific pK(a)'s in the unfolded state. This method requires equilibrium stability measurements of the wild type and single-point mutants in which titrable residues are replaced with charge-neutral ones under two pH conditions. Application of the proposed approach reveals a highly depressed pK(a) for Asp8 in the unfolded state of the NTL9 protein. Knowledge of unfolded-state pK(a)'s enables quantitative estimation of the unfolded-state electrostatic effects on protein stability. It also provides valuable benchmarks for the improvement of force fields and validation of microscopic information from molecular dynamics simulations.

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

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

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

2014-09-15

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

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.

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.

The use of National Weather Service Data to Compute the Dose to the MEOI.

PubMed

Vickers, Linda

2018-05-01

The Turner method is the "benchmark method" for computing the stability class that is used to compute the X/Q (s m). The Turner method should be used to ascertain the validity of X/Q results determined by other methods. This paper used site-specific meteorological data obtained from the National Weather Service. The Turner method described herein is simple, quick, accurate, and transparent because all of the data, calculations, and results are visible for verification and validation with published literature.

Linguistic and psychometric validation of the Malaysian version of Diabetes Quality of Life-Brief Clinical Inventory (DQoL-BCI).

PubMed

Samah, Syamimi; Neoh, Chin Fen; Wong, Yuet Yen; Hassali, Mohamed Azmi; Shafie, Asrul Akmal; Lim, Siong Meng; Ramasamy, Kalavathy; Mat Nasir, Nafiza; Han, Yung Wen; Burroughs, Thomas

2017-11-01

Quality of life (QoL) assessment provides valuable outcome to support clinical decision-making, particularly for patients with chronic diseases that are incurable. A brief, 15-item diabetes-specific tool [i.e. Diabetes Quality of Life-Brief Clinical Inventory (DQoL-BCI)] is known to be developed in English and validated for use in clinical practice. This simplified tool, however, is not readily available for use in the Malaysian setting. To translate the DQoL-BCI into a Malaysian version and to assess its construct validity (factorial validity, convergent validity and discriminant validity), reliability (internal consistency) and floor and ceiling effects among the Malaysian diabetic population. A forward-backward translation, involving professional translators and experts with vast experience in translation of patient reported outcome measures, was conducted. A total of 202 patients with Type 2 diabetes mellitus (T2DM) who fulfilled the inclusion criteria were invited to complete the translated DQoL-BCI. Data were analysed using SPSS for exploratory factor analysis (EFA), convergent and discriminant validity, reliability and test-retest, and AMOS software for confirmatory factor analysis (CFA). Findings from EFA indicated that the 4-factor structure of the Malaysian version of DQoL-BCI was optimal and explained 50.9% of the variance; CFA confirmed the 4-factor model fit. There was negative, moderate correlation between the scores of DQoL-BCI (Malaysian version) and EQ-5D-3L utility score (r = -0.329, p = 0.003). Patients with higher glycated haemoglobin levels (p = 0.008), diabetes macrovascular (p = 0.017) and microvascular (p = 0.013) complications reported poorer QoL. Cronbach's alpha coefficient and intraclass coefficient correlations (range) obtained were 0.703 and 0.86 (0.734-0.934), indicating good reliability and stability of the translated DQoL-BCI. This study had validated the linguistic and psychometric properties of DQoL-BCI (Malaysian version), thus providing a valid and reliable brief tool for assessing the QoL of Malaysian T2DM patients. Copyright © 2016 Elsevier Inc. All rights reserved.

The Resilience Questionnaire for Bipolar Disorder: Development and validation.

PubMed

Echezarraga, Ainara; Las Hayas, Carlota; González-Pinto, Ana María; Jones, Steven

2017-08-01

The goal of this research project was to develop a new questionnaire to assess resilience in Bipolar Disorder (BD), the Resilience Questionnaire for Bipolar Disorder (RBD). To examine its psychometric properties, a sample of 125 patients diagnosed with BD and a comparison sample of 107 people completed the new RBD and established measures of generic resilience and health-related outcomes. Exploratory factor analysis for the RBD yielded a 23-item 5-factor solution, and confirmatory factor analysis indicated adequate fit indices. Internal consistency, stability, concurrent validation and known-groups' validity were also supported. The RBD obtained higher responsiveness (6-month follow-up) than the generic resilience scale (BD sample). The RBD is a robust measure to monitor resilience in BD. Copyright © 2017 Elsevier Inc. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2015-06-01

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

Rank Order Entropy: why one metric is not enough

PubMed Central

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

2011-01-01

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

Development and validation of an attributional style questionnaire for adolescents.

PubMed

Rodríguez-Naranjo, Carmen; Caño, Antonio

2010-12-01

We describe the development and psychometric characteristics of a new version of the Attributional Style Questionnaire (ASQ; Seligman, Abramson, Semmell, & Von Baeyer, 1979)--a version called the Attributional Style Questionnaire for Adolescents (ASQ-A)--using 3 samples (Ns = 547, 438, and 240) of Spanish secondary school students. In Study 1, the initial pool of 87 items was reduced to 54. Study 2 further analyzed the 54 scale items and revealed that the Internality, Stability, and Globality subscale scores had good reliability, good factorial construct validity, and satisfactory associations with maladaptive mood ratings. In Study 3, the regression analyses showed good and specific predictive validities of ASQ-A subscales for the attributions that the adolescents made about a particular real-life stressful situation. Study 4 showed that over an 8-month period the changes in the Stability and Globality subscales depended on the intensity of stressful life events experienced in this period. Overall, the studies revealed that the new ASQ-A served as an appropriate instrument to assess attributional style in adolescents.

Clinical validation of the nursing diagnosis of ineffective protection in haemodialysis patients.

PubMed

de Sá Tinôco, Jéssica Dantas; de Paiva, Maria das Graças Mariano Nunes; de Queiroz Frazão, Cecília Maria Farias; Lucio, Kadyjina Daiane Batista; Fernandes, Maria Isabel da Conceição Dias; de Oliveira Lopes, Marcos Venicios; de Carvalho Lira, Ana Luisa Brandão

2018-01-01

To evaluate the clinical validity of indicators of the nursing diagnosis of "ineffective protection" in haemodialysis patients. Haemodialysis patients have reduced protection. Studies on the nursing diagnosis of "ineffective protection" are scarce in the literature. The use of indicators to diagnose "ineffective protection" could improve the care of haemodialysis patients. The clinical usefulness of the indicators requires clinical validation. This was a diagnostic accuracy study. This study assessed a sample of 200 patients undergoing haemodialysis in a reference clinic for nephrology during the first half of 2015. Operational definitions were created for each clinical indicator based on concept analysis and content validation by experts for these indicators. Diagnostic accuracy measurement was performed with latent class analysis with randomised effects. The clinical indicator of "fatigue" had high sensitivity (p = .999) and specificity (p = 1.000) for the identification of "ineffective protection." Additionally, "maladaptive response to stress" (p = .711) and "coagulation change" (p = .653) were sensitive indicators. The main indicators that showed high specificity were "fever" (p = .987), "increased number of hospitalisations" (p = .911), "weakness" (p = .937), "infected vascular access" (p = .962) and "vascular access dysfunction" (p = .722). A set of nine clinical indicators of "ineffective protection" were accurate and statistically significant for haemodialysis patients. Three clinical indicators showed sensitivity, and six indicators showed specificity. Accurate measures for nursing diagnoses can help nurses confirm or rule out the probability of the occurrence of "ineffective protection" in patients undergoing haemodialysis. © 2017 John Wiley & Sons Ltd.

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.

Disordered Cold Regulated15 Proteins Protect Chloroplast Membranes during Freezing through Binding and Folding, But Do Not Stabilize Chloroplast Enzymes in Vivo1[W][OPEN

PubMed Central

Thalhammer, Anja; Bryant, Gary; Sulpice, Ronan; Hincha, Dirk K.

2014-01-01

Freezing can severely damage plants, limiting geographical distribution of natural populations and leading to major agronomical losses. Plants native to cold climates acquire increased freezing tolerance during exposure to low nonfreezing temperatures in a process termed cold acclimation. This involves many adaptative responses, including global changes in metabolite content and gene expression, and the accumulation of cold-regulated (COR) proteins, whose functions are largely unknown. Here we report that the chloroplast proteins COR15A and COR15B are necessary for full cold acclimation in Arabidopsis (Arabidopsis thaliana). They protect cell membranes, as indicated by electrolyte leakage and chlorophyll fluorescence measurements. Recombinant COR15 proteins stabilize lactate dehydrogenase during freezing in vitro. However, a transgenic approach shows that they have no influence on the stability of selected plastidic enzymes in vivo, although cold acclimation results in increased enzyme stability. This indicates that enzymes are stabilized by other mechanisms. Recombinant COR15 proteins are disordered in water, but fold into amphipathic α-helices at high osmolyte concentrations in the presence of membranes, a condition mimicking molecular crowding induced by dehydration during freezing. X-ray scattering experiments indicate protein-membrane interactions specifically under such crowding conditions. The COR15-membrane interactions lead to liposome stabilization during freezing. Collectively, our data demonstrate the requirement for COR15 accumulation for full cold acclimation of Arabidopsis. The function of these intrinsically disordered proteins is the stabilization of chloroplast membranes during freezing through a folding and binding mechanism, but not the stabilization of chloroplastic enzymes. This indicates a high functional specificity of these disordered plant proteins. PMID:25096979

Stress Studies of Tenofovir Disoproxil Fumarate by HPTLC in Bulk Drug and Pharmaceutical Formulation

PubMed Central

Havele, Shweta; Dhaneshwar, Sunil R.

2012-01-01

A stability-indicating high-performance thin-layer chromatographic (HPTLC) method for determination of tenofovir disoproxil fumarate in bulk drug and in tablet has been developed and validated. The mobile phase selected was chloroform : methanol (9.0 : 1.0, v/v) with ultraviolet (UV) detection at 260 nm. The retention factor was found to be 0.49 ± 0.03 with correlation coefficients of 0.9994 in the range 300–1500 ng/spot and with an accuracy of 99.25%. Method had the potential to determine tenofovir disoproxil fumarate from tablet without any interference, and it was a stability-indicating one. PMID:22606065

Testing Postural Stability: Are the Star Excursion Balance Test and Biodex Balance System Limits of Stability Tests Consistent?

PubMed

Glave, A Page; Didier, Jennifer J; Weatherwax, Jacqueline; Browning, Sarah J; Fiaud, Vanessa

2016-01-01

There are a variety of options to test postural stability; however many physical tests lack validity information. Two tests of postural stability - the Star Excursion Balance Test (SEBT) and Biodex Balance System Limits of Stability Test (LOS) - were examined to determine if similar components of balance were measured. Healthy adults (n=31) completed the LOS (levels 6 and 12) and SEBT (both legs). SEBT directions were offset by 180° to approximate LOS direction. Correlations and partial correlations controlling for height were analyzed. Correlations were significant for SEBT 45° and LOS back-left (6: r=-0.41; 12: r=-0.42; p<0.05), SEBT 90° and LOS 6 left (r=-0.51, p<0.05), SEBT 135(o) and LOS 6 front-left (r=-0.53, p<0.05), SEBT overall and LOS 6 overall (r=-0.43, p<0.05). Partial correlations were significant for SEBT 90° and LOS 6 left (rSEBT,LOS·H=-0.45, p<0.05) and SEBT 135° and LOS 6 front-left (rSEBT,LOS·H=-0.51, p<0.05), and SEBT overall and LOS 6 overall (rSEBT,LOS·H=-0.37, p<0.05). These findings indicate the tests seem to assess different components of balance. Research is needed to determine and define what specific components of balance are being assessed. Care must be taken when choosing balance tests to best match the test to the purpose of testing (fall risk, athletic performance, etc.). Copyright © 2015 Elsevier B.V. All rights reserved.

Cross-Cultural Psychometric Assessment of the Leeds Assessment of Neuropathic Symptoms and Signs (LANSS) Pain Scale in the Portuguese Population.

PubMed

Barbosa, Margarida; Bennett, Michael I; Verissimo, Ramiro; Carvalho, Davide

2014-09-01

Chronic pain is a well-known phenomenon. The differential diagnosis between neuropathic and nociceptive pain syndromes is a challenge. Consequently, assessment instruments that can distinguish between these conditions in a standardized way are of the utmost importance. The Leeds Assessment of Neuropathic Symptoms and Signs (LANSS) is a screening tool developed to identify chronic neuropathic pain. The aim of this study was the Portuguese language translation, linguistic adaptation of the LANSS pain scale, its semantic validation, internal consistency, temporal stability, as well its validity and discriminative power. LANSS Portuguese version scale was applied to 165 consecutive patients attending the pain clinic: 103 fulfilled the clinical criteria for the diagnosis of pain of neuropathic origin and the remaining 62 fulfilled the criteria for nociceptive pain. The scale proved to be an internally consistent (Cronbach's alpha = 0.78) and reliable instrument with good test-retest stability (r = 0.7; P < 0.001). However, its validity and specificity with a cutoff point of ≥ 12, for differentiating patients with neuropathic pain from those with non-neuropathic pain, had 89% sensitivity, 74% specificity, positive predictive value of 85%, and negative predictive value of 81%. The Portuguese LANSS version pain scale properties lead us to the conclusion that such a cross-cultural version is a reliable and valid instrument for the differentiation of this type of pain. Its usage is recommended. © 2013 World Institute of Pain.

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

PubMed

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

2015-10-15

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

Recommendations for designing and conducting cold-fill hold challenge studies for acidified food products

USDA-ARS?s Scientific Manuscript database

A scheduled process developed for manufacture of acidified foods must be validated with data from existing literature or from a product-specific challenge study, either of which can establish both safety and shelf stability. The challenge study would evaluate the ability of a particular food product...

Development, optimization, and single laboratory validation of an event-specific real-time PCR method for the detection and quantification of Golden Rice 2 using a novel taxon-specific assay.

PubMed

Jacchia, Sara; Nardini, Elena; Savini, Christian; Petrillo, Mauro; Angers-Loustau, Alexandre; Shim, Jung-Hyun; Trijatmiko, Kurniawan; Kreysa, Joachim; Mazzara, Marco

2015-02-18

In this study, we developed, optimized, and in-house validated a real-time PCR method for the event-specific detection and quantification of Golden Rice 2, a genetically modified rice with provitamin A in the grain. We optimized and evaluated the performance of the taxon (targeting rice Phospholipase D α2 gene)- and event (targeting the 3' insert-to-plant DNA junction)-specific assays that compose the method as independent modules, using haploid genome equivalents as unit of measurement. We verified the specificity of the two real-time PCR assays and determined their dynamic range, limit of quantification, limit of detection, and robustness. We also confirmed that the taxon-specific DNA sequence is present in single copy in the rice genome and verified its stability of amplification across 132 rice varieties. A relative quantification experiment evidenced the correct performance of the two assays when used in combination.

Selection and Validation of Appropriate Reference Genes for qRT-PCR Analysis in Isatis indigotica Fort.

PubMed Central

Li, Tao; Wang, Jing; Lu, Miao; Zhang, Tianyi; Qu, Xinyun; Wang, Zhezhi

2017-01-01

Due to its sensitivity and specificity, real-time quantitative PCR (qRT-PCR) is a popular technique for investigating gene expression levels in plants. Based on the Minimum Information for Publication of Real-Time Quantitative PCR Experiments (MIQE) guidelines, it is necessary to select and validate putative appropriate reference genes for qRT-PCR normalization. In the current study, three algorithms, geNorm, NormFinder, and BestKeeper, were applied to assess the expression stability of 10 candidate reference genes across five different tissues and three different abiotic stresses in Isatis indigotica Fort. Additionally, the IiYUC6 gene associated with IAA biosynthesis was applied to validate the candidate reference genes. The analysis results of the geNorm, NormFinder, and BestKeeper algorithms indicated certain differences for the different sample sets and different experiment conditions. Considering all of the algorithms, PP2A-4 and TUB4 were recommended as the most stable reference genes for total and different tissue samples, respectively. Moreover, RPL15 and PP2A-4 were considered to be the most suitable reference genes for abiotic stress treatments. The obtained experimental results might contribute to improved accuracy and credibility for the expression levels of target genes by qRT-PCR normalization in I. indigotica. PMID:28702046

Developmental validation of an X-Insertion/Deletion polymorphism panel and application in HAN population of China.

PubMed

Zhang, Suhua; Sun, Kuan; Bian, Yingnan; Zhao, Qi; Wang, Zheng; Ji, Chaoneng; Li, Chengtao

2015-12-14

InDels are short-length polymorphisms characterized by low mutation rates, high inter-population diversity, short amplicon strategy and simplicity of laboratory analysis. This work describes the developmental validation of an X-InDels panel amplifying 18 bi-allelic markers and Amelogenin in one single PCR system. Developmental validation indicated that this novel panel was reproducible, accurate, sensitive and robust for forensic application. Sensitivity testing of the panel was such that a full profile was obtainable even with 125 pg of human DNA with intra-locus balance above 70%. Specificity testing was demonstrated by the lack of cross-reactivity with a variety of commonly encountered animal species and microorganisms. For the stability testing in cases of PCR inhibition, full profiles have been obtained with hematin (≤1000 μM) and humic acid (≤150 ng/μL). For the forensic investigation of the 18 X-InDels in the HAN population of China, no locus deviated from the Hardy-Weinberg equilibrium and linkage disequilibrium. Since they are independent from each other, the CDPfemale was 0.999999726 and CDPmale was 0.999934223. The forensic parameters suggested that this X-Indel panel is polymorphic and informative, which provides valuable X-linked information for deficient relationship cases where autosomal markers are uninformative.

Developmental validation of an X-Insertion/Deletion polymorphism panel and application in HAN population of China

PubMed Central

Zhang, Suhua; Sun, Kuan; Bian, Yingnan; Zhao, Qi; Wang, Zheng; Ji, Chaoneng; Li, Chengtao

2015-01-01

InDels are short-length polymorphisms characterized by low mutation rates, high inter-population diversity, short amplicon strategy and simplicity of laboratory analysis. This work describes the developmental validation of an X-InDels panel amplifying 18 bi-allelic markers and Amelogenin in one single PCR system. Developmental validation indicated that this novel panel was reproducible, accurate, sensitive and robust for forensic application. Sensitivity testing of the panel was such that a full profile was obtainable even with 125 pg of human DNA with intra-locus balance above 70%. Specificity testing was demonstrated by the lack of cross-reactivity with a variety of commonly encountered animal species and microorganisms. For the stability testing in cases of PCR inhibition, full profiles have been obtained with hematin (≤1000 μM) and humic acid (≤150 ng/μL). For the forensic investigation of the 18 X-InDels in the HAN population of China, no locus deviated from the Hardy–Weinberg equilibrium and linkage disequilibrium. Since they are independent from each other, the CDPfemale was 0.999999726 and CDPmale was 0.999934223. The forensic parameters suggested that this X-Indel panel is polymorphic and informative, which provides valuable X-linked information for deficient relationship cases where autosomal markers are uninformative. PMID:26655948

Development and validation of the Self-Stigma Questionnaire (SSQ) for people with schizophrenia and its relation to social functioning.

PubMed

Ochoa, Susana; Martínez-Zambrano, Francisco; Garcia-Franco, Mar; Vilamala, Sonia; Ribas, Maria; Arenas, Oti; Garcia-Morales, Esther; Álvarez, Irene; Escartin, Gemma; Villellas, Raul; Escandell, Maria Jose; Martínez-Raves, Mónica; López-Arias, Elisabeth; Cunyat, Christian; Haro, Josep Maria

2015-10-01

Self-stigma specifically in people with schizophrenia has been little studied. The aims of the present study were to validate a new instrument for the assessment of self-stigma (SSQ) and to assess the relationship between self-stigma and social functioning in people with schizophrenia. A sample of 76 people with schizophrenia was assessed at two moments in time with the SSQ, the PDD (stigma), two scales of social functioning (LSP, SFS), and a scale of general functioning (GAF). The results indicated that SSQ presented good psychometric properties, with Cronbach's alpha ranging between 0.75 and 0.901. The stability of the instrument was between 0.836 and 0.402. Three factors were found in the factor analysis (social discrimination, perceived capabilities, concealment of the disease), explaining 62.66% of the total variance. A relationship was found between self-stigma and social functioning in people with schizophrenia, especially in relation to social contact. In conclusion, the SSQ seems to be a valid and reliable questionnaire for the assessment of self-stigma in people with schizophrenia, and interventions should be designed to cope with self-stigma in order to improve the social functioning of people who suffer schizophrenia. Copyright © 2015 Elsevier Inc. All rights reserved.

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).

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 the results obtained by normal fluorescence and derivative synchronous methods and the official one using student's t-test and F-ratio showed no significant difference regarding accuracy and precision.

Trait-specific dependence in romantic relationships.

PubMed

Ellis, Bruce J; Simpson, Jeffry A; Campbell, Lorne

2002-10-01

Informed by three theoretical frameworks--trait psychology, evolutionary psychology, and interdependence theory--we report four investigations designed to develop and test the reliability and validity of a new construct and accompanying multiscale inventory, the Trait-Specific Dependence Inventory (TSDI). The TSDI assesses comparisons between present and alternative romantic partners on major dimensions of mate value. In Study 1, principal components analyses revealed that the provisional pool of theory-generated TSDI items were represented by six factors: Agreeable/Committed, Resource Accruing Potential, Physical Prowess, Emotional Stability, Surgency, and Physical Attractiveness. In Study 2, confirmatory factor analysis replicated these results on a different sample and tested how well different structural models fit the data. Study 3 provided evidence for the convergent and discriminant validity of the six TSDI scales by correlating each one with a matched personality trait scale that did not explicitly incorporate comparisons between partners. Study 4 provided further validation evidence, revealing that the six TSDI scales successfully predicted three relationship outcome measures--love, time investment, and anger/upset--above and beyond matched sets of traditional personality trait measures. These results suggest that the TSDI is a reliable, valid, and unique construct that represents a new trait-specific method of assessing dependence in romantic relationships. The construct of trait-specific dependence is introduced and linked with other theories of mate value.

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.

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

PubMed

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

2015-07-01

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

Software for imaging phase-shift interference microscope

NASA Astrophysics Data System (ADS)

Malinovski, I.; França, R. S.; Couceiro, I. B.

2018-03-01

In recent years absolute interference microscope was created at National Metrology Institute of Brazil (INMETRO). The instrument by principle of operation is imaging phase-shifting interferometer (PSI) equipped with two stabilized lasers of different colour as traceable reference wavelength sources. We report here some progress in development of the software for this instrument. The status of undergoing internal validation and verification of the software is also reported. In contrast with standard PSI method, different methodology of phase evaluation is applied. Therefore, instrument specific procedures for software validation and verification are adapted and discussed.

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.

Stability of Cyclophosphamide in Extemporaneous Oral Suspensions

PubMed Central

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

2010-01-01

Background 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. Objectives The goals of this study were (1) to develop and validate a stability-indicating HPLC method to measure cyclophosphamide concentrations in simple syrup and Ora-Plus, and (2) to assess the 56-day chemical stability and physical appearance of cyclophosphamide in these suspensions at both room temperature and 4°C. Methods The i.v. formulation of cyclophosphamide was diluted to 20 mg/mL in normal saline, compounded 1:1 with either suspending vehicle, and stored in the dark in 3mL amber polypropylene oral syringes at 4°C and 22°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. Results Samples of cyclophosphamide in both simple syrup and Ora-Plus were stable when kept at 4°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. Conclusion Cyclophosphamide can be extemporaneously prepared in simple syrup or Ora-Plus and stored at least 2 months under refrigeration without significant degradation. PMID:20103616

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.

Dynamic trunk stabilization: a conceptual back injury prevention program for volleyball athletes.

PubMed

Smith, Chad E; Nyland, John; Caudill, Paul; Brosky, Joseph; Caborn, David N M

2008-11-01

The sport of volleyball creates considerable dynamic trunk stability demands. Back injury occurs all too frequently in volleyball, particularly among female athletes. The purpose of this clinical commentary is to review functional anatomy, muscle coactivation strategies, assessment of trunk muscle performance, and the characteristics of effective exercises for the trunk or core. From this information, a conceptual progressive 3-phase volleyball-specific training program is presented to improve dynamic trunk stability and to potentially reduce the incidence of back injury among volleyball athletes. Phase 1 addresses low-velocity motor control, kinesthetic awareness, and endurance, with the clinician providing cues to teach achievement of biomechanically neutral spine alignment. Phase 2 focuses on progressively higher velocity dynamic multiplanar endurance, coordination, and strength-power challenges integrating upper and lower extremity movements, while maintaining neutral spine alignment. Phase 3 integrates volleyball-specific skill simulations by breaking down composite movement patterns into their component parts, with differing dynamic trunk stability requirements, while maintaining neutral spine alignment. Prospective research is needed to validate the efficacy of this program.

Psychometric properties evaluation of a new ergonomics-related job factors questionnaire developed for nursing workers.

PubMed

Coluci, Marina Zambon Orpinelli; Alexandre, Neusa Maria Costa

2014-11-01

The objectives of this study were to develop a questionnaire that evaluates the perception of nursing workers to job factors that may contribute to musculoskeletal symptoms, and to evaluate its psychometric properties. Internationally recommended methodology was followed: construction of domains, items and the instrument as a whole, content validity, and pre-test. Psychometric properties were evaluated among 370 nursing workers. Construct validity was analyzed by the factorial analysis, known-groups technique, and convergent validity. Reliability was assessed through internal consistency and stability. Results indicated satisfactory fit indices during confirmatory factor analysis, significant difference (p < 0.01) between the responses of nursing and office workers, and moderate correlations between the new questionnaire and Numeric Pain Scale, SF-36 and WRFQ. Cronbach's alpha was close to 0.90 and ICC values ranged from 0.64 to 0.76. Therefore, results indicated that the new questionnaire had good psychometric properties for use in studies involving nursing workers. Copyright © 2014 Elsevier Ltd and The Ergonomics Society. All rights reserved.

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.

Tests for the Assessment of Sport-Specific Performance in Olympic Combat Sports: A Systematic Review With Practical Recommendations.

PubMed

Chaabene, Helmi; Negra, Yassine; Bouguezzi, Raja; Capranica, Laura; Franchini, Emerson; Prieske, Olaf; Hbacha, Hamdi; Granacher, Urs

2018-01-01

The regular monitoring of physical fitness and sport-specific performance is important in elite sports to increase the likelihood of success in competition. This study aimed to systematically review and to critically appraise the methodological quality, validation data, and feasibility of the sport-specific performance assessment in Olympic combat sports like amateur boxing, fencing, judo, karate, taekwondo, and wrestling. A systematic search was conducted in the electronic databases PubMed, Google-Scholar, and Science-Direct up to October 2017. Studies in combat sports were included that reported validation data (e.g., reliability, validity, sensitivity) of sport-specific tests. Overall, 39 studies were eligible for inclusion in this review. The majority of studies (74%) contained sample sizes <30 subjects. Nearly, 1/3 of the reviewed studies lacked a sufficient description (e.g., anthropometrics, age, expertise level) of the included participants. Seventy-two percent of studies did not sufficiently report inclusion/exclusion criteria of their participants. In 62% of the included studies, the description and/or inclusion of a familiarization session (s) was either incomplete or not existent. Sixty-percent of studies did not report any details about the stability of testing conditions. Approximately half of the studies examined reliability measures of the included sport-specific tests (intraclass correlation coefficient [ICC] = 0.43-1.00). Content validity was addressed in all included studies, criterion validity (only the concurrent aspect of it) in approximately half of the studies with correlation coefficients ranging from r = -0.41 to 0.90. Construct validity was reported in 31% of the included studies and predictive validity in only one. Test sensitivity was addressed in 13% of the included studies. The majority of studies (64%) ignored and/or provided incomplete information on test feasibility and methodological limitations of the sport-specific test. In 28% of the included studies, insufficient information or a complete lack of information was provided in the respective field of the test application. Several methodological gaps exist in studies that used sport-specific performance tests in Olympic combat sports. Additional research should adopt more rigorous validation procedures in the application and description of sport-specific performance tests in Olympic combat sports.

Boundary layer stability on a yawed spinning body of revolution and its effect on the magnus force and moment

NASA Technical Reports Server (NTRS)

Jacobson, I. D.; Morton, J. B.

1972-01-01

The parameters are established which are important to the stability of a boundary layer flow over a yawed spinning cylinder in a uniform stream. It is shown that transition occurs asymmetrically in general and this asymmetry can be important for the prediction of aerodynamic forces and moments (e.g., the Magnus effect). Instability of the steady-state boundary layer flow is determined using small disturbance theory. Although the approach is strictly valid only for the calculation of the conditions for stability in the small, experimental data indicate that in many problems, it provides a good estimate for the transition to turbulence.

Media ratings for movies, music, video games, and television: a review of the research and recommendations for improvements.

PubMed

Gentile, Douglas A; Humphrey, Jeremy; Walsh, David A

2005-06-01

This article review is organized by studies that are relevant for testing the reliability and validity of ratings systems. Specifically, the interrater reliability, consistency, temporal stability, content validity, construct validity, and criterion validity of media ratings systems are reviewed. Data that are related to testing the "forbidden fruit" and "tainted fruit" hypotheses also are reviewed. Several changes are recommended to improve the ratings systems, including the creation of a universal ratings system that could be applied equally to all media. The research reviewed here can provide a guide for how to construct a reliable, valid, and more useful ratings system. This is important because the decisions that parents make regarding their children's media use can be only as good as the information to which the parents have access.

Liquid chromatography/tandem mass spectrometry method for simultaneous determination of cocaine and its metabolite (-)ecgonine methyl ester in human acidified stabilized plasma samples.

PubMed

Liu, Yongzhen; Zheng, Bo; Strafford, Stephanie; Orugunty, Ravi; Sullivan, Michael; Gus, Jeffrey; Heidbreder, Christian; Fudala, Paul J; Nasser, Azmi

2014-06-15

Two simple, sensitive and rapid liquid chromatography/electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) methods (low range and high range) were developed and validated for the quantification of cocaine and its metabolite (-)ecgonine methyl ester (EME) in human acidified stabilized plasma samples. In the low range assay, cocaine and the internal standard, cocaine-D3, were extracted using a single step liquid-liquid extraction from human acidified stabilized plasma. For the high range assay, human acidified stabilized plasma containing cocaine, EME, and the internal standards, cocaine-D3 and EME-D3, was mixed with acetonitrile, and the protein precipitate was separated by centrifugation. Both cocaine and EME extracted from both assays were separated on a HILIC column and detected in positive ion mode using multiple reaction monitoring (MRM). Both methods were validated and the specificity, linearity, lower limit of quantitation (LLOQ), precision, accuracy, recoveries and stability were determined. The linear range for the low range assay was 0.01-5ng/mL for cocaine; in the high range assay values were 5-1000ng/mL for cocaine and 1-200ng/mL for EME. The correlation coefficient (R(2)) values for both assays were 0.993 or greater. The precision and accuracy for intra-day and inter-day were better than 13.0%. The recovery was above 85% and matrix effects were low with the matrix factor ranging from 0.817 to 1.10 for both analytes in both assays. The validated methods were successfully used to quantify the plasma concentrations of cocaine and EME in clinical pharmacokinetic and pharmacodynamic studies. Copyright © 2014 Elsevier B.V. All rights reserved.

miREE: miRNA recognition elements ensemble

PubMed Central

2011-01-01

Background Computational methods for microRNA target prediction are a fundamental step to understand the miRNA role in gene regulation, a key process in molecular biology. In this paper we present miREE, a novel microRNA target prediction tool. miREE is an ensemble of two parts entailing complementary but integrated roles in the prediction. The Ab-Initio module leverages upon a genetic algorithmic approach to generate a set of candidate sites on the basis of their microRNA-mRNA duplex stability properties. Then, a Support Vector Machine (SVM) learning module evaluates the impact of microRNA recognition elements on the target gene. As a result the prediction takes into account information regarding both miRNA-target structural stability and accessibility. Results The proposed method significantly improves the state-of-the-art prediction tools in terms of accuracy with a better balance between specificity and sensitivity, as demonstrated by the experiments conducted on several large datasets across different species. miREE achieves this result by tackling two of the main challenges of current prediction tools: (1) The reduced number of false positives for the Ab-Initio part thanks to the integration of a machine learning module (2) the specificity of the machine learning part, obtained through an innovative technique for rich and representative negative records generation. The validation was conducted on experimental datasets where the miRNA:mRNA interactions had been obtained through (1) direct validation where even the binding site is provided, or through (2) indirect validation, based on gene expression variations obtained from high-throughput experiments where the specific interaction is not validated in detail and consequently the specific binding site is not provided. Conclusions The coupling of two parts: a sensitive Ab-Initio module and a selective machine learning part capable of recognizing the false positives, leads to an improved balance between sensitivity and specificity. miREE obtains a reasonable trade-off between filtering false positives and identifying targets. miREE tool is available online at http://didattica-online.polito.it/eda/miREE/ PMID:22115078

Validation of Self-Report Impairment Measures for Section III Obsessive-Compulsive and Avoidant Personality Disorders.

PubMed

Liggett, Jacqueline; Carmichael, Kieran L C; Smith, Alexander; Sellbom, Martin

2017-01-01

This study examined the validity of newly developed disorder-specific impairment scales (IS), modeled on the Level of Personality Functioning Scale, for obsessive-compulsive (OCPD) and avoidant (AvPD) personality disorders. The IS focused on content validity (items directly reflected the disorder-specific impairments listed in DSM-5 Section III) and severity of impairment. A community sample of 313 adults completed personality inventories indexing the DSM-5 Sections II and III diagnostic criteria for OCPD and AvPD, as well as measures of impairment in the domains of self- and interpersonal functioning. Results indicated that both impairment measures (for AvPD in particular) showed promise in their ability to measure disorder-specific impairment, demonstrating convergent validity with their respective Section II counterparts and discriminant validity with their noncorresponding Section II disorder and with each other. The pattern of relationships between scores on the IS and scores on external measures of personality functioning, however, did not indicate that it is useful to maintain a distinction between impairment in the self- and interpersonal domains, at least for AvPD and OCPD.

Value-Added Teacher Estimates as Part of Teacher Evaluations: Exploring the Effects of Data and Model Specifications on the Stability of Teacher Value-Added Scores

ERIC Educational Resources Information Center

Kersting, Nicole B.; Chen, Mei-kuang; Stigler, James W.

2013-01-01

If teacher value-added estimates (VAEs) are to be used as indicators of individual teacher performance in teacher evaluation and accountability systems, it is important to understand how much VAEs are affected by the data and model specifications used to estimate them. In this study we explored the effects of three conditions on the stability of…

Stability of minoxidil in Espumil foam base.

PubMed

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

2013-01-01

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

Validation of the REA bioassay to detect estrogenic activity in the water cycle.

PubMed

Nguyen, Mai Thao; van der Oost, Ron; Bovee, Toine F H

2011-12-01

Endocrine disrupting compounds (EDCs) with estrogenic potency contaminate water and might eventually cause adverse effects to the aquatic environment. Many estrogenic compounds are not completely removed by wastewater treatment systems and, together with the run-off from agricultural areas, they enter surface waters. Chemical analytical methods to determine these compounds are usually expensive and laborious. Therefore, screening bioassays which are able to detect compounds based on their effects offer a solution for prior selection of samples that need to be chemically analyzed. In this study, the REA (RIKILT yeast Estrogen bioAssay), which has been developed to detect estrogenic compounds in calf urine and animal feed at RIKILT, is validated at the Water Board Laboratory of Waterproef for water samples. According to EC Decision 2002/657, detection capability CCβ, specificity and stability have to be determined for the internal validation of a qualitative screening test. In addition, surface water and effluent samples were analyzed to further demonstrate the applicability of the validated test procedure. Results demonstrate that the REA assay is reproducible and specific for estrogenic compounds in water and meets the criteria as prescribed in EC Decision 2002/657. The assay was sensitive enough to detect estrogenic activity of pollutants in water with a limit of quantification (LOQ) below 1 ng EEQ/L. This means that samples can be compared with preliminary threshold levels for drinking water and surface waters (7 and 1 ng EEQ/L, respectively). The stability of estrogenic activity in water samples is at least 4 weeks, when stored at 4 °C. Copyright © 2011 Elsevier Ltd. All rights reserved.

An experimentally validated network of nine haematopoietic transcription factors reveals mechanisms of cell state stability

PubMed Central

Schütte, Judith; Wang, Huange; Antoniou, Stella; Jarratt, Andrew; Wilson, Nicola K; Riepsaame, Joey; Calero-Nieto, Fernando J; Moignard, Victoria; Basilico, Silvia; Kinston, Sarah J; Hannah, Rebecca L; Chan, Mun Chiang; Nürnberg, Sylvia T; Ouwehand, Willem H; Bonzanni, Nicola; de Bruijn, Marella FTR; Göttgens, Berthold

2016-01-01

Transcription factor (TF) networks determine cell-type identity by establishing and maintaining lineage-specific expression profiles, yet reconstruction of mammalian regulatory network models has been hampered by a lack of comprehensive functional validation of regulatory interactions. Here, we report comprehensive ChIP-Seq, transgenic and reporter gene experimental data that have allowed us to construct an experimentally validated regulatory network model for haematopoietic stem/progenitor cells (HSPCs). Model simulation coupled with subsequent experimental validation using single cell expression profiling revealed potential mechanisms for cell state stabilisation, and also how a leukaemogenic TF fusion protein perturbs key HSPC regulators. The approach presented here should help to improve our understanding of both normal physiological and disease processes. DOI: http://dx.doi.org/10.7554/eLife.11469.001 PMID:26901438

The development and psychometric assessment of a questionnaire to assess sleep and daily troubles in parents of children and young adults with severe psychomotor impairment.

PubMed

Tietze, Anna L; Zernikow, Boris; Otto, Michael; Hirschfeld, Gerrit; Michel, Erik; Koh, Michelle; Blankenburg, Markus

2014-02-01

Children with severe psychomotor impairment (SPMI) often experience sleep disturbances that severely distress both the child and his or her parents. Validated questionnaires for the assessment of parents' distress related to their child's sleep disturbances are lacking. We developed and validated a new questionnaire, the HOST (holistic assessment of sleep and daily troubles in parents of children with SPMI) to assess the effect of the sleep disturbances in children with SPMI on their parents. The questionnaire was developed based on published data and expert opinion, and it was refined via direct consultation with affected parents. Its psychometric characteristics were assessed in a sample of parents of 214 children with SPMI. It was retested using a random subsample of the participants. Explorative factor analysis revealed that the HOST was composed of four scales. Fit indices, item analysis, and convergent validity (coherence with preexisting instruments of sleep disturbances and health status) were adequate. Retest analysis (n=62) revealed high stability of the HOST questionnaire and adequate replication validity. Sleep-related difficulties significantly impact the sociomedical characteristics of the parents of children with complex neurologic diseases. Typically, parents are severely affected in various aspects of daily life (i.e., medical health, social life, professional life). The HOST proved to be a valid, reliable and economical assessment tool of sleep-related difficulties in parents and relatives of children with SPMI. The HOST is capable of identifying individuals and specific areas requiring intervention. Copyright © 2013 Elsevier B.V. All rights reserved.

Relapse Risk Assessment for Schizophrenia Patients (RASP): A New Self-Report Screening Tool.

PubMed

Velligan, Dawn; Carpenter, William; Waters, Heidi C; Gerlanc, Nicole M; Legacy, Susan N; Ruetsch, Charles

2018-01-01

The Relapse Assessment for Schizophrenia Patients (RASP) was developed as a six-question self-report screener that measures indicators of Increased Anxiety and Social Isolation to assess patient stability and predict imminent relapse. This paper describes the development and psychometric characteristics of the RASP. The RASP and Positive and Negative Syndrome Scale (PANSS) were administered to patients with schizophrenia (n=166) three separate times. Chart data were collected on a subsample of patients (n=81). Psychometric analyses of RASP included tests of reliability, construct validity, and concurrent validity of items. Factors from RASP were correlated with subscales from PANSS (sensitivity to change and criterion validity [agreement between RASP and evidence of relapse]). Test-retest reliability returned modest to strong agreement at the item level and strong agreement at the questionnaire level. RASP showed good item response curves and internal consistency for the total instrument and within each of the two subscales (Increased Anxiety and Social Isolation). RASP Total Score and subscales showed good concurrent validity when correlated with PANSS Total Score, Positive, Excitement, and Anxiety subscales. RASP correctly predicted relapse in 67% of cases, with good specificity and negative predictive power and acceptable positive predictive power and sensitivity. The reliability and validity data presented support the use of RASP in settings where addition of a brief self-report assessment of relapse risk among patients with schizophrenia may be of benefit. Ease of use and scoring, and the ability to administer without clinical supervision allows for routine administration and assessment of relapse risk.

Introducing conjoint analysis method into delayed lotteries studies: its validity and time stability are higher than in adjusting.

PubMed

Białek, Michał; Markiewicz, Łukasz; Sawicki, Przemysław

2015-01-01

The delayed lotteries are much more common in everyday life than are pure lotteries. Usually, we need to wait to find out the outcome of the risky decision (e.g., investing in a stock market, engaging in a relationship). However, most research has studied the time discounting and probability discounting in isolation using the methodologies designed specifically to track changes in one parameter. Most commonly used method is adjusting, but its reported validity and time stability in research on discounting are suboptimal. The goal of this study was to introduce the novel method for analyzing delayed lotteries-conjoint analysis-which hypothetically is more suitable for analyzing individual preferences in this area. A set of two studies compared the conjoint analysis with adjusting. The results suggest that individual parameters of discounting strength estimated with conjoint have higher predictive value (Study 1 and 2), and they are more stable over time (Study 2) compared to adjusting. We discuss these findings, despite the exploratory character of reported studies, by suggesting that future research on delayed lotteries should be cross-validated using both methods.

Stability-based validation of dietary patterns obtained by cluster analysis.

PubMed

Sauvageot, Nicolas; Schritz, Anna; Leite, Sonia; Alkerwi, Ala'a; Stranges, Saverio; Zannad, Faiez; Streel, Sylvie; Hoge, Axelle; Donneau, Anne-Françoise; Albert, Adelin; Guillaume, Michèle

2017-01-14

Cluster analysis is a data-driven method used to create clusters of individuals sharing similar dietary habits. However, this method requires specific choices from the user which have an influence on the results. Therefore, there is a need of an objective methodology helping researchers in their decisions during cluster analysis. The objective of this study was to use such a methodology based on stability of clustering solutions to select the most appropriate clustering method and number of clusters for describing dietary patterns in the NESCAV study (Nutrition, Environment and Cardiovascular Health), a large population-based cross-sectional study in the Greater Region (N = 2298). Clustering solutions were obtained with K-means, K-medians and Ward's method and a number of clusters varying from 2 to 6. Their stability was assessed with three indices: adjusted Rand index, Cramer's V and misclassification rate. The most stable solution was obtained with K-means method and a number of clusters equal to 3. The "Convenient" cluster characterized by the consumption of convenient foods was the most prevalent with 46% of the population having this dietary behaviour. In addition, a "Prudent" and a "Non-Prudent" patterns associated respectively with healthy and non-healthy dietary habits were adopted by 25% and 29% of the population. The "Convenient" and "Non-Prudent" clusters were associated with higher cardiovascular risk whereas the "Prudent" pattern was associated with a decreased cardiovascular risk. Associations with others factors showed that the choice of a specific dietary pattern is part of a wider lifestyle profile. This study is of interest for both researchers and public health professionals. From a methodological standpoint, we showed that using stability of clustering solutions could help researchers in their choices. From a public health perspective, this study showed the need of targeted health promotion campaigns describing the benefits of healthy dietary patterns.

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.

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.

Validation of the Acoustic Voice Quality Index in the Japanese Language.

PubMed

Hosokawa, Kiyohito; Barsties, Ben; Iwahashi, Toshihiko; Iwahashi, Mio; Kato, Chieri; Iwaki, Shinobu; Sasai, Hisanori; Miyauchi, Akira; Matsushiro, Naoki; Inohara, Hidenori; Ogawa, Makoto; Maryn, Youri

2017-03-01

The Acoustic Voice Quality Index (AVQI) is a multivariate construct for quantification of overall voice quality based on the analysis of continuous speech and sustained vowel. The stability and validity of the AVQI is well established in several language families. However, the Japanese language has distinct characteristics with respect to several parameters of articulatory and phonatory physiology. The aim of the study was to confirm the criterion-related concurrent validity of AVQI, as well as its responsiveness to change and diagnostic accuracy for voice assessment in the Japanese-speaking population. This is a retrospective study. A total of 336 voice recordings, which included 69 pairs of voice recordings (before and after therapeutic interventions), were eligible for the study. The auditory-perceptual judgment of overall voice quality was evaluated by five experienced raters. The concurrent validity, responsiveness to change, and diagnostic accuracy of the AVQI were estimated. The concurrent validity and responsiveness to change based on the overall voice quality was indicated by high correlation coefficients 0.828 and 0.767, respectively. Receiver operating characteristic analysis revealed an excellent diagnostic accuracy for discrimination between dysphonic and normophonic voices (area under the curve: 0.905). The best threshold level for the AVQI of 3.15 corresponded with a sensitivity of 72.5% and specificity of 95.2%, with the positive and negative likelihood ratios of 15.1 and 0.29, respectively. We demonstrated the validity of the AVQI as a tool for assessment of overall voice quality and that of voice therapy outcomes in the Japanese-speaking population. Copyright © 2017 The Voice Foundation. Published by Elsevier Inc. All rights reserved.

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.

Plasma Transport and Magnetic Flux Circulation in Saturn's Magnetosphere

NASA Astrophysics Data System (ADS)

Neupane, B. R.; Delamere, P. A.; Ma, X.; Wilson, R. J.

2017-12-01

Radial transport of plasma in the rapidly rotating magnetospheres is an important dynamical process. Radial transport is due to the centrifugally driven interchange instability and magnetodisc reconnection, allowing net mass to be transported outward while conserving magnetic flux. Using Cassini Plasma Spectrometer instrument (CAPS) data products (e.g., Thomsen et al., [2010]; Wilson et al., [2017]) we estimate plasma mass and magnetic flux transport rates as functions of radial distance and local time. The physical requirement for zero net magnetic flux transport provides a key benchmark for assessing the validity of our mass transport estimate. We also evaluate magnetodisc stability using a two-dimensional axisymmetric equilibrium model [Caudal, 1986]. Observed local properties (e.g., specific entropy and estimates of flux tube mass and entropy content) are compared with modeled equilibrium conditions such that departures from equilibrium can be correlated with radial flows and local magnetic field structure. Finally, observations of specific entropy indicate that plasma is non-adiabatic heated during transport. However, the values of specific entropy are well organized in inner magnetosphere (i.e. L<10), and become widely scattered in the middle magnetosphere, suggesting that the transport dynamics of the inner and middle magnetosphere are different.

Proteins QSAR with Markov average electrostatic potentials.

PubMed

González-Díaz, Humberto; Uriarte, Eugenio

2005-11-15

Classic physicochemical and topological indices have been largely used in small molecules QSAR but less in proteins QSAR. In this study, a Markov model is used to calculate, for the first time, average electrostatic potentials xik for an indirect interaction between aminoacids placed at topologic distances k within a given protein backbone. The short-term average stochastic potential xi1 for 53 Arc repressor mutants was used to model the effect of Alanine scanning on thermal stability. The Arc repressor is a model protein of relevance for biochemical studies on bioorganics and medicinal chemistry. A linear discriminant analysis model developed correctly classified 43 out of 53, 81.1% of proteins according to their thermal stability. More specifically, the model classified 20/28, 71.4% of proteins with near wild-type stability and 23/25, 92.0% of proteins with reduced stability. Moreover, predictability in cross-validation procedures was of 81.0%. Expansion of the electrostatic potential in the series xi0, xi1, xi2, and xi3, justified the use of the abrupt truncation approach, being the overall accuracy >70.0% for xi0 but equal for xi1, xi2, and xi3. The xi1 model compared favorably with respect to others based on D-Fire potential, surface area, volume, partition coefficient, and molar refractivity, with less than 77.0% of accuracy [Ramos de Armas, R.; González-Díaz, H.; Molina, R.; Uriarte, E. Protein Struct. Func. Bioinf.2004, 56, 715]. The xi1 model also has more tractable interpretation than others based on Markovian negentropies and stochastic moments. Finally, the model is notably simpler than the two models based on quadratic and linear indices. Both models, reported by Marrero-Ponce et al., use four-to-five time more descriptors. Introduction of average stochastic potentials may be useful for QSAR applications; having xik amenable physical interpretation and being very effective.

Stability of Behavioral Ratings of Children with SLI.

ERIC Educational Resources Information Center

Redmond, Sean M.; Rice, Mabel L.

2002-01-01

A study investigated the long-term stability of the teacher and parent behavioral ratings of 37 children with specific language impairment. Results indicate diminishment in teacher-reported behavior problems in most areas of socioemotional development from kindergarten to second grade and increasing congruence between teacher and parent ratings.…

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

PubMed

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

2017-04-12

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

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.

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

The Self-esteem Stability Scale (SESS) for Cross-Sectional Direct Assessment of Self-esteem Stability

PubMed Central

Altmann, Tobias; Roth, Marcus

2018-01-01

Self-esteem stability describes fluctuations in the level of self-esteem experienced by individuals over a brief period of time. In recent decades, self-esteem stability has repeatedly been shown to be an important variable affecting psychological functioning. However, measures of self-esteem stability are few and lacking in validity. In this paper, we present the Self-Esteem Stability Scale (SESS), a unidimensional and very brief scale to directly assess self-esteem stability. In four studies (total N = 826), we describe the development of the SESS and present evidence for its validity with respect to individual outcomes (life satisfaction, neuroticism, and vulnerable narcissism) and dyadic outcomes (relationship satisfaction in self- and partner ratings) through direct comparisons with existing measures. The new SESS proved to be a stronger predictor than the existing scales and had incremental validity over and above self-esteem level. The results also showed that all cross-sectional measures of self-esteem stability were only moderately associated with variability in self-esteem levels assessed longitudinally with multiple administrations of the Rosenberg Self-Esteem Scale. We discuss this validity issue, arguing that direct and indirect assessment approaches measure relevant, yet different aspects of self-esteem stability. PMID:29487551

The Self-esteem Stability Scale (SESS) for Cross-Sectional Direct Assessment of Self-esteem Stability.

PubMed

Altmann, Tobias; Roth, Marcus

2018-01-01

Self-esteem stability describes fluctuations in the level of self-esteem experienced by individuals over a brief period of time. In recent decades, self-esteem stability has repeatedly been shown to be an important variable affecting psychological functioning. However, measures of self-esteem stability are few and lacking in validity. In this paper, we present the Self-Esteem Stability Scale (SESS), a unidimensional and very brief scale to directly assess self-esteem stability. In four studies (total N = 826), we describe the development of the SESS and present evidence for its validity with respect to individual outcomes (life satisfaction, neuroticism, and vulnerable narcissism) and dyadic outcomes (relationship satisfaction in self- and partner ratings) through direct comparisons with existing measures. The new SESS proved to be a stronger predictor than the existing scales and had incremental validity over and above self-esteem level. The results also showed that all cross-sectional measures of self-esteem stability were only moderately associated with variability in self-esteem levels assessed longitudinally with multiple administrations of the Rosenberg Self-Esteem Scale. We discuss this validity issue, arguing that direct and indirect assessment approaches measure relevant, yet different aspects of self-esteem stability.

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.

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.

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

PubMed

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

2015-01-01

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

Cluster Analysis of Rat Olfactory Bulb Responses to Diverse Odorants

PubMed Central

Falasconi, Matteo; Leon, Michael; Johnson, Brett A.; Marco, Santiago

2012-01-01

In an effort to deepen our understanding of mammalian olfactory coding, we have used an objective method to analyze a large set of odorant-evoked activity maps collected systematically across the rat olfactory bulb to determine whether such an approach could identify specific glomerular regions that are activated by related odorants. To that end, we combined fuzzy c-means clustering methods with a novel validity approach based on cluster stability to evaluate the significance of the fuzzy partitions on a data set of glomerular layer responses to a large diverse group of odorants. Our results confirm the existence of glomerular response clusters to similar odorants. They further indicate a partial hierarchical chemotopic organization wherein larger glomerular regions can be subdivided into smaller areas that are rather specific in their responses to particular functional groups of odorants. These clusters bear many similarities to, as well as some differences from, response domains previously proposed for the glomerular layer of the bulb. These data also provide additional support for the concept of an identity code in the mammalian olfactory system. PMID:22459165

Assessing the stability of human locomotion: a review of current measures

PubMed Central

Bruijn, S. M.; Meijer, O. G.; Beek, P. J.; van Dieën, J. H.

2013-01-01

Falling poses a major threat to the steadily growing population of the elderly in modern-day society. A major challenge in the prevention of falls is the identification of individuals who are at risk of falling owing to an unstable gait. At present, several methods are available for estimating gait stability, each with its own advantages and disadvantages. In this paper, we review the currently available measures: the maximum Lyapunov exponent (λS and λL), the maximum Floquet multiplier, variability measures, long-range correlations, extrapolated centre of mass, stabilizing and destabilizing forces, foot placement estimator, gait sensitivity norm and maximum allowable perturbation. We explain what these measures represent and how they are calculated, and we assess their validity, divided up into construct validity, predictive validity in simple models, convergent validity in experimental studies, and predictive validity in observational studies. We conclude that (i) the validity of variability measures and λS is best supported across all levels, (ii) the maximum Floquet multiplier and λL have good construct validity, but negative predictive validity in models, negative convergent validity and (for λL) negative predictive validity in observational studies, (iii) long-range correlations lack construct validity and predictive validity in models and have negative convergent validity, and (iv) measures derived from perturbation experiments have good construct validity, but data are lacking on convergent validity in experimental studies and predictive validity in observational studies. In closing, directions for future research on dynamic gait stability are discussed. PMID:23516062

The premature ejaculation diagnostic tool (PEDT): linguistic validity of the Chinese version.

PubMed

Huang, Yan-Ping; Chen, Bin; Ping, Ping; Wang, Hong-Xiang; Hu, Kai; Zhang, Tao; Yang, Hao; Jin, Yan; Yang, Qi; Huang, Yi-Ran

2014-09-01

The premature ejaculation diagnostic tool (PEDT) was developed to standardize the diagnosis of PE and has been applied in many countries. However, a linguistic validation of the Chinese version of PEDT does not exist. This study aims to undertake the Chinese validation of the PEDT and to evaluate its association with self-estimated intravaginal ejaculatory latency time (IELT) and clinical expert diagnosis of PE. A Chinese version of PEDT was confirmed by andrologist and bilingual linguist. Participants were recruited among seven different communities of Shanghai from 2011 to 2012, and their information regarding self-reported PE, self-estimated IELT, expert diagnosis of PE, and PEDT scores were collected. Validity of the PEDT and its association with clinical expert diagnosis of PE and self-estimated IELT were analyzed. A total of 143 patients without PE (mean age 55.11 ± 7.65 years) and 100 men with PE (mean age 53.07 ± 8.08 years) were enrolled for validation. Of the patients in PE group, the number of men reporting self-estimated IELTs of ≤1, 1-2, and >2 minutes were 34 (34.0%), 22 (22.0%), and 44 (44.0%), respectively. The Cronbach's alpha score (α = 0.77) showed adequate internal consistency, and the test-retest correlation coefficients of each item (r ≥ 0.70, P < 0.001) indicated excellent stability over time. The frequency of agreement showed that there was excellent concordance between PEDT diagnosis and clinician diagnosis when the PEDT scores ≥11. An adequate correlation was found between total PEDT score and self-estimated IELT (ρ = -0.396, P < 0.001), and sensitivity and specificity analyses suggested a score of ≤8 indicated no time-defined PE (self-estimated IELT ≤1 minute). The Chinese version of PEDT is valid in screening the presence of PE among Chinese men. The PEDT showed an adequate negative correlation with self-estimated IELT and an excellent concordance with clinician diagnosis of PE. © 2014 International Society for Sexual Medicine.

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.

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

PubMed

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

2015-01-01

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

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

PubMed Central

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

2013-01-01

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

Psychometric Testing of the Self-Efficacy for Interdisciplinary Plans of Care Scale.

PubMed

Molle, Elizabeth; Froman, Robin

2017-01-01

Computerized interdisciplinary plans of care have revitalized nurse-centric care plans into dynamic and meaningful electronic documents. To maximize the benefits of these documents, it is important to understand healthcare professionals' attitudes, specifically their confidence, for making computerized interdisciplinary care plans useful and meaningful documents. The purpose of the study was to test the psychometric properties of the Self-Efficacy for Interdisciplinary Plans of Care instrument intended to measure healthcare professionals' self-efficacy for using such documents. Content validity was assessed by an expert review panel. Content validity indices ranged from 0.75 to 1.00, with a scale CVI of 0.94. A sample of 389 healthcare providers completed the 14-item instrument. Principal axis factoring was used to assess factor structure. The exploratory factor analysis yielded a single-factor structure accounting for 71.76% of covariance. Cronbach internal consistency coefficient for the single factor solution was .97. The corrected item-total correlations ranged from 0.71 to 0.90. The coefficient of stability, during a 2-week period, with a subset of the sample (n = 38), was estimated at 0.82. The results of this study suggest that the Self-Efficacy for Interdisciplinary Plans of Care has sturdy reliability and validity for measuring the self-efficacy of healthcare providers to make computerized interdisciplinary plans of care meaningful and useful documents.

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.

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.

Data-driven modeling of sleep EEG and EOG reveals characteristics indicative of pre-Parkinson's and Parkinson's disease.

PubMed

Christensen, Julie A E; Zoetmulder, Marielle; Koch, Henriette; Frandsen, Rune; Arvastson, Lars; Christensen, Søren R; Jennum, Poul; Sorensen, Helge B D

2014-09-30

Manual scoring of sleep relies on identifying certain characteristics in polysomnograph (PSG) signals. However, these characteristics are disrupted in patients with neurodegenerative diseases. This study evaluates sleep using a topic modeling and unsupervised learning approach to identify sleep topics directly from electroencephalography (EEG) and electrooculography (EOG). PSG data from control subjects were used to develop an EOG and an EEG topic model. The models were applied to PSG data from 23 control subjects, 25 patients with periodic leg movements (PLMs), 31 patients with idiopathic REM sleep behavior disorder (iRBD) and 36 patients with Parkinson's disease (PD). The data were divided into training and validation datasets and features reflecting EEG and EOG characteristics based on topics were computed. The most discriminative feature subset for separating iRBD/PD and PLM/controls was estimated using a Lasso-regularized regression model. The features with highest discriminability were the number and stability of EEG topics linked to REM and N3, respectively. Validation of the model indicated a sensitivity of 91.4% and a specificity of 68.8% when classifying iRBD/PD patients. The topics showed visual accordance with the manually scored sleep stages, and the features revealed sleep characteristics containing information indicative of neurodegeneration. This study suggests that the amount of N3 and the ability to maintain NREM and REM sleep have potential as early PD biomarkers. Data-driven analysis of sleep may contribute to the evaluation of neurodegenerative patients. Copyright © 2014 Elsevier B.V. All rights reserved.

Clarifying the Behavioral Economics of Social Anxiety Disorder: Effects of Interpersonal Problems and Symptom Severity on Generosity.

PubMed

Rodebaugh, Thomas L; Heimberg, Richard G; Taylor, Kristin P; Lenze, Eric J

2016-01-01

Social anxiety disorder is associated with lower interpersonal warmth, possibly explaining its associated interpersonal impairment. Across two samples, we attempted to replicate previous findings that the disorder's constraint of interpersonal warmth can be detected via behavioral economic tasks. We also tested the test-retest stability of task indices. Results indicated that factors associated with social anxiety disorder (and not the disorder itself), such as the severity of social anxiety and more extreme interpersonal problems, lead to less generous behavior on the economic task examined. Results were clearest regarding fine-grained indices derived from latent trajectories. Unexpectedly, the combination of generalized anxiety disorder and higher depression also restricted generosity. Two of three indices showed acceptable test-retest stability. Maladaptive giving behavior may be a treatment target to improve interpersonal functioning in psychiatric disorders; therefore, future work should more precisely characterize behavioral economic tasks, including basic psychometric work (i.e., tests of reliability and validity).

Clarifying the Behavioral Economics of Social Anxiety Disorder: Effects of Interpersonal Problems and Symptom Severity on Generosity

PubMed Central

Rodebaugh, Thomas L.; Heimberg, Richard G.; Taylor, Kristin P.; Lenze, Eric J.

2015-01-01

Social anxiety disorder is associated with lower interpersonal warmth, possibly explaining its associated interpersonal impairment. Across two samples, we attempted to replicate previous findings that the disorder’s constraint of interpersonal warmth can be detected via behavioral economic tasks. We also tested the test-retest stability of task indices. Results indicated that factors associated with social anxiety disorder (and not the disorder itself), such as the severity of social anxiety and more extreme interpersonal problems, lead to less generous behavior on the economic task examined. Results were clearest regarding fine-grained indices derived from latent trajectories. Unexpectedly, the combination of generalized anxiety disorder and higher depression also restricted generosity. Two of three indices showed acceptable test-retest stability. Maladaptive giving behavior may be a treatment target to improve interpersonal functioning in psychiatric disorders; therefore, future work should more precisely characterize behavioral economic tasks, including basic psychometric work (i.e., tests of reliability and validity). PMID:27034911

A multicenter prospective cohort study on camera navigation training for key user groups in minimally invasive surgery.

PubMed

Graafland, Maurits; Bok, Kiki; Schreuder, Henk W R; Schijven, Marlies P

2014-06-01

Untrained laparoscopic camera assistants in minimally invasive surgery (MIS) may cause suboptimal view of the operating field, thereby increasing risk for errors. Camera navigation is often performed by the least experienced member of the operating team, such as inexperienced surgical residents, operating room nurses, and medical students. The operating room nurses and medical students are currently not included as key user groups in structured laparoscopic training programs. A new virtual reality laparoscopic camera navigation (LCN) module was specifically developed for these key user groups. This multicenter prospective cohort study assesses face validity and construct validity of the LCN module on the Simendo virtual reality simulator. Face validity was assessed through a questionnaire on resemblance to reality and perceived usability of the instrument among experts and trainees. Construct validity was assessed by comparing scores of groups with different levels of experience on outcome parameters of speed and movement proficiency. The results obtained show uniform and positive evaluation of the LCN module among expert users and trainees, signifying face validity. Experts and intermediate experience groups performed significantly better in task time and camera stability during three repetitions, compared to the less experienced user groups (P < .007). Comparison of learning curves showed significant improvement of proficiency in time and camera stability for all groups during three repetitions (P < .007). The results of this study show face validity and construct validity of the LCN module. The module is suitable for use in training curricula for operating room nurses and novice surgical trainees, aimed at improving team performance in minimally invasive surgery. © The Author(s) 2013.

Frequency Discrimination Deficits in People with Specific Language Impairment: Reliability, Validity, and Linguistic Correlates

ERIC Educational Resources Information Center

McArthur, G. M.; Bishop, D. V. M.

2004-01-01

The reliability and validity of a frequency discrimination (FD) task were tested in 16 people with specific language impairment (SLI) and 16 people with normal spoken language (controls). The FD thresholds of the 2 groups indicated that FD thresholds for 25-ms and 250-ms tones were remarkably stable across 18 months. The FD thresholds were lower…

On the manifestation of coexisting nontrivial equilibria leading to potential well escapes in an inhomogeneous floating body

NASA Astrophysics Data System (ADS)

Sequeira, Dane; Wang, Xue-She; Mann, B. P.

2018-02-01

This paper examines the bifurcation and stability behavior of inhomogeneous floating bodies, specifically a rectangular prism with asymmetric mass distribution. A nonlinear model is developed to determine the stability of the upright and tilted equilibrium positions as a function of the vertical position of the center of mass within the prism. These equilibria positions are defined by an angle of rotation and a vertical position where rotational motion is restricted to a two dimensional plane. Numerical investigations are conducted using path-following continuation methods to determine equilibria solutions and evaluate stability. Bifurcation diagrams and basins of attraction that illustrate the stability of the equilibrium positions as a function of the vertical position of the center of mass within the prism are generated. These results reveal complex stability behavior with many coexisting solutions. Static experiments are conducted to validate equilibria orientations against numerical predictions with results showing good agreement. Dynamic experiments that examine potential well hopping behavior in a waveflume for various wave conditions are also conducted.

Test system stability and natural variability of a Lemna gibba L. bioassay.

PubMed

Scherr, Claudia; Simon, Meinhard; Spranger, Jörg; Baumgartner, Stephan

2008-09-04

In ecotoxicological and environmental studies Lemna spp. are used as test organisms due to their small size, rapid predominantly vegetative reproduction, easy handling and high sensitivity to various chemicals. However, there is not much information available concerning spatial and temporal stability of experimental set-ups used for Lemna bioassays, though this is essential for interpretation and reliability of results. We therefore investigated stability and natural variability of a Lemna gibba bioassay assessing area-related and frond number-related growth rates under controlled laboratory conditions over about one year. Lemna gibba L. was grown in beakers with Steinberg medium for one week. Area-related and frond number-related growth rates (r(area) and r(num)) were determined with a non-destructive image processing system. To assess inter-experimental stability, 35 independent experiments were performed with 10 beakers each in the course of one year. We observed changes in growth rates by a factor of two over time. These did not correlate well with temperature or relative humidity in the growth chamber. In order to assess intra-experimental stability, we analysed six systematic negative control experiments (nontoxicant tests) with 96 replicate beakers each. Evaluation showed that the chosen experimental set-up was stable and did not produce false positive results. The coefficient of variation was lower for r(area) (2.99%) than for r(num) (4.27%). It is hypothesised that the variations in growth rates over time under controlled conditions are partly due to endogenic periodicities in Lemna gibba. The relevance of these variations for toxicity investigations should be investigated more closely. Area-related growth rate seems to be more precise as non-destructive calculation parameter than number-related growth rate. Furthermore, we propose two new validity criteria for Lemna gibba bioassays: variability of average specific and section-by-section segmented growth rate, complementary to average specific growth rate as the only validity criterion existing in guidelines for duckweed bioassays.

Test System Stability and Natural Variability of a Lemna Gibba L. Bioassay

PubMed Central

Scherr, Claudia; Simon, Meinhard; Spranger, Jörg; Baumgartner, Stephan

2008-01-01

Background In ecotoxicological and environmental studies Lemna spp. are used as test organisms due to their small size, rapid predominantly vegetative reproduction, easy handling and high sensitivity to various chemicals. However, there is not much information available concerning spatial and temporal stability of experimental set-ups used for Lemna bioassays, though this is essential for interpretation and reliability of results. We therefore investigated stability and natural variability of a Lemna gibba bioassay assessing area-related and frond number-related growth rates under controlled laboratory conditions over about one year. Methology/Principal Findings Lemna gibba L. was grown in beakers with Steinberg medium for one week. Area-related and frond number-related growth rates (r(area) and r(num)) were determined with a non-destructive image processing system. To assess inter-experimental stability, 35 independent experiments were performed with 10 beakers each in the course of one year. We observed changes in growth rates by a factor of two over time. These did not correlate well with temperature or relative humidity in the growth chamber. In order to assess intra-experimental stability, we analysed six systematic negative control experiments (nontoxicant tests) with 96 replicate beakers each. Evaluation showed that the chosen experimental set-up was stable and did not produce false positive results. The coefficient of variation was lower for r(area) (2.99%) than for r(num) (4.27%). Conclusions/Significance It is hypothesised that the variations in growth rates over time under controlled conditions are partly due to endogenic periodicities in Lemna gibba. The relevance of these variations for toxicity investigations should be investigated more closely. Area-related growth rate seems to be more precise as non-destructive calculation parameter than number-related growth rate. Furthermore, we propose two new validity criteria for Lemna gibba bioassays: variability of average specific and section-by-section segmented growth rate, complementary to average specific growth rate as the only validity criterion existing in guidelines for duckweed bioassays. PMID:18769541

Multiple Imputation based Clustering Validation (MIV) for Big Longitudinal Trial Data with Missing Values in eHealth.

PubMed

Zhang, Zhaoyang; Fang, Hua; Wang, Honggang

2016-06-01

Web-delivered trials are an important component in eHealth services. These trials, mostly behavior-based, generate big heterogeneous data that are longitudinal, high dimensional with missing values. Unsupervised learning methods have been widely applied in this area, however, validating the optimal number of clusters has been challenging. Built upon our multiple imputation (MI) based fuzzy clustering, MIfuzzy, we proposed a new multiple imputation based validation (MIV) framework and corresponding MIV algorithms for clustering big longitudinal eHealth data with missing values, more generally for fuzzy-logic based clustering methods. Specifically, we detect the optimal number of clusters by auto-searching and -synthesizing a suite of MI-based validation methods and indices, including conventional (bootstrap or cross-validation based) and emerging (modularity-based) validation indices for general clustering methods as well as the specific one (Xie and Beni) for fuzzy clustering. The MIV performance was demonstrated on a big longitudinal dataset from a real web-delivered trial and using simulation. The results indicate MI-based Xie and Beni index for fuzzy-clustering are more appropriate for detecting the optimal number of clusters for such complex data. The MIV concept and algorithms could be easily adapted to different types of clustering that could process big incomplete longitudinal trial data in eHealth services.

Multiple Imputation based Clustering Validation (MIV) for Big Longitudinal Trial Data with Missing Values in eHealth

PubMed Central

Zhang, Zhaoyang; Wang, Honggang

2016-01-01

Web-delivered trials are an important component in eHealth services. These trials, mostly behavior-based, generate big heterogeneous data that are longitudinal, high dimensional with missing values. Unsupervised learning methods have been widely applied in this area, however, validating the optimal number of clusters has been challenging. Built upon our multiple imputation (MI) based fuzzy clustering, MIfuzzy, we proposed a new multiple imputation based validation (MIV) framework and corresponding MIV algorithms for clustering big longitudinal eHealth data with missing values, more generally for fuzzy-logic based clustering methods. Specifically, we detect the optimal number of clusters by auto-searching and -synthesizing a suite of MI-based validation methods and indices, including conventional (bootstrap or cross-validation based) and emerging (modularity-based) validation indices for general clustering methods as well as the specific one (Xie and Beni) for fuzzy clustering. The MIV performance was demonstrated on a big longitudinal dataset from a real web-delivered trial and using simulation. The results indicate MI-based Xie and Beni index for fuzzy-clustering is more appropriate for detecting the optimal number of clusters for such complex data. The MIV concept and algorithms could be easily adapted to different types of clustering that could process big incomplete longitudinal trial data in eHealth services. PMID:27126063

Tests for the Assessment of Sport-Specific Performance in Olympic Combat Sports: A Systematic Review With Practical Recommendations

PubMed Central

Chaabene, Helmi; Negra, Yassine; Bouguezzi, Raja; Capranica, Laura; Franchini, Emerson; Prieske, Olaf; Hbacha, Hamdi; Granacher, Urs

2018-01-01

The regular monitoring of physical fitness and sport-specific performance is important in elite sports to increase the likelihood of success in competition. This study aimed to systematically review and to critically appraise the methodological quality, validation data, and feasibility of the sport-specific performance assessment in Olympic combat sports like amateur boxing, fencing, judo, karate, taekwondo, and wrestling. A systematic search was conducted in the electronic databases PubMed, Google-Scholar, and Science-Direct up to October 2017. Studies in combat sports were included that reported validation data (e.g., reliability, validity, sensitivity) of sport-specific tests. Overall, 39 studies were eligible for inclusion in this review. The majority of studies (74%) contained sample sizes <30 subjects. Nearly, 1/3 of the reviewed studies lacked a sufficient description (e.g., anthropometrics, age, expertise level) of the included participants. Seventy-two percent of studies did not sufficiently report inclusion/exclusion criteria of their participants. In 62% of the included studies, the description and/or inclusion of a familiarization session (s) was either incomplete or not existent. Sixty-percent of studies did not report any details about the stability of testing conditions. Approximately half of the studies examined reliability measures of the included sport-specific tests (intraclass correlation coefficient [ICC] = 0.43–1.00). Content validity was addressed in all included studies, criterion validity (only the concurrent aspect of it) in approximately half of the studies with correlation coefficients ranging from r = −0.41 to 0.90. Construct validity was reported in 31% of the included studies and predictive validity in only one. Test sensitivity was addressed in 13% of the included studies. The majority of studies (64%) ignored and/or provided incomplete information on test feasibility and methodological limitations of the sport-specific test. In 28% of the included studies, insufficient information or a complete lack of information was provided in the respective field of the test application. Several methodological gaps exist in studies that used sport-specific performance tests in Olympic combat sports. Additional research should adopt more rigorous validation procedures in the application and description of sport-specific performance tests in Olympic combat sports. PMID:29692739

Impact of syncope on quality of life: validation of a measure in patients undergoing tilt testing.

PubMed

Nave-Leal, Elisabete; Oliveira, Mário; Pais-Ribeiro, José; Santos, Sofia; Oliveira, Eunice; Alves, Teresa; Cruz Ferreira, Rui

2015-03-01

Recurrent syncope has a significant impact on quality of life. The development of measurement scales to assess this impact that are easy to use in clinical settings is crucial. The objective of the present study is a preliminary validation of the Impact of Syncope on Quality of Life questionnaire for the Portuguese population. The instrument underwent a process of translation, validation, analysis of cultural appropriateness and cognitive debriefing. A population of 39 patients with a history of recurrent syncope (>1 year) who underwent tilt testing, aged 52.1 ± 16.4 years (21-83), 43.5% male, most in active employment (n=18) or retired (n=13), constituted a convenience sample. The resulting Portuguese version is similar to the original, with 12 items in a single aggregate score, and underwent statistical validation, with assessment of reliability, validity and stability over time. With regard to reliability, the internal consistency of the scale is 0.9. Assessment of convergent and discriminant validity showed statistically significant results (p<0.01). Regarding stability over time, a test-retest of this instrument at six months after tilt testing with 22 patients of the sample who had not undergone any clinical intervention found no statistically significant changes in quality of life. The results indicate that this instrument is of value for assessing quality of life in patients with recurrent syncope in Portugal. Copyright © 2014 Sociedade Portuguesa de Cardiologia. Published by Elsevier España. All rights reserved.

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.

New Stability-Indicating RP-HPLC Method for Determination of Diclofenac Potassium and Metaxalone from their Combined Dosage Form

PubMed Central

Panda, Sagar Suman; Patanaik, Debasis; Ravi Kumar, Bera V. V.

2012-01-01

A simple, precise and accurate isocratic RP-HPLC stability-indicating assay method has been developed to determine diclofenac potassium and metaxalone in their combined dosage forms. Isocratic separation was achieved on a Hibar-C18, Lichrosphere-100® (250 mm × 4.6 mm i.d., particle size 5 μm) column at room temperature in isocratic mode, the mobile phase consists of methanol: water (80:20, v/v) at a flow rate of 1.0 ml/min, the injection volume was 20 μl and UV detection was carried out at 280nm. The drug was subjected to acid and alkali hydrolysis, oxidation, photolysis and heat as stress conditions. The method was validated for specificity, linearity, precision, accuracy, robustness and system suitability. The method was linear in the drug concentration range of 2.5–30 μg/ml and 20–240 μg/ml for diclofenac potassium and metaxalone, respectively. The precision (RSD) of six samples was 0.83 and 0.93% for repeatability, and the intermediate precision (RSD) among six-sample preparation was 1.63 and 0.49% for diclofenac potassium and metaxalone, respectively. The mean recoveries were between 100.99–102.58% and 99.97–100.01% for diclofenac potassium and metaxalone, respectively. The proposed method can be used successfully for routine analysis of the drug in bulk and combined pharmaceutical dosage forms. PMID:22396909

Jacobi Shape Transitions Within the LSD Model and the Skyrme-Etf Approach

NASA Astrophysics Data System (ADS)

Bartel, Johann; Pomorski, Krzysztof

The "Modified Funny-Hills parametrisation" is used together with the Lublin-Strasbourg Drop Model to evaluate the stability of rotating nuclei. The Jacobi transition into triaxial shapes is studied. By a comparison with selfconsistent semiclassical calculations in the framework of the Extended Thomas-Fermi method, the validity of the present approach is demonstrated and possible improvements are indicated.

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.

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

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.

Trends in Thermostability Provide Information on the Nature of Substrate, Inhibitor, and Lipid Interactions with Mitochondrial Carriers*

PubMed Central

Crichton, Paul G.; Lee, Yang; Ruprecht, Jonathan J.; Cerson, Elizabeth; Thangaratnarajah, Chancievan; King, Martin S.; Kunji, Edmund R. S.

2015-01-01

Mitochondrial carriers, including uncoupling proteins, are unstable in detergents, which hampers structural and mechanistic studies. To investigate carrier stability, we have purified ligand-free carriers and assessed their stability with a fluorescence-based thermostability assay that monitors protein unfolding with a thiol-reactive dye. We find that mitochondrial carriers from both mesophilic and thermophilic organisms exhibit poor stability in mild detergents, indicating that instability is inherent to the protein family. Trends in the thermostability of yeast ADP/ATP carrier AAC2 and ovine uncoupling protein UCP1 allow optimal conditions for stability in detergents to be established but also provide mechanistic insights into the interactions of lipids, substrates, and inhibitors with these proteins. Both proteins exhibit similar stability profiles across various detergents, where stability increases with the size of the associated detergent micelle. Detailed analysis shows that lipids stabilize carriers indirectly by increasing the associated detergent micelle size, but cardiolipin stabilizes by direct interactions as well. Cardiolipin reverses destabilizing effects of ADP and bongkrekic acid on AAC2 and enhances large stabilizing effects of carboxyatractyloside, revealing that this lipid interacts in the m-state and possibly other states of the transport cycle, despite being in a dynamic interface. Fatty acid activators destabilize UCP1 in a similar way, which can also be prevented by cardiolipin, indicating that they interact like transport substrates. Our controls show that carriers can be soluble but unfolded in some commonly used detergents, such as the zwitterionic Fos-choline-12, which emphasizes the need for simple validation assays like the one used here. PMID:25653283

Psychometric validation of the PROQOL-HIV questionnaire, a new health-related quality of life instrument-specific to HIV disease.

PubMed

Duracinsky, Martin; Lalanne, Christophe; Le Coeur, Sophie; Herrmann, Susan; Berzins, Baiba; Armstrong, Andrew Richard; Lau, Joseph Tak Fai; Fournier, Isabelle; Chassany, Olivier

2012-04-15

This study reports the psychometric validation of a new HIV/AIDS-specific health-related quality of life (HRQL) questionnaire, the Patient Reported Outcomes Quality of Life-HIV. The instrument was developed simultaneously across Europe, North and South America, Africa, Asia, and Australia to assess multidimensional quality of life impairments in the era of highly active antiretroviral therapy. A cross-sectional study was performed in 8 countries. The pilot 70-item questionnaire was co-administered with the HIV symptoms index, the EQ-5D and Medical Outcomes Study-HIV questionnaires. Demographic and biomedical data were collected. After item analysis and reduction, convergent discriminant concurrent validity and known-group validity were examined. Internal consistency and reliability scores were assessed using Cronbach alpha and intraclass correlation. The final sample of 791 patients was composed of 64% males (median age: 41 years, HIV diagnosis = 5 years), 13.8% were treatment naive. Item reduction yielded a 43-item form surveying 8 dimensions and 1 global health item that showed good convergent and discriminant validity and reliability (98% scaling success; Cronbach alphas 0.77-0.89). Correlations with EQ-5D and Medical Outcomes Study-HIV complied with concurrent validity expectations; likewise, correlations against the number of self-reported symptoms and depression showed good support for criterion validity. A test-retest study on French patients (n = 34) showed temporal stability (intraclass correlation coefficient = 0.86). Significant and meaningful differences of HRQL scores between countries were found. The Patient Reported Outcomes Quality of Life-HIV questionnaire is a valid and reliable instrument for assessing HRQL specific to HIV disease in different cultures and healthcare systems.

Integrated Technology Rotor Methodology Assessment Workshop

NASA Technical Reports Server (NTRS)

Mcnulty, Michael J. (Editor); Bousman, William G. (Editor)

1988-01-01

The conference proceedings contains 14 formal papers and the results of two panel discussions. In addition, a transcript of discussion that followed the paper presentations and panels is included. The papers are of two kinds. The first seven papers were directed specifically to the correlation of industry and government mathematical models with data for rotorcraft stability from six experiments. The remaining 7 papers dealt with related topics in the prediction of rotor aeroelastic or aeromechanical stability. The first of the panels provided an evaluation of the correlation that was shown between the mathematical models and the experimental data. The second panel addressed the general problems of the validation of mathematical models.

A spectrally accurate boundary-layer code for infinite swept wings

NASA Technical Reports Server (NTRS)

Pruett, C. David

1994-01-01

This report documents the development, validation, and application of a spectrally accurate boundary-layer code, WINGBL2, which has been designed specifically for use in stability analyses of swept-wing configurations. Currently, we consider only the quasi-three-dimensional case of an infinitely long wing of constant cross section. The effects of streamwise curvature, streamwise pressure gradient, and wall suction and/or blowing are taken into account in the governing equations and boundary conditions. The boundary-layer equations are formulated both for the attachment-line flow and for the evolving boundary layer. The boundary-layer equations are solved by marching in the direction perpendicular to the leading edge, for which high-order (up to fifth) backward differencing techniques are used. In the wall-normal direction, a spectral collocation method, based upon Chebyshev polynomial approximations, is exploited. The accuracy, efficiency, and user-friendliness of WINGBL2 make it well suited for applications to linear stability theory, parabolized stability equation methodology, direct numerical simulation, and large-eddy simulation. The method is validated against existing schemes for three test cases, including incompressible swept Hiemenz flow and Mach 2.4 flow over an airfoil swept at 70 deg to the free stream.

A new, rapid, stability-indicating UPLC method for separation and determination of impurities in amlodipine besylate, valsartan and hydrochlorothiazide in their combined tablet dosage form.

PubMed

Vojta, Jiří; Jedlička, Aleš; Coufal, Pavel; Janečková, Lucie

2015-05-10

A new rapid stability-indicating UPLC method for separation and determination of impurities in amlodipine besylate, valsartan and hydrochlorothiazide in their combined tablet dosage form was developed. The separation of Ph. Eur. related substances of amlodipine besylate (A, B, D, E, F, G), hydrochlorothiazide (A, B, C), valsartan (B, C), two other valsartan impurities (S)-2-(N-{[2'-cyanobiphenyl-4-yl]methyl}pentanamido)-3-methylbutanoic acid and (S)-3-methyl-2-{[2'-(1H-tetrazol-5-yl)biphenyl-4-yl]methylamino}butanoic acid and several unknown impurities was achieved by reversed phase liquid chromatography with UV detection. The detection wavelengths were set as follows: 225nm for valsartan, its impurities and for the impurity D of amlodipine, 271nm for hydrochlorothiazide and its impurities and 360nm for amlodipine and its impurities except for impurity D. Zorbax Eclipse C8 RRHD (100mm×3.0mm, 1.8μm) was used as a separation column and the analytes were eluted within 11min by a programmed gradient mixture of 0.01M phosphate buffer pH 2.5 and acetonitrile. The method was successfully validated in accordance to the International Conference of Harmonization (ICH) guidelines for amlodipine besylate and its impurity D, valsartan and its impurity C and hydrochlorothiazide and its impurities A, B and C. The triple-combined tablets were exposed to thermal, higher humidity, acid, alkaline, oxidative and photolytic stress conditions. Stressed samples were analyzed by the proposed method. All the significant degradation products and impurities were satisfactory separated from each other and from the principal peaks of drug substances. The peak purity test complied for peaks of amlodipine, valsartan and hydrochlorothiazide in all the stressed samples and indicated no co-elution of degradation products. The method was found to be precise, linear, accurate, sensitive, specific, robust and stability-indicating and could be used as a routine purity test method for amlodipine besylate, valsartan, hydrochlorothiazide and their pharmaceutical combinations. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed

Chen, Calvin Yu-Chian

2013-01-01

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

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

PubMed

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

2010-11-01

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

Assessing cognitive insight in nonpsychiatric individuals and outpatients with schizophrenia in Taiwan: an investigation using the Beck Cognitive Insight Scale

PubMed Central

2011-01-01

Background The Beck Cognitive Insight Scale (BCIS) was designed for the assessment of the cognitive processes involved in self-reflection and the ability to modify erroneous beliefs and misinterpretations. Studies investigating the factor structure of the BCIS have indicated a two-factor model in the psychotic population. The factor structure of the BCIS, however, has not received much consideration in the nonpsychiatric population. The present study examined the factor structure and validity of the BCIS and compared its scores between nonpsychiatric individuals and outpatients with psychosis. Method The Taiwanese version of the BCIS was administered to 507 nonpsychiatric individuals and 118 outpatients with schizophrenia. The psychometric properties of the BCIS were examined through the following analyses: exploratory and confirmatory factor analyses, reliability, correlation analyses, and discriminative validity. Results The BCIS showed adequate internal consistency and stability over time. Exploratory and confirmatory factor analyses on the 15-item measure indicated a two-factor solution that supported the two dimensions of the Taiwanese BCIS, which was also observed with the original BCIS. Following the construct validation, we obtained a composite index (self-reflectiveness minus self-certainty) of the Taiwanese BCIS that reflected cognitive insight. Consistent with previous studies, our results indicated that psychosis is associated with low self-reflectiveness and high self-certainty, which possibly reflect lower cognitive insight. Our results also showed that better cognitive insight is related to worse depression in patients with schizophrenia spectrum disorders, but not in nonpsychiatric individuals. The receiver operating characteristic (ROC) analyses revealed that the area under the curve (AUC) was 0.731. A composite index of 3 was a good limit, with a sensitivity of 87% and a specificity of 51%. Conclusion The BCIS proved to be useful for measuring cognitive insight in Taiwanese nonpsychiatric and psychotic populations. PMID:22018413

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.

NIKE: a new clinical tool for establishing levels of indications for cataract surgery.

PubMed

Lundström, Mats; Albrecht, Susanne; Håkansson, Ingemar; Lorefors, Ragnhild; Ohlsson, Sven; Polland, Werner; Schmid, Andrea; Svensson, Göran; Wendel, Eva

2006-08-01

The purpose of this study was to construct a new clinical tool for establishing levels of indications for cataract surgery, and to validate this tool. Teams from nine eye clinics reached an agreement about the need to develop a clinical tool for setting levels of indications for cataract surgery and about the items that should be included in the tool. The tool was to be called 'NIKE' (Nationell Indikationsmodell för Kataraktextraktion). The Canadian Cataract Priority Criteria Tool served as a model for the NIKE tool, which was modified for Swedish conditions. Items included in the tool were visual acuity of both eyes, patients' perceived difficulties in day-to-day life, cataract symptoms, the ability to live independently, and medical/ophthalmic reasons for surgery. The tool was validated and tested in 343 cataract surgery patients. Validity, stability and reliability were tested and the outcome of surgery was studied in relation to the indication setting. Four indication groups (IGs) were suggested. The group with the greatest indications for surgery was named group 1 and that with the lowest, group 4. Validity was proved to be good. Surgery had the greatest impact on the group with the highest indications for surgery. Test-retest reliability test and interexaminer tests of indication settings showed statistically significant intraclass correlations (intraclass correlation coefficients [ICCs] 0.526 and 0.923, respectively). A new clinical tool for indication setting in cataract surgery is presented. This tool, the NIKE, takes into account both visual acuity and the patient's perceived problems in day-to-day life because of cataract. The tool seems to be stable and reliable and neutral towards different examiners.

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

PubMed Central

Abdel-Khalek, Ahmed M.; Lester, David

2017-01-01

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

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

PubMed

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

2017-01-01

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

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

PubMed

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

2016-07-01

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

Development and evaluation of the EOL-ICDQ as a measure of experiences, attitudes and knowledge in end-of-life in patients living with an implantable cardioverter defibrillator.

PubMed

Thylén, Ingela; Wenemark, Marika; Fluur, Christina; Strömberg, Anna; Bolse, Kärstin; Årestedt, Kristofer

2014-04-01

Due to extended indications and resynchronization therapy, many implantable cardioverter defibrillator (ICD) recipients will experience progressive co-morbid conditions and will be more likely to die of causes other than cardiac death. It is therefore important to elucidate the ICD patients' preferences when nearing end-of-life. Instead of avoiding the subject of end-of-life, a validated questionnaire may be helpful to explore patients' experiences and attitudes about end-of-life concerns and to assess knowledge of the function of the ICD in end-of-life. Validated instruments assessing patients' perspective concerning end-of-life issues are scarce. The purpose of this study was to develop and evaluate respondent satisfaction and measurement properties of the 'Experiences, Attitudes and Knowledge of End-of-Life Issues in Implantable Cardioverter Defibrillator Patients' Questionnaire' (EOL-ICDQ). The instrument was tested for validity, respondent satisfaction, and for homogeneity and stability in the Swedish language. An English version of the EOL-ICDQ was validated, but has not yet been pilot tested. The final instrument contained three domains, which were clustered into 39 items measuring: experiences (10 items), attitudes (18 items), and knowledge (11 items) of end-of-life concerns in ICD patients. In addition, the questionnaire also contained items on socio-demographic background (six items) and ICD-specific background (eight items). The validity and reliability properties were considered sufficient. The EOL-ICDQ has the potential to be used in clinical practice and future research. Further studies are needed using this instrument in an Anglo-Saxon context with a sample of English-speaking ICD recipients.

Validity of questions about activities of daily living to screen for dependency in older adults

PubMed Central

Rebouças, Monica; Coelho-Filho, João Macedo; Veras, Renato Peixoto; Lima-Costa, Maria Fernanda; Ramos, Luiz Roberto

2017-01-01

ABSTRACT OBJECTIVE To determine the criterion validity of the activities of daily living present in functionality questionnaires in older adults for population surveys and to identify which activities are valid to quantify the real daily need for help of this population. METHODS This is a population sample of older adults stratified by levels of functionality, according to self-perception of dependency in the activities of daily living. Self-perception was compared with the gold standard – direct observation of these activities in the household of older adults by a trained professional, blinded to the answers in the questionnaire. At the visit, it was decided if the older adult needed help to perform any of the activities of daily living for the research. The sensitivity of each activity of daily living was greater when the self-assessment that there was no need for help coincided with the assessment of the professional. Specificity indicates coincidence regarding the need for help in the activities of daily living – coefficients of sensitivity and specificity above 70% were considered as indicative of good validity. RESULTS Self-assessments showed better sensitivity than specificity – older adults and observers agreed more on daily independency than on dependency. All activities showed sensitivity above 70%. Some activities had low (go shopping: 55%) or very low specificity (brush the hair: 33%). The best specificities were to take a shower and dress up (95.8% for both), among the personal ones, and to use transportation and perform banking transactions (78% for both), among the instrumental ones. CONCLUSIONS Activities of daily living can be valid indicators of functional dependence. The best coefficients of validity were generally obtained for personal activities. Some activities with good sensitivities and specificities – walk 100 meters, take a shower, and lie down in and get out of the bed – can be used to classify older adults into low, average, and high need for help depending on the affected activities and, therefore, can help in the planning of health services aimed at them. PMID:28876414

Validity of self-assessment in a quality improvement collaborative in Ecuador.

PubMed

Hermida, Jorge; Broughton, Edward I; Miller Franco, Lynne

2011-12-01

Health care quality improvement (QI) efforts commonly use self-assessment to measure compliance with quality standards. This study investigates the validity of self-assessment of quality indicators. Cross sectional. A maternal and newborn care improvement collaborative intervention conducted in health facilities in Ecuador in 2005. Four external evaluators were trained in abstracting medical records to calculate six indicators reflecting compliance with treatment standards. About 30 medical records per month were examined at 12 participating health facilities for a total of 1875 records. The same records had already been reviewed by QI teams at these facilities (self-assessment). Overall compliance, agreement (using the Kappa statistic), sensitivity and specificity were analyzed. We also examined patterns of disagreement and the effect of facility characteristics on levels of agreement. External evaluators reported compliance of 69-90%, while self-assessors reported 71-92%, with raw agreement of 71-95% and Kappa statistics ranging from fair to almost perfect agreement. Considering external evaluators as the gold standard, sensitivity of self-assessment ranged from 90 to 99% and specificity from 48 to 86%. Simpler indicators had fewer disagreements. When disagreements occurred between self-assessment and external valuators, the former tended to report more positive findings in five of six indicators, but this tendency was not of a magnitude to change program actions. Team leadership, understanding of the tools and facility size had no overall impact on the level of agreement. When compared with external evaluation (gold standard), self-assessment was found to be sufficiently valid for tracking QI team performance. Sensitivity was generally higher than specificity. Simplifying indicators may improve validity.

Structure-activity relationships between sterols and their thermal stability in oil matrix.

PubMed

Hu, Yinzhou; Xu, Junli; Huang, Weisu; Zhao, Yajing; Li, Maiquan; Wang, Mengmeng; Zheng, Lufei; Lu, Baiyi

2018-08-30

Structure-activity relationships between 20 sterols and their thermal stabilities were studied in a model oil system. All sterol degradations were found to be consistent with a first-order kinetic model with determination of coefficient (R 2 ) higher than 0.9444. The number of double bonds in the sterol structure was negatively correlated with the thermal stability of sterol, whereas the length of the branch chain was positively correlated with the thermal stability of sterol. A quantitative structure-activity relationship (QSAR) model to predict thermal stability of sterol was developed by using partial least squares regression (PLSR) combined with genetic algorithm (GA). A regression model was built with R 2 of 0.806. Almost all sterol degradation constants can be predicted accurately with R 2 of cross-validation equals to 0.680. Four important variables were selected in optimal QSAR model and the selected variables were observed to be related with information indices, RDF descriptors, and 3D-MoRSE descriptors. Copyright © 2018 Elsevier Ltd. All rights reserved.

Development and exploratory analysis of the Neurorehabilitation Program Styles Survey.

PubMed

McCorkel, Beth A; Glueckauf, Robert L; Ecklund-Johnson, Eric P; Tomusk, Allison B; Trexler, Lance E; Diller, Leonard

2003-01-01

To develop a survey instrument that assesses implementation of key components of outpatient neurorehabilitation programs and test the capacity of this instrument to differentiate between rehabilitation approaches. The Neurorehabilitation Program Styles Survey (NPSS) was administered to 18 outpatient facilities: 10 specialized and 8 discipline-specific outpatient neurorehabilitation programs. Scores were compared between types of programs using independent samples t tests. The NPSS showed good reliability and contrasted groups validity, significantly differentiating between types of programs. The NPSS holds considerable promise as a tool for distinguishing among different types of brain injury programs, and for assessing the differential effectiveness of specialized versus discipline-specific outpatient brain rehabilitation programs. Future research on the NPSS will assess the stability of the instrument over time, its content validity, and capacity to differentiate the full continuum of neurorehabilitation programs.

Introducing conjoint analysis method into delayed lotteries studies: its validity and time stability are higher than in adjusting

PubMed Central

Białek, Michał; Markiewicz, Łukasz; Sawicki, Przemysław

2015-01-01

The delayed lotteries are much more common in everyday life than are pure lotteries. Usually, we need to wait to find out the outcome of the risky decision (e.g., investing in a stock market, engaging in a relationship). However, most research has studied the time discounting and probability discounting in isolation using the methodologies designed specifically to track changes in one parameter. Most commonly used method is adjusting, but its reported validity and time stability in research on discounting are suboptimal. The goal of this study was to introduce the novel method for analyzing delayed lotteries—conjoint analysis—which hypothetically is more suitable for analyzing individual preferences in this area. A set of two studies compared the conjoint analysis with adjusting. The results suggest that individual parameters of discounting strength estimated with conjoint have higher predictive value (Study 1 and 2), and they are more stable over time (Study 2) compared to adjusting. We discuss these findings, despite the exploratory character of reported studies, by suggesting that future research on delayed lotteries should be cross-validated using both methods. PMID:25674069

42 CFR 424.515 - Requirements for reporting changes and updates to, and the periodic revalidation of Medicare...

Code of Federal Regulations, 2010 CFR

2010-10-01

... care fraud problems, national initiatives, complaints, or other reasons that cause CMS to question the... indicating noncompliance with the statute or regulations by specific provider or supplier types. The schedule... statute and regulations by specific provider or supplier types indicates that less frequent validation is...

42 CFR 424.515 - Requirements for reporting changes and updates to, and the periodic revalidation of Medicare...

Code of Federal Regulations, 2011 CFR

2011-10-01

... care fraud problems, national initiatives, complaints, or other reasons that cause CMS to question the... indicating noncompliance with the statute or regulations by specific provider or supplier types. The schedule... statute and regulations by specific provider or supplier types indicates that less frequent validation is...

A nomogram for predicting complications in patients with solid tumours and seemingly stable febrile neutropenia.

PubMed

Fonseca, Paula Jiménez; Carmona-Bayonas, Alberto; García, Ignacio Matos; Marcos, Rosana; Castañón, Eduardo; Antonio, Maite; Font, Carme; Biosca, Mercè; Blasco, Ana; Lozano, Rebeca; Ramchandani, Avinash; Beato, Carmen; de Castro, Eva Martínez; Espinosa, Javier; Martínez-García, Jerónimo; Ghanem, Ismael; Cubero, Jorge Hernando; Manrique, Isabel Aragón; Navalón, Francisco García; Sevillano, Elena; Manzano, Aránzazu; Virizuela, Juan; Garrido, Marcelo; Mondéjar, Rebeca; Arcusa, María Ángeles; Bonilla, Yaiza; Pérez, Quionia; Gallardo, Elena; Del Carmen Soriano, Maria; Cardona, Mercè; Lasheras, Fernando Sánchez; Cruz, Juan Jesús; Ayala, Francisco

2016-05-24

We sought to develop and externally validate a nomogram and web-based calculator to individually predict the development of serious complications in seemingly stable adult patients with solid tumours and episodes of febrile neutropenia (FN). The data from the FINITE study (n=1133) and University of Salamanca Hospital (USH) FN registry (n=296) were used to develop and validate this tool. The main eligibility criterion was the presence of apparent clinical stability, defined as events without acute organ dysfunction, abnormal vital signs, or major infections. Discriminatory ability was measured as the concordance index and stratification into risk groups. The rate of infection-related complications in the FINITE and USH series was 13.4% and 18.6%, respectively. The nomogram used the following covariates: Eastern Cooperative Group (ECOG) Performance Status ⩾2, chronic obstructive pulmonary disease, chronic cardiovascular disease, mucositis of grade ⩾2 (National Cancer Institute Common Toxicity Criteria), monocytes <200/mm(3), and stress-induced hyperglycaemia. The nomogram predictions appeared to be well calibrated in both data sets (Hosmer-Lemeshow test, P>0.1). The concordance index was 0.855 and 0.831 in each series. Risk group stratification revealed a significant distinction in the proportion of complications. With a ⩾116-point cutoff, the nomogram yielded the following prognostic indices in the USH registry validation series: 66% sensitivity, 83% specificity, 3.88 positive likelihood ratio, 48% positive predictive value, and 91% negative predictive value. We have developed and externally validated a nomogram and web calculator to predict serious complications that can potentially impact decision-making in patients with seemingly stable FN.

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

PubMed Central

Wasiak, Mathieu; Jouannet, Mireille; Sautou, Valérie

2018-01-01

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

Validation of the Weight Concerns Scale Applied to Brazilian University Students.

PubMed

Dias, Juliana Chioda Ribeiro; da Silva, Wanderson Roberto; Maroco, João; Campos, Juliana Alvares Duarte Bonini

2015-06-01

The aim of this study was to evaluate the validity and reliability of the Portuguese version of the Weight Concerns Scale (WCS) when applied to Brazilian university students. The scale was completed by 1084 university students from Brazilian public education institutions. A confirmatory factor analysis was conducted. The stability of the model in independent samples was assessed through multigroup analysis, and the invariance was estimated. Convergent, concurrent, divergent, and criterion validities as well as internal consistency were estimated. Results indicated that the one-factor model presented an adequate fit to the sample and values of convergent validity. The concurrent validity with the Body Shape Questionnaire and divergent validity with the Maslach Burnout Inventory for Students were adequate. Internal consistency was adequate, and the factorial structure was invariant in independent subsamples. The results present a simple and short instrument capable of precisely and accurately assessing concerns with weight among Brazilian university students. Copyright © 2015 Elsevier Ltd. All rights reserved.

Development and validation of the Cancer Exercise Stereotypes Scale.

PubMed

Falzon, Charlène; Sabiston, Catherine; Bergamaschi, Alessandro; Corrion, Karine; Chalabaev, Aïna; D'Arripe-Longueville, Fabienne

2014-01-01

The objective of this study was to develop and validate a French-language questionnaire measuring stereotypes related to exercise in cancer patients: The Cancer Exercise Stereotypes Scale (CESS). Four successive steps were carried out with 806 participants. First, a preliminary version was developed on the basis of the relevant literature and qualitative interviews. A test of clarity then led to the reformulation of six of the 30 items. Second, based on the modification indices of the first confirmatory factorial analysis, 11 of the 30 initial items were deleted. A new factorial structure analysis showed a good fit and validated a 19-item instrument with five subscales. Third, the stability of the instrument was tested over time. Last, tests of construct validity were conducted to examine convergent validity and discriminant validity. The French-language CESS appears to have good psychometric qualities and can be used to test theoretical tenets and inform intervention strategies on ways to foster exercise in cancer patients.

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

PubMed

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

2016-10-01

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

APPROACHES TO ASSESSING THE VALIDITY OF A FUNCTIONAL OBSERVATIONAL BATTERY

EPA Science Inventory

With the growing importance of neurobehavioral assessments at the preliminary stage of chemical testing, it is critical that the screening procedures utilized be valid indicators of neurobehavioral dysfunction in addition to being sensitive, specific, and reliable. fforts in this...

The MG Composite

PubMed Central

Burns, Ted M.; Conaway, Mark; Sanders, Donald B.

2010-01-01

Objective: To study the concurrent and construct validity and test-retest reliability in the practice setting of an outcome measure for myasthenia gravis (MG). Methods: Eleven centers participated in the validation study of the Myasthenia Gravis Composite (MGC) scale. Patients with MG were evaluated at 2 consecutive visits. Concurrent and construct validities of the MGC were assessed by evaluating MGC scores in the context of other MG-specific outcome measures. We used numerous potential indicators of clinical improvement to assess the sensitivity and specificity of the MGC for detecting clinical improvement. Test-retest reliability was performed on patients at the University of Virginia. Results: A total of 175 patients with MG were enrolled at 11 sites from July 1, 2008, to January 31, 2009. A total of 151 patients were seen in follow-up. Total MGC scores showed excellent concurrent validity with other MG-specific scales. Analyses of sensitivities and specificities of the MGC revealed that a 3-point improvement in total MGC score was optimal for signifying clinical improvement. A 3-point improvement in the MGC also appears to represent a meaningful improvement to most patients, as indicated by improved 15-item myasthenia gravis quality of life scale (MG-QOL15) scores. The psychometric properties were no better for an individualized subscore made up of the 2 functional domains that the patient identified as most important to treat. The test-retest reliability coefficient of the MGC was 98%, with a lower 95% confidence interval of 97%, indicating excellent test-retest reliability. Conclusions: The Myasthenia Gravis Composite is a reliable and valid instrument for measuring clinical status of patients with myasthenia gravis in the practice setting and in clinical trials. PMID:20439845

Binding mode analysis, dynamic simulation and binding free energy calculations of the MurF ligase from Acinetobacter baumannii.

PubMed

Ahmad, Sajjad; Raza, Saad; Uddin, Reaz; Azam, Syed Sikander

2017-10-01

MurF ligase catalyzes the final cytoplasmic step of bacterial peptidoglycan biosynthesis and, as such, is a validated target for therapeutic intervention. Herein, we performed molecular docking to identify putative inhibitors of Acinetobacter baumannii MurF (AbMurF). Based on comparative docking analysis, compound 114 (ethyl pyridine substituted 3-cyanothiophene) was predicted to potentially be the most active ligand. Computational pharmacokinetic characterization of drug-likeness of the compound showed it to fulfil all the parameters of Muegge and the MDDR rule. A molecular dynamic simulation of 114 indicated the complex to be stable on the basis of an average root mean square deviation (RMSD) value of 2.09Å for the ligand. The stability of the complex was further supported by root mean square fluctuation (RMSF), beta factor and radius of gyration values. Analyzing the complex using radial distribution function (RDF) and a novel analytical tool termed the axial frequency distribution (AFD) illustrated that after simulation the ligand is positioned in close vicinity of the protein active site where Thr42 and Asp43 participate in hydrogen bonding and stabilization of the complex. Binding free energy calculations based on the Poisson-Boltzmann or Generalized-Born Surface Area Continuum Solvation (MM(PB/GB)SA) method indicated the van der Waals contribution to the overall binding energy of the complex to be dominant along with electrostatic contributions involving the hot spot amino acids from the protein active site. The present results indicate that the screened compound 114 may act as a parent structure for designing potent derivatives against AbMurF in specific and MurF of other bacterial pathogens in general. Copyright © 2017 Elsevier Inc. All rights reserved.

A critical analysis of test-retest reliability in instrument validation studies of cancer patients under palliative care: a systematic review

PubMed Central

2014-01-01

Background Patient-reported outcome validation needs to achieve validity and reliability standards. Among reliability analysis parameters, test-retest reliability is an important psychometric property. Retested patients must be in a clinically stable condition. This is particularly problematic in palliative care (PC) settings because advanced cancer patients are prone to a faster rate of clinical deterioration. The aim of this study was to evaluate the methods by which multi-symptom and health-related qualities of life (HRQoL) based on patient-reported outcomes (PROs) have been validated in oncological PC settings with regards to test-retest reliability. Methods A systematic search of PubMed (1966 to June 2013), EMBASE (1980 to June 2013), PsychInfo (1806 to June 2013), CINAHL (1980 to June 2013), and SCIELO (1998 to June 2013), and specific PRO databases was performed. Studies were included if they described a set of validation studies. Studies were included if they described a set of validation studies for an instrument developed to measure multi-symptom or multidimensional HRQoL in advanced cancer patients under PC. The COSMIN checklist was used to rate the methodological quality of the study designs. Results We identified 89 validation studies from 746 potentially relevant articles. From those 89 articles, 31 measured test-retest reliability and were included in this review. Upon critical analysis of the overall quality of the criteria used to determine the test-retest reliability, 6 (19.4%), 17 (54.8%), and 8 (25.8%) of these articles were rated as good, fair, or poor, respectively, and no article was classified as excellent. Multi-symptom instruments were retested over a shortened interval when compared to the HRQoL instruments (median values 24 hours and 168 hours, respectively; p = 0.001). Validation studies that included objective confirmation of clinical stability in their design yielded better results for the test-retest analysis with regard to both pain and global HRQoL scores (p < 0.05). The quality of the statistical analysis and its description were of great concern. Conclusion Test-retest reliability has been infrequently and poorly evaluated. The confirmation of clinical stability was an important factor in our analysis, and we suggest that special attention be focused on clinical stability when designing a PRO validation study that includes advanced cancer patients under PC. PMID:24447633

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

PubMed

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

2017-01-01

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

Guidelines for the practical stability studies of anticancer drugs: a European consensus conference.

PubMed

Bardin, C; Astier, A; Vulto, A; Sewell, G; Vigneron, J; Trittler, R; Daouphars, M; Paul, M; Trojniak, M; Pinguet, F

2011-07-01

Stability studies performed by the pharmaceutical industry are only designed to fulfill licensing requirements. Thus, post-dilution or -reconstitution stability data are frequently limited to 24h only for bacteriological reasons regardless of the true chemical stability which could, in many cases, be longer. In practice, the pharmacy-based centralized preparation may require infusions to be made several days in advance to provide, for example, the filling of ambulatory devices for continuous infusions or batch preparations for dose banding. Furthermore, a non-justified limited stability for expensive products is obviously very costly. Thus, there is a compelling need for additional stability data covering practical uses of anticancer drugs. A European conference consensus was held in France, May 2010, under the auspices of the French Society of Oncology Pharmacy (SFPO) to propose adapted rules on stability in practical situations and guidelines to perform corresponding stability studies. For each anticancer drug, considering their therapeutic index, the pharmacokinetics/pharmacodynamics (PK/PD) variability, specific clinical use and risks related to degradation products, the classical limit of 10% of degradation can be inappropriate. Therefore, acceptance limits must be clinically relevant and should be defined for each drug individually. Design of stability studies has to reflect the different needs of the clinical practice (preparation for the week-ends, outpatient transportations, implantable devices, dose banding…). It is essential to use validated stability-indicating methods, separating degradation products being formed in the practical use of the drug. Sequential temperature designs should be encouraged to replicate problems seen in daily practice such as rupture of the cold-chain or temperature-cycling between refrigerated storage and ambient in-use conditions. Stressed conditions are recommended to evaluate not only the role of classical variables (pH, temperature, light) but also the mechanical stress. Physical stability such as particles' formation should be systematically evaluated. The consensus conference focused on the need to perform more studies on the stability of biotherapies, including a minimum of three complementary separating methods and a careful evaluation of submicron aggregates. The determination of the biological activity of proteins could be also useful. A guideline on the practical stability of anticancer drugs is proposed to cover current clinical and pharmaceutical practice. It should contribute to improved security of use, optimization of centralized handling and reduced costs. Finally, we have attempted to establish a new drug stability paradigm based on practical clinical needs, to complement regulatory guidelines which are essentially orientated to the stability of manufactured drugs. Copyright © 2011 Elsevier Masson SAS. All rights reserved.

A preliminary correlation of the orbiter stability and control aerodynamics from the first two Space Shuttle flights /STS-1 & 2/ with preflight predictions

NASA Technical Reports Server (NTRS)

Underwood, J. M.; Cooke, D. R.

1982-01-01

A correlation of the stability and control derivatives from flight (STS-1 & 2) with preflight predictions is presented across the Mach range from 0.9 to 25. Flight data obtained from specially designed flight test maneuvers as well as from conventional bank maneuvers generally indicate good agreement with predicted data. However, the vehicle appears to be lateral-directionally more stable than predicted in the transonic regime. Aerodynamic 'reasonableness tests' are employed to test for validity of flight data. The importance of testing multiple models in multiple wind tunnels at the same test conditions is demonstrated.

Quantitative bioanalysis of strontium in human serum by inductively coupled plasma-mass spectrometry

PubMed Central

Somarouthu, Srikanth; Ohh, Jayoung; Shaked, Jonathan; Cunico, Robert L; Yakatan, Gerald; Corritori, Suzana; Tami, Joe; Foehr, Erik D

2015-01-01

Aim: A bioanalytical method using inductively-coupled plasma-mass spectrometry to measure endogenous levels of strontium in human serum was developed and validated. Results & methodology: This article details the experimental procedures used for the method development and validation thus demonstrating the application of the inductively-coupled plasma-mass spectrometry method for quantification of strontium in human serum samples. The assay was validated for specificity, linearity, accuracy, precision, recovery and stability. Significant endogenous levels of strontium are present in human serum samples ranging from 19 to 96 ng/ml with a mean of 34.6 ± 15.2 ng/ml (SD). Discussion & conclusion: Calibration procedures and sample pretreatment were simplified for high throughput analysis. The validation demonstrates that the method was sensitive, selective for quantification of strontium (88Sr) and is suitable for routine clinical testing of strontium in human serum samples. PMID:28031925

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.

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.

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.

Dagger on Point: Assessing the Regionally-Aligned Brigade

DTIC Science & Technology

2013-04-01

missions in support of geographic combatant commanders’ (GCCs) Theater Campaign Plans ( TCPs ).7 Specifically, this EXORD provided direction for...studies of U.S. involvement in BPC and tested a series of validating factors and hypotheses to determine how they held up to real-world case examples55...hampered by other factors . Proposals for a bi-modal Army which include either a permanent Advisory Corps or a specialized Stability and

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.

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…

Influence of outdoor running fatigue and medial tibial stress syndrome on accelerometer-based loading and stability.

PubMed

Schütte, Kurt H; Seerden, Stefan; Venter, Rachel; Vanwanseele, Benedicte

2018-01-01

Medial tibial stress syndrome (MTSS) is a common overuse running injury with pathomechanics likely to be exaggerated by fatigue. Wearable accelerometry provides a novel alternative to assess biomechanical parameters continuously while running in more ecologically valid settings. The purpose of this study was to determine the influence of outdoor running fatigue and MTSS on both dynamic loading and dynamic stability derived from trunk and tibial accelerometery. Runners with (n=14) and without (n=16) history of MTSS performed an outdoor fatigue run of 3200m. Accelerometer-based measures averaged per lap included dynamic loading of the trunk and tibia (i.e. axial peak positive acceleration, signal power magnitude, and shock attenuation) as well as dynamic trunk stability (i.e. tri-axial root mean square ratio, step and stride regularity, and sample entropy). Regression coefficients from generalised estimating equations were used to evaluate group by fatigue interactions. No evidence could be found for dynamic loading being higher with fatigue in runners with MTSS history (all measures p>0.05). One significant group by running fatigue interaction effect was detected for dynamic stability. Specifically, in MTSS only, decreases mediolateral sample entropy i.e. loss of complexity was associated with running fatigue (p<0.01). The current results indicate that entire acceleration waveform signals reflecting mediolateral trunk control is related to MTSS history, a compensation that went undetected in the non-fatigued running state. We suggest that a practical outdoor running fatigue protocol that concurrently captures trunk accelerometry-based movement complexity warrants further prospective investigation as an in-situ screening tool for MTSS individuals. Copyright © 2017 Elsevier B.V. All rights reserved.

Quantification of endocrine disruptors and pesticides in water by gas chromatography-tandem mass spectrometry. Method validation using weighted linear regression schemes.

PubMed

Mansilha, C; Melo, A; Rebelo, H; Ferreira, I M P L V O; Pinho, O; Domingues, V; Pinho, C; Gameiro, P

2010-10-22

A multi-residue methodology based on a solid phase extraction followed by gas chromatography-tandem mass spectrometry was developed for trace analysis of 32 compounds in water matrices, including estrogens and several pesticides from different chemical families, some of them with endocrine disrupting properties. Matrix standard calibration solutions were prepared by adding known amounts of the analytes to a residue-free sample to compensate matrix-induced chromatographic response enhancement observed for certain pesticides. Validation was done mainly according to the International Conference on Harmonisation recommendations, as well as some European and American validation guidelines with specifications for pesticides analysis and/or GC-MS methodology. As the assumption of homoscedasticity was not met for analytical data, weighted least squares linear regression procedure was applied as a simple and effective way to counteract the greater influence of the greater concentrations on the fitted regression line, improving accuracy at the lower end of the calibration curve. The method was considered validated for 31 compounds after consistent evaluation of the key analytical parameters: specificity, linearity, limit of detection and quantification, range, precision, accuracy, extraction efficiency, stability and robustness. Copyright © 2010 Elsevier B.V. All rights reserved.

Capacitive sensing of N-formylamphetamine based on immobilized molecular imprinted polymers.

PubMed

Graniczkowska, Kinga; Pütz, Michael; Hauser, Frank M; De Saeger, Sarah; Beloglazova, Natalia V

2017-06-15

A highly sensitive, capacitive biosensor was developed to monitor trace amounts of an amphetamine precursor in aqueous samples. The sensing element is a gold electrode with molecular imprinted polymers (MIPs) immobilized on its surface. A continuous-flow system with timed injections was used to simulate flowing waterways, such as sewers, springs, rivers, etc., ensuring wide applicability of the developed product. MIPs, implemented as a recognition element due to their stability under harsh environmental conditions, were synthesized using thermo- and UV-initiated polymerization techniques. The obtained particles were compared against commercially available MIPs according to specificity and selectivity metrics; commercial MIPs were characterized by quite broad cross-reactivity to other structurally related amphetamine-type stimulants. After the best batch of MIPs was chosen, different strategies for immobilizing them on the gold electrode's surface were evaluated, and their stability was also verified. The complete, developed system was validated through analysis of spiked samples. The limit of detection (LOD) for N-formyl amphetamine was determined to be 10μM in this capacitive biosensor system. The obtained results indicate future possible applications of this MIPs-based capacitive biosensor for environmental and forensic analysis. To the best of our knowledge there are no existing MIPs-based sensors toward amphetamine-type stimulants (ATS). Copyright © 2016 Elsevier B.V. All rights reserved.

Characterization of Monobody Scaffold Interactions with Ligand via Force Spectroscopy and Steered Molecular Dynamics

NASA Astrophysics Data System (ADS)

Cheung, Luthur Siu-Lun; Shea, Daniel J.; Nicholes, Nathan; Date, Amol; Ostermeier, Marc; Konstantopoulos, Konstantinos

2015-02-01

Monobodies are antibody alternatives derived from fibronectin that are thermodynamically stable, small in size, and can be produced in bacterial systems. Monobodies have been engineered to bind a wide variety of target proteins with high affinity and specificity. Using alanine-scanning mutagenesis simulations, we identified two scaffold residues that are critical to the binding interaction between the monobody YS1 and its ligand, maltose-binding protein (MBP). Steered molecular dynamics (SMD) simulations predicted that the E47A and R33A mutations in the YS1 scaffold substantially destabilize the YS1-MBP interface by reducing the bond rupture force and the lifetime of single hydrogen bonds. SMD simulations further indicated that the R33A mutation weakens the hydrogen binding between all scaffold residues and MBP and not just between R33 and MBP. We validated the simulation data and characterized the effects of mutations on YS1-MBP binding by using single-molecule force spectroscopy and surface plasmon resonance. We propose that interfacial stability resulting from R33 of YS1 stacking with R344 of MBP synergistically stabilizes both its own bond and the interacting scaffold residues of YS1. Our integrated approach improves our understanding of the monobody scaffold interactions with a target, thus providing guidance for the improved engineering of monobodies.

A novel stability-indicating UPLC method development and validation for the determination of seven impurities in various diclofenac pharmaceutical dosage forms.

PubMed

Azougagh, M; Elkarbane, M; Bakhous, K; Issmaili, S; Skalli, A; Iben Moussad, S; Benaji, B

2016-09-01

An innovative simple, fast, precise and accurate ultra-high performance liquid chromatography (UPLC) method was developed for the determination of diclofenac (Dic) along with its impurities including the new dimer impurity in various pharmaceutical dosage forms. An Acquity HSS T3 (C18, 100×2.1mm, 1.8μm) column in gradient mode was used with mobile phase comprising of phosphoric acid, which has a pH value of 2.3 and methanol. The flow rate and the injection volume were set at 0.35ml·min(-1) and 1μl, respectively, and the UV detection was carried out at 254nm by using photodiode array detector. Dic was subjected to stress conditions from acid, base, hydrolytic, thermal, oxidative and photolytic degradation. The new developed method was successfully validated in accordance to the International Conference on Harmonization (ICH) guidelines with respect to specificity, limit of detection, limit of quantitation, precision, linearity, accuracy and robustness. The degradation products were well resolved from main peak and its seven impurities, proving the specificity power of the method. The method showed good linearity with consistent recoveries for Dic content and its impurities. The relative percentage of standard deviation obtained for the repeatability and intermediate precision experiments was less than 3% and LOQ was less than 0.5μg·ml(-1) for all compounds. The new proposed method was found to be accurate, precise, specific, linear and robust. In addition, the method was successfully applied for the assay determination of Dic and its impurities in the several pharmaceutical dosage forms. Copyright © 2016 Académie Nationale de Pharmacie. Published by Elsevier Masson SAS. All rights reserved.

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

PubMed

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

2016-05-01

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

[THERMAL STABILITY AS A PROGNOSTIC INDICATOR OF CONSERVATION OF LIVE EMBRYONIC SMALLPOX VACCINE (TEOVAC) DURING STORAGE].

PubMed

Zhukov, V A; Kokorev, S V; Rogozhkina, S V; Melnikov, D G; Terentiev, A I; Kovalchuk, E A; Vakhnov, E Yu; Borisevich, S V

2016-01-01

Determination of values of coefficients of thermal stability of TEOVac for prognosis of conservation of the vaccine (specific biological activity) during the process of warranty period storage. TEOVac (masticatory tablets) in primary packaging was kept at increased temperature (accelerated and stress-tests) and at the conditions established by PAP for the preparation (long-term tests). Biological activity of the vaccine was determined by titration on 12-day chicken embryos. A correlation between the value of coefficients of thermal stability and conservation of the prepared series of the condition preparation at the final date of storage was experimentally established. Coefficients of thermal stability could be used as a prognostic indicator of quality of the produced pelleted formulation of the preparation for evaluation of conservation of the vaccine during warranty period storage.

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

PubMed

Campos, Juliana Alvares Duarte Bonini; Maroco, João

2012-10-01

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

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

PubMed

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

2013-04-01

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

Multivariate approaches for stability control of the olive oil reference materials for sensory analysis - part I: framework and fundamentals.

PubMed

Valverde-Som, Lucia; Ruiz-Samblás, Cristina; Rodríguez-García, Francisco P; Cuadros-Rodríguez, Luis

2018-02-09

Virgin olive oil is the only food product for which sensory analysis is regulated to classify it in different quality categories. To harmonize the results of the sensorial method, the use of standards or reference materials is crucial. The stability of sensory reference materials is required to enable their suitable control, aiming to confirm that their specific target values are maintained on an ongoing basis. Currently, such stability is monitored by means of sensory analysis and the sensory panels are in the paradoxical situation of controlling the standards that are devoted to controlling the panels. In the present study, several approaches based on similarity analysis are exploited. For each approach, the specific methodology to build a proper multivariate control chart to monitor the stability of the sensory properties is explained and discussed. The normalized Euclidean and Mahalanobis distances, the so-called nearness and hardiness indices respectively, have been defined as new similarity indices to range the values from 0 to 1. Also, the squared mean from Hotelling's T 2 -statistic and Q 2 -statistic has been proposed as another similarity index. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

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.

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

PubMed

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

2010-11-01

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

Validation of an asthma questionnaire for use in healthcare workers

PubMed Central

Delclos, G L; Arif, A A; Aday, L; Carson, A; Lai, D; Lusk, C; Stock, T; Symanski, E; Whitehead, L W; Benavides, F G; Antó, J M

2006-01-01

Background Previous studies have described increased occurrence of asthma among healthcare workers, but to our knowledge there are no validated survey questionnaires with which to study this occupational group. Aims To develop, validate, and refine a new survey instrument on asthma for use in epidemiological studies of healthcare workers. Methods An initial draft questionnaire, designed by a multidisciplinary team, used previously validated questions where possible; the occupational exposure section was developed by updating health services specific chemical lists through hospital walk‐through surveys and review of material safety data sheets. A cross‐sectional validation study was conducted in 118 non‐smoking subjects, who also underwent bronchial challenge testing, an interview with an industrial hygienist, and measurement of specific IgE antibodies to common aeroallergens. Results The final version consisted of 43 main questions in four sections. Time to completion of the questionnaire ranged from 13 to 25 minutes. Test–retest reliability of asthma and allergy items ranged from 75% to 94%, and internal consistency for these items was excellent (Cronbach's α ⩾ 0.86). Against methacholine challenge, an eight item combination of asthma related symptoms had a sensitivity of 71% and specificity of 70%; against a physician diagnosis of asthma, this same combination showed a sensitivity of 79% and specificity of 98%. Agreement between self‐reported exposures and industrial hygienist review was similar to previous studies and only moderate, indicating the need to incorporate more reliable methods of exposure assessment. Against the aerollergen panel, the best combinations of sensitivity and specificity were obtained for a history of allergies to dust, dust mite, and animals. Conclusions Initial evaluation of this new questionnaire indicates good validity and reliability, and further field testing and cross‐validation in a larger healthcare worker population is in progress. The need for development of more reliable occupational exposure assessment methods that go beyond self‐report is underscored. PMID:16497858

Development, Validation and Application of RP-HPLC Method: Simultaneous Determination of Antihistamine and Preservatives with Paracetamol in Liquid Formulations and Human Serum.

PubMed

Hasan, Najmul; Chaiharn, Mathurot; Toor, Umair Ali; Mirani, Zulfiqar Ali; Sajjad, Ghulam; Sher, Nawab; Aziz, Mubashir; Siddiqui, Farhan Ahmed

2016-01-01

In this article we describe development and validation of stability indicating, accurate, specific, precise and simple Ion-pairing RP-HPLC method for simultaneous determination of paracetamol and cetirizine HCl along with preservatives i.e. propylparaben, and methylparaben in pharmaceutical dosage forms of oral solution and in serum. Acetonitrile: Buffer: Sulfuric Acid (45:55:0.3 v/v/v) was the mobile phase at flow rate 1.0 mL min(-1) using a Hibar(®) Lichrosorb(®) C18 column and monitored at wavelength of 230nm. The averages of absolute and relative recoveries were found to be 99.3%, 99.5%, 99.8% and 98.7% with correlation coefficient of 0.9977, 0.9998, 0.9984, and 0.9997 for cetirizine HCl, paracetamol, methylparaben and Propylparaben respectively. The limit of quantification and limit of detection were in range of 0.3 to 2.7 ng mL(-1) and 0.1 to 0.8 ng mL(-1) respectively. Under stress conditions of acidic, basic, oxidative, and thermal degradation, maximum degradation was observed in basic and oxidative stress where a significant impact was observed while all drugs were found almost stable in the other conditions. The developed method was validated in accordance with ICH and AOAC guidelines. The proposed method was successfully applied to quantify amount of paracetamol, cetirizine HCl and two most common microbial preservatives in bulk, dosage form and physiological fluid.

Development, Validation and Application of RP-HPLC Method: Simultaneous Determination of Antihistamine and Preservatives with Paracetamol in Liquid Formulations and Human Serum

PubMed Central

Hasan, Najmul; Chaiharn, Mathurot; Toor, Umair Ali; Mirani, Zulfiqar Ali; Sajjad, Ghulam; Sher, Nawab; Aziz, Mubashir; Siddiqui, Farhan Ahmed

2016-01-01

In this article we describe development and validation of stability indicating, accurate, specific, precise and simple Ion-pairing RP-HPLC method for simultaneous determination of paracetamol and cetirizine HCl along with preservatives i.e. propylparaben, and methylparaben in pharmaceutical dosage forms of oral solution and in serum. Acetonitrile: Buffer: Sulfuric Acid (45:55:0.3 v/v/v) was the mobile phase at flow rate 1.0 mL min-1 using a Hibar® Lichrosorb® C18 column and monitored at wavelength of 230nm. The averages of absolute and relative recoveries were found to be 99.3%, 99.5%, 99.8% and 98.7% with correlation coefficient of 0.9977, 0.9998, 0.9984, and 0.9997 for cetirizine HCl, paracetamol, methylparaben and Propylparaben respectively. The limit of quantification and limit of detection were in range of 0.3 to 2.7 ng mL-1 and 0.1 to 0.8 ng mL-1 respectively. Under stress conditions of acidic, basic, oxidative, and thermal degradation, maximum degradation was observed in basic and oxidative stress where a significant impact was observed while all drugs were found almost stable in the other conditions. The developed method was validated in accordance with ICH and AOAC guidelines. The proposed method was successfully applied to quantify amount of paracetamol, cetirizine HCl and two most common microbial preservatives in bulk, dosage form and physiological fluid. PMID:27651840

Reliability, validity, sensitivity and specificity of Guajarati version of the Roland-Morris Disability Questionnaire.

PubMed

Nambi, S Gopal

2013-01-01

The most common instruments developed to assess the functional status of patients with Non specific low back pain is the Roland-Morris Disability Questionnaire (RMDQ). Clinical and epidemiological research related to low back pain in the Gujarati population would be facilitated by the availability of well-established outcome measures. To find the reliability, validity, sensitivity and specificity of the Gujarati version of the RMDQ for use in Non Specific Chronic low back pain. A reliability, validity, sensitivity and specificity study of Gujarati version of the Roland-Morris Disability Questionnaire (RMDQ). Thirty out patients with Non Specific Chronic low back pain were assessed by the RMDQ. Reliability is assessed by using internal consistency and the intra-class correlation coefficient (ICC). Internal construct validity is assessed by RASCH Analysis and external construct validity is assessed by association with pain and spinal movement. Clinical calculator was used to determine the sensitivity and specificity. Internal consistency of the RMDQ is found to be adequate (> 0.65) at both times, with high ICC's also at both time points. Internal construct validity of the scale is good, indicating a single underlying construct. Expected associations with pain and spinal movement confirm external construct validity. The Sensitivity and Specificity at cut off point of 0.5 was 80% and 84% with respectively positive predictive value (PPV) of 83.33% and negative predictive value (NPV) of 80.76%. The Questionnaire is at the ordinal level. The RMDQ is a one-dimensional, ordinal measure, which works well in the Gujarati population.

Adaptive GSA-based optimal tuning of PI controlled servo systems with reduced process parametric sensitivity, robust stability and controller robustness.

PubMed

Precup, Radu-Emil; David, Radu-Codrut; Petriu, Emil M; Radac, Mircea-Bogdan; Preitl, Stefan

2014-11-01

This paper suggests a new generation of optimal PI controllers for a class of servo systems characterized by saturation and dead zone static nonlinearities and second-order models with an integral component. The objective functions are expressed as the integral of time multiplied by absolute error plus the weighted sum of the integrals of output sensitivity functions of the state sensitivity models with respect to two process parametric variations. The PI controller tuning conditions applied to a simplified linear process model involve a single design parameter specific to the extended symmetrical optimum (ESO) method which offers the desired tradeoff to several control system performance indices. An original back-calculation and tracking anti-windup scheme is proposed in order to prevent the integrator wind-up and to compensate for the dead zone nonlinearity of the process. The minimization of the objective functions is carried out in the framework of optimization problems with inequality constraints which guarantee the robust stability with respect to the process parametric variations and the controller robustness. An adaptive gravitational search algorithm (GSA) solves the optimization problems focused on the optimal tuning of the design parameter specific to the ESO method and of the anti-windup tracking gain. A tuning method for PI controllers is proposed as an efficient approach to the design of resilient control systems. The tuning method and the PI controllers are experimentally validated by the adaptive GSA-based tuning of PI controllers for the angular position control of a laboratory servo system.

Peptide-dependent Conformational Fluctuation Determines the Stability of the Human Leukocyte Antigen Class I Complex*

PubMed Central

Yanaka, Saeko; Ueno, Takamasa; Shi, Yi; Qi, Jianxun; Gao, George F.; Tsumoto, Kouhei; Sugase, Kenji

2014-01-01

In immune-mediated control of pathogens, human leukocyte antigen (HLA) class I presents various antigenic peptides to CD8+ T-cells. Long-lived peptide presentation is important for efficient antigen-specific T-cell activation. Presentation time depends on the peptide sequence and the stability of the peptide-HLA complex (pHLA). However, the determinant of peptide-dependent pHLA stability remains elusive. Here, to reveal the pHLA stabilization mechanism, we examined the crystal structures of an HLA class I allomorph in complex with HIV-derived peptides and evaluated site-specific conformational fluctuations using NMR. Although the crystal structures of various pHLAs were almost identical independent of the peptides, fluctuation analyses identified a peptide-dependent minor state that would be more tightly packed toward the peptide. The minor population correlated well with the thermostability and cell surface presentation of pHLA, indicating that this newly identified minor state is important for stabilizing the pHLA and facilitating T-cell recognition. PMID:25028510

Estimating Classification Consistency and Accuracy for Cognitive Diagnostic Assessment

ERIC Educational Resources Information Center

Cui, Ying; Gierl, Mark J.; Chang, Hua-Hua

2012-01-01

This article introduces procedures for the computation and asymptotic statistical inference for classification consistency and accuracy indices specifically designed for cognitive diagnostic assessments. The new classification indices can be used as important indicators of the reliability and validity of classification results produced by…

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

PubMed

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

2008-08-06

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

Climate Change, State Stability, and Political Risk in Africa

DTIC Science & Technology

2016-09-30

instructions , searching existing data sources, gathering and maintaining the data needed, and completing and reviewing the collection of information ...with a collection of information if it does not display a currently valid OMB control number. PLEASE DO NOT RETURN YOUR FORM TO THE ABOVE ADDRESS...model. For a number of indicators, particularly in the household and community resilience basket, data from the USAID Demographic and Health Surveys

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.

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.

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

Effects of McGill stabilization exercises and conventional physiotherapy on pain, functional disability and active back range of motion in patients with chronic non-specific low back pain.

PubMed

Ghorbanpour, Arsalan; Azghani, Mahmoud Reza; Taghipour, Mohammad; Salahzadeh, Zahra; Ghaderi, Fariba; Oskouei, Ali E

2018-04-01

[Purpose] The aim of this study was to compare the effects of "McGill stabilization exercises" and "conventional physiotherapy" on pain, functional disability and active back flexion and extension range of motion in patients with chronic non-specific low back pain. [Subjects and Methods] Thirty four patients with chronic non-specific low back pain were randomly assigned to McGill stabilization exercises group (n=17) and conventional physiotherapy group (n=17). In both groups, patients performed the corresponding exercises for six weeks. The visual analog scale (VAS), Quebec Low Back Pain Disability Scale Questionnaire and inclinometer were used to measure pain, functional disability, and active back flexion and extension range of motion, respectively. [Results] Statistically significant improvements were observed in pain, functional disability, and active back extension range of motion in McGill stabilization exercises group. However, active back flexion range of motion was the only clinical symptom that statistically increased in patients who performed conventional physiotherapy. There was no significant difference between the clinical characteristics while compared these two groups of patients. [Conclusion] The results of this study indicated that McGill stabilization exercises and conventional physiotherapy provided approximately similar improvement in pain, functional disability, and active back range of motion in patients with chronic non-specific low back pain. However, it appears that McGill stabilization exercises provide an additional benefit to patients with chronic non-specific low back, especially in pain and functional disability improvement.

Factors affecting unsafe behavior in construction projects: development and validation of a new questionnaire.

PubMed

Asilian-Mahabadi, Hassan; Khosravi, Yahya; Hassanzadeh-Rangi, Narmin; Hajizadeh, Ebrahim; Behzadan, Amir H

2018-02-05

Occupational safety in general, and construction safety in particular, is a complex phenomenon. This study was designed to develop a new valid measure to evaluate factors affecting unsafe behavior in the construction industry. A new questionnaire was generated from qualitative research according to the principles of grounded theory. Key measurement properties (face validity, content validity, construct validity, reliability and discriminative validity) were examined using qualitative and quantitative approaches. The receiver operating characteristic curve was used to estimate the discriminating power and the optimal cutoff score. Construct validity revealed an interpretable 12-factor structure which explained 61.87% of variance. Good internal consistency (Cronbach's α = 0.94) and stability (intra-class correlation coefficient = 0.93) were found for the new instrument. The area under the curve, sensitivity and specificity were 0.80, 0.80 and 0.75, respectively. The new instrument also discriminated safety performance among the construction sites with different workers' accident histories (F = 6.40, p < 0.05). The new instrument appears to be a valid, reliable and sensitive instrument that will contribute to investigating the root causes of workers' unsafe behaviors, thus promoting safety performance in the construction industry.

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

PubMed Central

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

2014-01-01

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

Validity and Utility of the Parent--Teacher Relationship Scale-II

ERIC Educational Resources Information Center

Dawson, Anne E.; Wymbs, Brian T.

2016-01-01

Preliminary findings indicate that positive relations between parents and teachers are associated with successful school outcomes for children. However, measures available to assess parent-teacher relations are scant. The current study examined validity evidence for the Parent-Teacher Relationship Scale-I (PTRS). Specifically, the internal…

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.

A Stability-Indicating HPLC Method for the Determination of Nitrosylcobalamin (NO-Cbl), a Novel Vitamin B12 Analog.

PubMed

Dunphy, Michael J; Sysel, Annette M; Lupica, Joseph A; Griffith, Kristie; Sherrod, Taylor; Bauer, Joseph A

2014-04-01

Nitrosylcobalamin (NO-Cbl), a novel vitamin B 12 analog and anti-tumor agent, functions as a biologic 'Trojan horse', utilizing the vitamin B 12 transcobalamin II transport protein and cell surface receptor to specifically target cancer cells. a stability-indicating HPLC method was developed for the detection of NO-Cbl during forced degradation studies. This method utilized an ascentis ® RP-amide (150 mm × 4.6 mm, 5 μm) column at 35 °C with a mobile phase (1.0 mL min -1 ) combining a gradient of methanol and an acetate buffer at pH 6.0. Detection wavelengths of 450 and 254 nm were used to detect corrin and non-corrin-based products, respectively. NO-Cbl, synthesized from hydroxocobalamin and pure nitric oxide gas, was subjected to degradative stress conditions including oxidation, hydrolysis and thermal and radiant energy challenge. The method was validated by assessing linearity, accuracy, precision, detection and quantitation limits and robustness. The method was applied successfully for purity assessment of synthesized NO-Cbl and for the determination of NO-Cbl during kinetic studies in aqueous solution and in solid-state degradation assessments. This HPLC method is suitable for the separation of cobalamins in aqueous and methanolic solutions, for routine detection of NO-Cbl and for purity assessment of synthesized NO-Cbl. additionally, this method has potential application in identification and monitoring of diseases involving altered nitric oxide homeostasis where vitamin B 12 therapy is utilized to scavenge excess nitric oxide, subsequently resulting in the in vivo production of NO-Cbl.

A Stability-Indicating HPLC Method for the Determination of Nitrosylcobalamin (NO-Cbl), a Novel Vitamin B12 Analog

PubMed Central

Dunphy, Michael J.; Sysel, Annette M.; Lupica, Joseph A.; Griffith, Kristie; Sherrod, Taylor

2014-01-01

Nitrosylcobalamin (NO-Cbl), a novel vitamin B12 analog and anti-tumor agent, functions as a biologic ‘Trojan horse’, utilizing the vitamin B12 transcobalamin II transport protein and cell surface receptor to specifically target cancer cells. a stability-indicating HPLC method was developed for the detection of NO-Cbl during forced degradation studies. This method utilized an ascentis® RP-amide (150 mm × 4.6 mm, 5 μm) column at 35 °C with a mobile phase (1.0 mL min−1) combining a gradient of methanol and an acetate buffer at pH 6.0. Detection wavelengths of 450 and 254 nm were used to detect corrin and non-corrin-based products, respectively. NO-Cbl, synthesized from hydroxocobalamin and pure nitric oxide gas, was subjected to degradative stress conditions including oxidation, hydrolysis and thermal and radiant energy challenge. The method was validated by assessing linearity, accuracy, precision, detection and quantitation limits and robustness. The method was applied successfully for purity assessment of synthesized NO-Cbl and for the determination of NO-Cbl during kinetic studies in aqueous solution and in solid-state degradation assessments. This HPLC method is suitable for the separation of cobalamins in aqueous and methanolic solutions, for routine detection of NO-Cbl and for purity assessment of synthesized NO-Cbl. additionally, this method has potential application in identification and monitoring of diseases involving altered nitric oxide homeostasis where vitamin B12 therapy is utilized to scavenge excess nitric oxide, subsequently resulting in the in vivo production of NO-Cbl. PMID:24855323

QSAR study on the removal efficiency of organic pollutants in supercritical water based on degradation temperature.

PubMed

Jiang, Ai; Cheng, Zhiwen; Shen, Zhemin; Guo, Weimin

2018-02-13

This paper aims to study temperature-dependent quantitative structure activity relationship (QSAR) models of supercritical water oxidation (SCWO) process which were developed based on Arrhenius equation between oxidation reaction rate and temperature. Through exploring SCWO process, each kinetic rate constant was studied for 21 organic substances, including azo dyes, heterocyclic compounds and ionic compounds. We propose the concept of T R95 , which is defined as the temperature at removal ratio of 95%, it is a key indicator to evaluate compounds' complete oxidation. By using Gaussian 09 and Material Studio 7.0, quantum chemical parameters were conducted for each organic compound. The optimum model is T R95  = 654.775 + 1761.910f(+) n  - 177.211qH with squared regression coefficient R 2  = 0.620 and standard error SE = 35.1. Nearly all the compounds could obtain accurate predictions of their degradation rate. Effective QSAR model exactly reveals three determinant factors, which are directly related to degradation rules. Specifically, the lowest f(+) value of main-chain atoms (f(+) n ) indicates the degree of affinity for nucleophilic attack. qH shows the ease or complexity of valence-bond breakage of organic molecules. BO x refers to the stability of a bond. Coincidentally, the degradation mechanism could reasonably be illustrated from each perspective, providing a deeper insight of universal and propagable oxidation rules. Besides, the satisfactory results of internal and external validations suggest the stability, reliability and predictive ability of optimum model.

Stabilization of protein-protein interactions in drug discovery.

PubMed

Andrei, Sebastian A; Sijbesma, Eline; Hann, Michael; Davis, Jeremy; O'Mahony, Gavin; Perry, Matthew W D; Karawajczyk, Anna; Eickhoff, Jan; Brunsveld, Luc; Doveston, Richard G; Milroy, Lech-Gustav; Ottmann, Christian

2017-09-01

PPIs are involved in every disease and specific modulation of these PPIs with small molecules would significantly improve our prospects of developing therapeutic agents. Both industry and academia have engaged in the identification and use of PPI inhibitors. However in comparison, the opposite strategy of employing small-molecule stabilizers of PPIs is underrepresented in drug discovery. Areas covered: PPI stabilization has not been exploited in a systematic manner. Rather, this concept validated by a number of therapeutically used natural products like rapamycin and paclitaxel has been shown retrospectively to be the basis of the activity of synthetic molecules originating from drug discovery projects among them lenalidomide and tafamidis. Here, the authors cover the growing number of synthetic small-molecule PPI stabilizers to advocate for a stronger consideration of this as a drug discovery approach. Expert opinion: Both the natural products and the growing number of synthetic molecules show that PPI stabilization is a viable strategy for drug discovery. There is certainly a significant challenge to adapt compound libraries, screening techniques and downstream methodologies to identify, characterize and optimize PPI stabilizers, but the examples of molecules reviewed here in our opinion justify these efforts.

Validation of the measure automobile emissions model : a statistical analysis

DOT National Transportation Integrated Search

2000-09-01

The Mobile Emissions Assessment System for Urban and Regional Evaluation (MEASURE) model provides an external validation capability for hot stabilized option; the model is one of several new modal emissions models designed to predict hot stabilized e...

Establishing Reliability and Validity of the Criterion Referenced Exam of GeoloGy Standards EGGS

NASA Astrophysics Data System (ADS)

Guffey, S. K.; Slater, S. J.; Slater, T. F.; Schleigh, S.; Burrows, A. C.

2016-12-01

Discipline-based geoscience education researchers have considerable need for a criterion-referenced, easy-to-administer and -score conceptual diagnostic survey for undergraduates taking introductory science survey courses in order for faculty to better be able to monitor the learning impacts of various interactive teaching approaches. To support ongoing education research across the geosciences, we are continuing to rigorously and systematically work to firmly establish the reliability and validity of the recently released Exam of GeoloGy Standards, EGGS. In educational testing, reliability refers to the consistency or stability of test scores whereas validity refers to the accuracy of the inferences or interpretations one makes from test scores. There are several types of reliability measures being applied to the iterative refinement of the EGGS survey, including test-retest, alternate form, split-half, internal consistency, and interrater reliability measures. EGGS rates strongly on most measures of reliability. For one, Cronbach's alpha provides a quantitative index indicating the extent to which if students are answering items consistently throughout the test and measures inter-item correlations. Traditional item analysis methods further establish the degree to which a particular item is reliably assessing students is actually quantifiable, including item difficulty and item discrimination. Validity, on the other hand, is perhaps best described by the word accuracy. For example, content validity is the to extent to which a measurement reflects the specific intended domain of the content, stemming from judgments of people who are either experts in the testing of that particular content area or are content experts. Perhaps more importantly, face validity is a judgement of how representative an instrument is reflective of the science "at face value" and refers to the extent to which a test appears to measure a the targeted scientific domain as viewed by laypersons, examinees, test users, the public, and other invested stakeholders.

[Reliability and validity of warning signs checklist for screening psychological, behavioral and developmental problems of children].

PubMed

Huang, X N; Zhang, Y; Feng, W W; Wang, H S; Cao, B; Zhang, B; Yang, Y F; Wang, H M; Zheng, Y; Jin, X M; Jia, M X; Zou, X B; Zhao, C X; Robert, J; Jing, Jin

2017-06-02

Objective: To evaluate the reliability and validity of warning signs checklist developed by the National Health and Family Planning Commission of the People's Republic of China (NHFPC), so as to determine the screening effectiveness of warning signs on developmental problems of early childhood. Method: Stratified random sampling method was used to assess the reliability and validity of checklist of warning sign and 2 110 children 0 to 6 years of age(1 513 low-risk subjects and 597 high-risk subjects) were recruited from 11 provinces of China. The reliability evaluation for the warning signs included the test-retest reliability and interrater reliability. With the use of Age and Stage Questionnaire (ASQ) and Gesell Development Diagnosis Scale (GESELL) as the criterion scales, criterion validity was assessed by determining the correlation and consistency between the screening results of warning signs and the criterion scales. Result: In terms of the warning signs, the screening positive rates at different ages ranged from 10.8%(21/141) to 26.2%(51/137). The median (interquartile) testing time for each subject was 1(0.6) minute. Both the test-retest reliability and interrater reliability of warning signs reached 0.7 or above, indicating that the stability was good. In terms of validity assessment, there was remarkable consistency between ASQ and warning signs, with the Kappa value of 0.63. With the use of GESELL as criterion, it was determined that the sensitivity of warning signs in children with suspected developmental delay was 82.2%, and the specificity was 77.7%. The overall Youden index was 0.6. Conclusion: The reliability and validity of warning signs checklist for screening early childhood developmental problems have met the basic requirements of psychological screening scales, with the characteristics of short testing time and easy operation. Thus, this warning signs checklist can be used for screening psychological and behavioral problems of early childhood, especially in community settings.

Transport of polymer stabilized nano-scale zero-valent iron in porous media

NASA Astrophysics Data System (ADS)

Mondal, Pulin K.; Furbacher, Paul D.; Cui, Ziteng; Krol, Magdalena M.; Sleep, Brent E.

2018-05-01

This study presents a set of laboratory-scale transport experiments and numerical simulations evaluating carboxymethyl cellulose (CMC) polymer stabilized nano-scale zero-valent iron (nZVI) transport. The experiments, performed in a glass-walled two-dimensional (2D) porous medium system, were conducted to identify the effects of water specific discharge and CMC concentration on nZVI transport and to produce data for model validation. The transport and movement of a tracer lissamine green B® (LGB) dye, CMC, and CMC-nZVI were evaluated through analysis of the breakthrough curves (BTCs) at the outlets, the time-lapsed images of the plume, and retained nZVI in the sandbox. The CMC mass recovery was > 95% when injected alone and about 65% when the CMC-nZVI mixture was used. However, the mean residence time of CMC was significantly higher than that of LGB. Of significance for field implementation, viscous fingering was observed in water displacement of previously injected CMC and CMC-nZVI. The mass recovery of nZVI was lower (< 50%) than CMC recovery due to attachment onto sand grain surfaces. Consecutive CMC-nZVI injections showed higher nZVI recovery in the second injection, a factor to be considered in field trials with successive CMC-nZVI injections. Transport of LGB, CMC, and nZVI were modeled using a flow and transport model considering LGB and CMC as solutes, and nZVI as a colloid, with variable solution viscosity due to changes in CMC concentrations. The simulation results matched the experimental observations and provided estimates of transport parameters, including attachment efficiency, that can be used to predict CMC stabilized nZVI transport in similar porous media, although the extent of viscous fingering may be underpredicted. The experimental and simulation results indicated that increasing specific discharge had a greater effect on decreasing CMC-nZVI attachment efficiency (corresponding to greater possible travel distances in the field) than increasing CMC concentration.

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

PubMed

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

2014-09-01

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

Sensitivity and Specificity of Stability Criteria for Immediately Loaded Splinted Maxillary Implants.

PubMed

Wentaschek, Stefan; Scheller, Herbert; Schmidtmann, Irene; Hartmann, Sinsa; Weyhrauch, Michael; Weibrich, Gernot; Lehmann, Karl Martin

2015-10-01

To assess the suitability of dental implants for immediate loading, primary stability is usually evaluated intraoperatively. This retrospective study aimed to assess the suitability of three stability parameters - namely, insertion torque (IT), implant stability quotient (ISQ; measured by resonance frequency analysis), and Periotest (PT) values - as potential predictors for the risk of nonosseointegration of immediately loaded splinted implants. The stability parameters were routinely collected under immediate loading. Nineteen patients with 11 edentulous and 8 partially edentulous maxillae were treated with 105 dental implants, which were immediately loaded using temporary fixed dentures. The IT results, PT values, and ISQ results were recorded. Receiver operating characteristic analysis was performed to assess the quality of each parameter as a diagnostic test. After a 3-month observation period, 11 implants in four patients were not osseointegrated. The IT and ISQ (IT 25.0 ± 12.5 Ncm and 8.4 ± 2.3 Ncm; PT -1.5 ± 3.0 and +2.7 ± 3.0; and ISQ 62.6 ± 6.7 and 54.7 ± 6.2) differed significantly between the osseointegrated and failed implants (p < .005). The IT showed the greatest specificity at a sensitivity of 1 and the greatest area under the curve (AUC; 0.929), followed by the PT value (AUC = 0.836) and ISQ (AUC = 0.811). Among the intraoperative parameters analyzed, IT showed the highest specificity at a high sensitivity of 1. Therefore, the IT can be considered the most valid prognostic factor for osseointegration of immediately loaded splinted dental implants. © 2014 Wiley Periodicals, Inc.

Social Cohesion and the Labour Market: Societal Regimes of Civic Attitudes and Labour Market Regimes

ERIC Educational Resources Information Center

Dimeglio, Isabelle; Janmaat, Jan Germen; Mehaut, Philippe

2013-01-01

The aim of this paper is to test the connections between the indicators used in the literature on social cohesion, which usually reflect "general" values or behaviours, and indicators specific to a particular space, namely the labour market. A key question is the stability of the social cohesion's indicators when moving from a societal…

An illness-specific version of the Revised Illness Perception Questionnaire in patients with atrial fibrillation (AF IPQ-R): Unpacking beliefs about treatment control, personal control and symptom triggers.

PubMed

Taylor, Elaina C; O'Neill, Mark; Hughes, Lyndsay D; Moss-Morris, Rona

2018-04-01

This study modified the Revised Illness Perception Questionnaire (IPQ-R) in patients with persistent atrial fibrillation (AF). Qualitative interviews and think-aloud techniques informed modification of the IPQ-R to be specific to AF patients. Confirmatory Factor Analysis (CFA) (n = 198) examined the validity of the modified IPQ-R (AF-IPQ-R). Exploratory factor analysis (EFA) examined the new AF-triggers scale. Construct validity examined associations between the AF-IPQ-R, quality of life (QoL) and beliefs about medicines. Test-retest and internal reliability were examined. Interviews indicated that patients viewed triggers of AF rather than initial causes of illness as more applicable. Patients believed specific behaviours such as rest could control AF. Treatment control beliefs related to pharmacological and procedural treatments. These data were used to modify the IPQ-R subscales and to develop a triggers of AF scale. CFA indicated good model fit. EFA of the triggers scale indicated three factors: emotional; health behaviours; and over-exertion triggers. Expected correlations were found between the AF-IPQ-R, QoL and treatment beliefs, evidencing good construct validity. The AF-IPQ-R showed sound psychometric properties. It provides more detailed specification than the IPQ-R of beliefs that may help to understand poor QoL in AF patients, and guidance for future interventions in this area.

Developing of Indicators of an E-Learning Benchmarking Model for Higher Education Institutions

ERIC Educational Resources Information Center

Sae-Khow, Jirasak

2014-01-01

This study was the development of e-learning indicators used as an e-learning benchmarking model for higher education institutes. Specifically, it aimed to: 1) synthesize the e-learning indicators; 2) examine content validity by specialists; and 3) explore appropriateness of the e-learning indicators. Review of related literature included…

Characterization and stability studies of bioactive compounds and food matrices as evidence in support of health claims.

PubMed

González-Ferrero, Carolina; Sáiz-Abajo, María-José

2015-07-01

The characterization and stability evaluation of food and food constituents (chemical active ingredient/microorganism) for which nutrition or health claims want to be requested are essential for the success of an application to EFSA. This work reviews the requirements that must be fulfilled for a full characterization of the active substance, comprising origin, elaboration, or extraction method, and chemical/microbiological composition, using validated analytical methods. The review focuses not only on establishing the specifications of the final active ingredient or food but also on ensuring homogeneity between batches. In addition, the article discusses the methodologies and conditions of the stability studies that need to be performed on food and food constituents to verify that the relevant compounds--chemical and microbiological active ingredients--will get to the consumer in the intended state and concentration to accomplish the claimed health effect over shelf life.

Quality of prenatal care questionnaire: instrument development and testing.

PubMed

Heaman, Maureen I; Sword, Wendy A; Akhtar-Danesh, Noori; Bradford, Amanda; Tough, Suzanne; Janssen, Patricia A; Young, David C; Kingston, Dawn A; Hutton, Eileen K; Helewa, Michael E

2014-06-03

Utilization indices exist to measure quantity of prenatal care, but currently there is no published instrument to assess quality of prenatal care. The purpose of this study was to develop and test a new instrument, the Quality of Prenatal Care Questionnaire (QPCQ). Data for this instrument development study were collected in five Canadian cities. Items for the QPCQ were generated through interviews with 40 pregnant women and 40 health care providers and a review of prenatal care guidelines, followed by assessment of content validity and rating of importance of items. The preliminary 100-item QPCQ was administered to 422 postpartum women to conduct item reduction using exploratory factor analysis. The final 46-item version of the QPCQ was then administered to another 422 postpartum women to establish its construct validity, and internal consistency and test-retest reliability. Exploratory factor analysis reduced the QPCQ to 46 items, factored into 6 subscales, which subsequently were validated by confirmatory factor analysis. Construct validity was also demonstrated using a hypothesis testing approach; there was a significant positive association between women's ratings of the quality of prenatal care and their satisfaction with care (r = 0.81). Convergent validity was demonstrated by a significant positive correlation (r = 0.63) between the "Support and Respect" subscale of the QPCQ and the "Respectfulness/Emotional Support" subscale of the Prenatal Interpersonal Processes of Care instrument. The overall QPCQ had acceptable internal consistency reliability (Cronbach's alpha = 0.96), as did each of the subscales. The test-retest reliability result (Intra-class correlation coefficient = 0.88) indicated stability of the instrument on repeat administration approximately one week later. Temporal stability testing confirmed that women's ratings of their quality of prenatal care did not change as a result of giving birth or between the early postpartum period and 4 to 6 weeks postpartum. The QPCQ is a valid and reliable instrument that will be useful in future research as an outcome measure to compare quality of care across geographic regions, populations, and service delivery models, and to assess the relationship between quality of care and maternal and infant health outcomes.

The role of glycosylation and domain interactions in the thermal stability of human angiotensin-converting enzyme.

PubMed

O'Neill, Hester G; Redelinghuys, Pierre; Schwager, Sylva L U; Sturrock, Edward D

2008-09-01

The N and C domains of somatic angiotensin-converting enzyme (sACE) differ in terms of their substrate specificity, inhibitor profiling, chloride dependency and thermal stability. The C domain is thermally less stable than sACE or the N domain. Since both domains are heavily glycosylated, the effect of glycosylation on their thermal stability was investigated by assessing their catalytic and physicochemical properties. Testis ACE (tACE) expressed in mammalian cells, mammalian cells in the presence of a glucosidase inhibitor and insect cells yielded proteins with altered catalytic and physicochemical properties, indicating that the more complex glycans confer greater thermal stabilization. Furthermore, a decrease in tACE and N-domain N-glycans using site-directed mutagenesis decreased their thermal stability, suggesting that certain N-glycans have an important effect on the protein's thermodynamic properties. Evaluation of the thermal stability of sACE domain swopover and domain duplication mutants, together with sACE expressed in insect cells, showed that the C domain contained in sACE is less dependent on glycosylation for thermal stabilization than a single C domain, indicating that stabilizing interactions between the two domains contribute to the thermal stability of sACE and are decreased in a C-domain-duplicating mutant.

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.

Pitching stability analysis of half-rotating wing air vehicle

NASA Astrophysics Data System (ADS)

Wang, Xiaoyi; Wu, Yang; Li, Qian; Li, Congmin; Qiu, Zhizhen

2017-06-01

Half-Rotating Wing (HRW) is a new power wing which had been developed by our work team using rotating-type flapping instead of oscillating-type flapping. Half-Rotating Wing Air Vehicle (HRWAV) is similar as Bionic Flapping Wing Air Vehicle (BFWAV). It is necessary to guarantee pitching stability of HRWAV to maintain flight stability. The working principle of HRW was firstly introduced in this paper. The rule of motion indicated that the fuselage of HRWAV without empennage would overturn forward as it generated increased pitching movement. Therefore, the empennage was added on the tail of HRWAV to balance the additional moment generated by aerodynamic force during flight. The stability analysis further shows that empennage could weaken rapidly the pitching disturbance on HRWAV and a new balance of fuselage could be achieved in a short time. Case study using numerical analysis verified correctness and validity of research results mentioned above, which could provide theoretical guidance to design and control HRWAV.

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

PubMed Central

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

2014-01-01

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

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

PubMed

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

2014-01-01

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

[Aseptic process validation and stability study of an injectable preparation of fructose (5%)-glycerol (10%) as part of a hospital clinical research program on endoscopic curative treatment for early epithelial neoplastic lesions of the gastrointestinal tract].

PubMed

Tall, M L; Salmon, D; Diouf, E; Drai, J; Filali, S; Lépilliez, V; Pioche, M; Laleye, D; Dhelens, C; Ponchon, T; Pivot, C; Pirot, F

2015-03-01

As part of a hospital clinical research program on endoscopic curative treatment for early epithelial neoplastic lesions of the gastrointestinal tract, a new hospital sterile and non-pyrogenic preparation of fructose (5%)-glycerol (10%) was realized. Under pharmaceutical legislation, the provision of this hospital preparation involves of aseptic process validation and achieve a stability study. After the aseptic process validation with Mediafill Test, the preparation was made under aseptic conditions associated with a sterilizing filtration according to the good practices preparation. Prepared flexible bags (100mL of solution) were stored for one year in a climatic chamber (25±2°C). To assess stability, the physicochemical controls (fructose concentration, glycerol concentration, hydroxy-methyl-5 furfural [5-HMF] concentration, sodium concentration, pH measure, osmolality and sub-visible particles count) and microbiological (bioburden, bacterial endotoxin and sterility) were performed at regular intervals for one year. Neither significant decrease of fructose concentration, glycerol concentration and sodium concentration nor pH, 5-HMF, osmolality variations out of specifications were observed for one year. The sub-visible particles count, the bacterial endotoxin and sterility were in accordance with the European pharmacopoeia attesting limpidity, apyrogenicity and sterility of this injectable preparation. The hospital preparation was stable over one year at 25±2°C, ensuring safe administration in humans within the framework of this clinical research. Copyright © 2014 Elsevier Masson SAS. All rights reserved.

Validating the Interpretations of PISA and TIMSS Tasks: A Rating Study

ERIC Educational Resources Information Center

Rindermann, Heiner; Baumeister, Antonia E. E.

2015-01-01

Scholastic tests regard cognitive abilities to be domain-specific competences. However, high correlations between competences indicate either high task similarity or a dependence on common factors. The present rating study examined the validity of 12 Programme for International Student Assessment (PISA) and Third or Trends in International…

Structural Validity of the WISC-IV for Students with Learning Disabilities

ERIC Educational Resources Information Center

Styck, Kara M.; Watkins, Marley W.

2016-01-01

The structural validity of the "Wechsler Intelligence Scale for Children-Fourth Edition" (WISC-IV) was evaluated using confirmatory factor analysis for a clinical sample of 1,537 students diagnosed with specific learning disabilities (SLD) by school psychologists in two large southwestern school districts. Results indicated that a…

A Powered Prosthetic Intervention for Bilateral Transfemoral Amputees

PubMed Central

Lawson, Brian E.; Ruhe, Brian; Shultz, Amanda; Goldfarb, Michael

2014-01-01

This paper presents the design and validation of a control system for a pair of powered knee and ankle prostheses to be used as a prosthetic intervention for bilateral transfemoral amputees. The control system leverages communication between the prostheses for enhanced awareness and stability, along with power generation at the knee and ankle joints to better restore biomechanical functionality in level ground walking. The control methodology employed is a combination of an impedance-based framework for weight-bearing portions of gait and a trajectory-based approach for the non-weight-bearing portions. The control system was implemented on a pair of self-contained powered knee and ankle prostheses, and the ability of the prostheses and control approach to provide walking functionality was assessed in a set of experimental trials with a bilateral transfemoral amputee subject. Specifically, experimental data from these trials indicate that the powered prostheses and bilateral control architecture provide gait kinematics that reproduce healthy gait kinematics to a greater extent than the subject’s daily-use passive prostheses. PMID:25014950

Reduction of Nuak1 Decreases Tau and Reverses Phenotypes in a Tauopathy Mouse Model.

PubMed

Lasagna-Reeves, Cristian A; de Haro, Maria; Hao, Shuang; Park, Jeehye; Rousseaux, Maxime W C; Al-Ramahi, Ismael; Jafar-Nejad, Paymaan; Vilanova-Velez, Luis; See, Lauren; De Maio, Antonia; Nitschke, Larissa; Wu, Zhenyu; Troncoso, Juan C; Westbrook, Thomas F; Tang, Jianrong; Botas, Juan; Zoghbi, Huda Y

2016-10-19

Many neurodegenerative proteinopathies share a common pathogenic mechanism: the abnormal accumulation of disease-related proteins. As growing evidence indicates that reducing the steady-state levels of disease-causing proteins mitigates neurodegeneration in animal models, we developed a strategy to screen for genes that decrease the levels of tau, whose accumulation contributes to the pathology of both Alzheimer disease (AD) and progressive supranuclear palsy (PSP). Integrating parallel cell-based and Drosophila genetic screens, we discovered that tau levels are regulated by Nuak1, an AMPK-related kinase. Nuak1 stabilizes tau by phosphorylation specifically at Ser356. Inhibition of Nuak1 in fruit flies suppressed neurodegeneration in tau-expressing Drosophila, and Nuak1 haploinsufficiency rescued the phenotypes of a tauopathy mouse model. These results demonstrate that decreasing total tau levels is a valid strategy for mitigating tau-related neurodegeneration and reveal Nuak1 to be a novel therapeutic entry point for tauopathies. Copyright © 2016 Elsevier Inc. All rights reserved.

The stability of hydrogen ion and specific conductance in filtered wet-deposition samples stored at ambient temperatures

USGS Publications Warehouse

Gordon, J.D.; Schroder, L.J.; Morden-Moore, A. L.; Bowersox, V.C.

1995-01-01

Separate experiments by the U.S. Geological Survey (USGS) and the Illinois State Water Survey Central Analytical Laboratory (CAL) independently assessed the stability of hydrogen ion and specific conductance in filtered wet-deposition samples stored at ambient temperatures. The USGS experiment represented a test of sample stability under a diverse range of conditions, whereas the CAL experiment was a controlled test of sample stability. In the experiment by the USGS, a statistically significant (?? = 0.05) relation between [H+] and time was found for the composited filtered, natural, wet-deposition solution when all reported values are included in the analysis. However, if two outlying pH values most likely representing measurement error are excluded from the analysis, the change in [H+] over time was not statistically significant. In the experiment by the CAL, randomly selected samples were reanalyzed between July 1984 and February 1991. The original analysis and reanalysis pairs revealed that [H+] differences, although very small, were statistically different from zero, whereas specific-conductance differences were not. Nevertheless, the results of the CAL reanalysis project indicate there appears to be no consistent, chemically significant degradation in sample integrity with regard to [H+] and specific conductance while samples are stored at room temperature at the CAL. Based on the results of the CAL and USGS studies, short-term (45-60 day) stability of [H+] and specific conductance in natural filtered wet-deposition samples that are shipped and stored unchilled at ambient temperatures was satisfactory.

Confirmatory factor analytic investigation of variance composition, gender invariance, and validity of the Male Role Norms Inventory-Adolescent-revised (MRNI-A-r).

PubMed

Levant, Ronald F; McDermott, Ryon C; Hewitt, Amber A; Alto, Kathleen M; Harris, Kyle T

2016-10-01

Confirmatory factor analysis of responses to the Male Role Norms Inventory-Adolescent-revised (MRNI-A-r) from 384 middle school students (163 boys, 221 girls) indicated that the best fit to the data was a bifactor model incorporating the hypothesized 3-factor structure while explicitly modeling an additional, general factor. Specifically, each item-level indicator loaded simultaneously on 2 factors: a general traditional masculinity ideology factor and a specific factor corresponding to 1 of the 3 hypothesized masculine norms for adolescents: Emotionally Detached Dominance, Toughness, and Avoidance of Femininity. Invariance testing across gender supported metric invariance for the general factor only. Although item loadings on the general factor were similar across boys and girls, the specific factor loadings varied substantially, with many becoming nonsignificant in the presence of the general factor for girls. A structural regression analysis predicting latent variables of the Meanings of Adolescent Masculinity Scale (MAMS), the Rosenberg Self-esteem Scale, and the Discipline, School Difficulties, and Positive Behavior Scale (DSDPBS) indicated that the general factor was a strong predictor of MAMS for both genders and DSDPBS for girls. Findings indicate that the MRNI-A-r general factor is a valid and reliable indicator of overall internalization of traditional masculinity ideology in adolescents; however, the specific factors may have different meanings for boys as compared with girls and lack validity in the presence of the general factor. These findings are consistent with a developmental perspective of gender ideology that views adolescence as a time when a differentiated cognitive schema of masculine norms is beginning to develop. (PsycINFO Database Record (c) 2016 APA, all rights reserved).

AHSP: a novel hemoglobin helper

PubMed Central

Bank, Arthur

2007-01-01

Recently, the small protein α hemoglobin–stabilizing protein (AHSP) was identified and found to specifically bind α-globin, stabilize its structure, and limit the toxic effects of excess α-globin, which are manifest in the inherited blood disorder β thalassemia. In this issue of the JCI, Yu, Weiss, and colleagues show that AHSP is also critical to the formation and stabilization of normal amounts of hemoglobin, even when α-globin is deficient, indicating unique and previously unidentified roles for this molecule (see the related article beginning on page 1856). PMID:17607349

Space Environment Effects on Stability of Medications Flown on Space Shuttles and the International Space Station (ISS)

NASA Technical Reports Server (NTRS)

Daniels, Vernie; Du, Jianping; Crady, Camille; Satterfield, Rick; Putcha, Lakshmi

2007-01-01

The purpose is to assess physical and chemical degradation of select pharmaceutical formulations from the Shuttle and ISS medical kits. Eleven pharmaceuticals dispensed as different dosage forms were selected based on their physical / chemical characteristics and susceptibility to environmental factors such as, temperature, humidity and light sensitivity. When available, ground-controls of the study medications with matching brand and lot numbers were used for comparison. Samples retrieved from flight were stored along with their matching controls in a temperature and humidity controlled environmental chamber. Temperature, humidity, and radiation data from the Shuttle and ISS were retrieved from onboard HOBO U12 Temp/RH Data Loggers, and from passive dosimeters. Physical and chemical analyses of the pharmaceuticals were conducted using validated United States Pharmacopeia (USP) methods. Results indicated degradation of 6 of the 11 formulations returned from space flights. Four formulations, Amoxicillin / Clavulanate, promethazine, sulfamethoxazole / trimethoprim, and ciprofloxacin tablets depicted discoloration after flight. Chemical content analyses using High or Ultra Performance Liquid Chromatography (HPLC / UPLC) methods revealed that dosage forms of Amoxicillin / Clavulanate, promethazine, sulfamethoxazole / trimethoprim, lidocaine, ciprofloxacin and mupirocin contained less than 95% of manufacturer s labeled claim of active drug compound. Shuttle and ISS environments affect stability and shelf life of certain mediations flown on these missions. Data analysis is in progress to examine the effect of specific space flight environmental factors on pharmaceutical stability. The degradation profiles generated from ground studies in analog environments will be useful in establishing predictive shelf-life profiles for medications intended for use during long-term space exploration missions.

Examination of the MMPI-2 restructured form (MMPI-2-RF) validity scales in civil forensic settings: findings from simulation and known group samples.

PubMed

Wygant, Dustin B; Ben-Porath, Yossef S; Arbisi, Paul A; Berry, David T R; Freeman, David B; Heilbronner, Robert L

2009-11-01

The current study examined the effectiveness of the MMPI-2 Restructured Form (MMPI-2-RF; Ben-Porath and Tellegen, 2008) over-reporting indicators in civil forensic settings. The MMPI-2-RF includes three revised MMPI-2 over-reporting validity scales and a new scale to detect over-reported somatic complaints. Participants dissimulated medical and neuropsychological complaints in two simulation samples, and a known-groups sample used symptom validity tests as a response bias criterion. Results indicated large effect sizes for the MMPI-2-RF validity scales, including a Cohen's d of .90 for Fs in a head injury simulation sample, 2.31 for FBS-r, 2.01 for F-r, and 1.97 for Fs in a medical simulation sample, and 1.45 for FBS-r and 1.30 for F-r in identifying poor effort on SVTs. Classification results indicated good sensitivity and specificity for the scales across the samples. This study indicates that the MMPI-2-RF over-reporting validity scales are effective at detecting symptom over-reporting in civil forensic settings.

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

PubMed

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

2018-01-01

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

Development and application of a validated stability-indicating HPLC method for simultaneous determination of granisetron hydrochloride, benzyl alcohol and their main degradation products in parenteral dosage forms.

PubMed

Hewala, Ismail; El-Fatatre, Hamed; Emam, Ehab; Mubrouk, Mokhtar

2010-06-30

A simple, rapid and sensitive reversed phase high performance liquid chromatographic method using photodiode array detection was developed and validated for the simultaneous determination of granisetron hydrochloride, benzyl alcohol, 1-methyl-1H-indazole-3-carboxylic acid (the main degradation product of granisetron) and benzaldehyde (the main degradation product of benzyl alcohol) in granisetron injections. The separation was achieved on Hypersil BDS C8 (250 mm x 4.6 mm i.d., 5 microm particle diameter) column using a mobile phase consisted of acetonitrile:0.05 M KH(2)PO(4):triethylamine (22:100:0.15) adjusted to pH 4.8. The column was maintained at 25 degrees C and 20 microL of solutions was injected. Photodiode array detector was used to test the peak purity and the chromatograms were extracted at 210 nm. Naphazoline hydrochloride was used as internal standard. The method was validated with respect to specificity, linearity, accuracy, precision, limit of quantitation and limit of detection. The validation acceptance criteria were met in all cases. Identification of the pure peaks was carried out using library match programmer and wavelengths of derivative optima of the spectrograms of the peaks. The method was successfully applied to the determination of the investigated drugs and their degradation products in different batches of granisetron injections. The method was proved to be sensitive for the determination down to 0.03 and 0.01% of granisetron degradation product and benzaldehyde, respectively, which are far below the compendia limits for testing these degradation products in their corresponding intact drugs. Copyright 2010 Elsevier B.V. All rights reserved.

Validation of the Headache Impact Test (HIT-6) in patients with chronic migraine.

PubMed

Rendas-Baum, Regina; Yang, Min; Varon, Sepideh F; Bloudek, Lisa M; DeGryse, Ronald E; Kosinski, Mark

2014-08-01

The Headache Impact Test (HIT)-6 was developed and has been validated in patients with various types of headache. The objective of this study was to report the psychometric properties of the HIT-6 among patients with chronic migraine. Data came from two international, multicenter, randomized, double-blind, placebo-controlled clinical trials of chronic migraine patients (N = 1,384) undergoing prophylaxis therapy. Confirmatory factor analysis and differential item functioning (DIF) analysis were used to test the latent structure and cross-cultural comparability of the HIT-6. Reliability, construct validity, and responsiveness were assessed. Two sets of criterion groups were used: (1) 28-day headache frequency: <10, 10-14, and ≥15 days; (2) sample quartiles of the total cumulative hours of headache: <140, 140 to <280, 280 to <420, and ≥420 hours. Two sets of responsiveness categories were defined as reduction of <30%, 30% to <50%, or ≥50% in (1) number of headache days and (2) cumulative hours of headache. Measurement invariance tests supported the stability of the HIT-6 latent structure across studies. DIF analysis supported cross-cultural comparability. Good reliability was observed across studies (Cronbach's α: 0.75-0.92; intraclass correlation coefficient: 0.76-0.80). HIT-6 scores correlated strongly (-0.86 to -0.59) with scores of the Migraine-Specific Quality-of-Life Questionnaire. Analysis of variance indicated that HIT-6 scores discriminated across both types of criterion groups (P<0.001), across studies and time points. HIT-6 change scores were significantly higher in magnitude in groups experiencing greater improvement (P<0.001). All measurement properties were consistently verified across the two studies, supporting the validity of the HIT-6 among chronic migraine patients. NCT00156910 and NCT00168428 on www.ClinicalTrials.gov.

A nomogram for predicting complications in patients with solid tumours and seemingly stable febrile neutropenia

PubMed Central

Fonseca, Paula Jiménez; Carmona-Bayonas, Alberto; García, Ignacio Matos; Marcos, Rosana; Castañón, Eduardo; Antonio, Maite; Font, Carme; Biosca, Mercè; Blasco, Ana; Lozano, Rebeca; Ramchandani, Avinash; Beato, Carmen; de Castro, Eva Martínez; Espinosa, Javier; Martínez-García, Jerónimo; Ghanem, Ismael; Cubero, Jorge Hernando; Manrique, Isabel Aragón; Navalón, Francisco García; Sevillano, Elena; Manzano, Aránzazu; Virizuela, Juan; Garrido, Marcelo; Mondéjar, Rebeca; Arcusa, María Ángeles; Bonilla, Yaiza; Pérez, Quionia; Gallardo, Elena; del Carmen Soriano, Maria; Cardona, Mercè; Lasheras, Fernando Sánchez; Cruz, Juan Jesús; Ayala, Francisco

2016-01-01

Background: We sought to develop and externally validate a nomogram and web-based calculator to individually predict the development of serious complications in seemingly stable adult patients with solid tumours and episodes of febrile neutropenia (FN). Patients and methods: The data from the FINITE study (n=1133) and University of Salamanca Hospital (USH) FN registry (n=296) were used to develop and validate this tool. The main eligibility criterion was the presence of apparent clinical stability, defined as events without acute organ dysfunction, abnormal vital signs, or major infections. Discriminatory ability was measured as the concordance index and stratification into risk groups. Results: The rate of infection-related complications in the FINITE and USH series was 13.4% and 18.6%, respectively. The nomogram used the following covariates: Eastern Cooperative Group (ECOG) Performance Status ⩾2, chronic obstructive pulmonary disease, chronic cardiovascular disease, mucositis of grade ⩾2 (National Cancer Institute Common Toxicity Criteria), monocytes <200/mm3, and stress-induced hyperglycaemia. The nomogram predictions appeared to be well calibrated in both data sets (Hosmer–Lemeshow test, P>0.1). The concordance index was 0.855 and 0.831 in each series. Risk group stratification revealed a significant distinction in the proportion of complications. With a ⩾116-point cutoff, the nomogram yielded the following prognostic indices in the USH registry validation series: 66% sensitivity, 83% specificity, 3.88 positive likelihood ratio, 48% positive predictive value, and 91% negative predictive value. Conclusions: We have developed and externally validated a nomogram and web calculator to predict serious complications that can potentially impact decision-making in patients with seemingly stable FN. PMID:27187687

Experimental and theoretical investigations on the validity of the geometrical optics model for calculating the stability of optical traps.

PubMed

Schut, T C; Hesselink, G; de Grooth, B G; Greve, J

1991-01-01

We have developed a computer program based on the geometrical optics approach proposed by Roosen to calculate the forces on dielectric spheres in focused laser beams. We have explicitly taken into account the polarization of the laser light and thd divergence of the laser beam. The model can be used to evaluate the stability of optical traps in a variety of different optical configurations. Our calculations explain the experimental observation by Ashkin that a stable single-beam optical trap, without the help of the gravitation force, can be obtained with a strongly divergent laser beam. Our calculations also predict a different trap stability in the directions orthogonal and parallel to the polarization direction of the incident light. Different experimental methods were used to test the predictions of the model for the gravity trap. A new method for measuring the radiation force along the beam axis in both the stable and instable regions is presented. Measurements of the radiation force on polystyrene spheres with diameters of 7.5 and 32 microns in a TEM00-mode laser beam showed a good qualitative correlation with the predictions and a slight quantitative difference. The validity of the geometrical approximations involved in the model will be discussed for spheres of different sizes and refractive indices.

Validity and reliability of the Diagnostic Adaptive Behaviour Scale.

PubMed

Tassé, M J; Schalock, R L; Balboni, G; Spreat, S; Navas, P

2016-01-01

The Diagnostic Adaptive Behaviour Scale (DABS) is a new standardised adaptive behaviour measure that provides information for evaluating limitations in adaptive behaviour for the purpose of determining a diagnosis of intellectual disability. This article presents validity evidence and reliability data for the DABS. Validity evidence was based on comparing DABS scores with scores obtained on the Vineland Adaptive Behaviour Scale, second edition. The stability of the test scores was measured using a test and retest, and inter-rater reliability was assessed by computing the inter-respondent concordance. The DABS convergent validity coefficients ranged from 0.70 to 0.84, while the test-retest reliability coefficients ranged from 0.78 to 0.95, and the inter-rater concordance as measured by intraclass correlation coefficients ranged from 0.61 to 0.87. All obtained validity and reliability indicators were strong and comparable with the validity and reliability coefficients of the most commonly used adaptive behaviour instruments. These results and the advantages of the DABS for clinician and researcher use are discussed. © 2015 MENCAP and International Association of the Scientific Study of Intellectual and Developmental Disabilities and John Wiley & Sons Ltd.

Role of the protein in the DNA sequence specificity of the cleavage site stabilized by the camptothecin topoisomerase IB inhibitor: a metadynamics study

PubMed Central

Coletta, Andrea; Desideri, Alessandro

2013-01-01

Camptothecin (CPT) is a topoisomerase IB (TopIB) selective inhibitor whose derivatives are currently used in cancer therapy. TopIB cleaves DNA at any sequence, but in the presence of CPT the only stabilized protein–DNA covalent complex is the one having a thymine in position −1 with respect to the cleavage site. A metadynamics simulation of two TopIB–DNA–CPT ternary complexes differing for the presence of a thymine or a cytosine in position −1 indicates the occurrence of two different drug’s unbinding pathways. The free-energy difference between the bound state and the transition state is large when a thymine is present in position −1 and is strongly reduced in presence of a cytosine, in line with the different drug stabilization properties of the two systems. Such a difference is strictly related to the changes in the hydrogen bond network between the protein, the DNA and the drug in the two systems, indicating a direct role of the protein in determining the specificity of the cleavage site sequence stabilized by the CPT. Calculations carried out in presence of one compound of the indenoisoquinoline family (NSC314622) indicate a comparable energy difference between the bound and the transition state independently of the presence of a thymine or a cytosine in position −1, in line with the experimental results. PMID:24003027

Positive mental health literacy: development and validation of a measure among Norwegian adolescents.

PubMed

Bjørnsen, Hanne Nissen; Eilertsen, Mary Elizabeth Bradley; Ringdal, Regine; Espnes, Geir Arild; Moksnes, Unni Karin

2017-09-18

Mental health literacy (MHL), or the knowledge and abilities necessary to benefit mental health, is a significant determinant of mental health and has the potential to benefit both individual and public mental health. MHL and its measures have traditionally focused on knowledge and beliefs about mental -ill-health rather than on mental health. No measures of MHL addressing knowledge of good or positive mental health have been identified. This study aimed to develop and validate an instrument measuring adolescents' knowledge of how to obtain and maintain good mental health and to evaluate the psychometric properties of the instrument. More specifically, the factor structure, internal and construct validity, and test-retest reliability were assessed. The participants were Norwegian upper secondary school students aged 15-21 years. The development and validation of the instrument entailed three phases: 1) item generation based on the basic psychological needs theory (BPNT), focus group interviews, and a narrative literature review, 2) a pilot study (n = 479), and 3) test-retest (n = 149), known-groups validity (n = 44), and scale construction, item reduction through principal component analysis (PCA), and confirmatory factor analysis (CFA) for factor structure and psychometric properties assessment (n = 1888). Thirty-two items were initially generated, and 15 were selected for the pilot study. PCA identified cross-loadings, and a one-factor solution was examined. After removing five problematic items, CFA yielded a satisfactory fit for a 10-item one-factor model, referred to as the mental health-promoting knowledge (MHPK-10) measure. The test-retest evaluation supported the stability of the measure. McDonald's omega was 0.84, and known-groups validity test indicated good construct validity. A valid and reliable one-dimensional instrument measuring knowledge of factors promoting good mental health among adolescents was developed. The instrument has the potential to complement current measures of MHL and may be useful when planning mental health promotion activities and evaluating public mental health education initiatives in adolescents.

Digitized Spiral Drawing: A Possible Biomarker for Early Parkinson's Disease.

PubMed

San Luciano, Marta; Wang, Cuiling; Ortega, Roberto A; Yu, Qiping; Boschung, Sarah; Soto-Valencia, Jeannie; Bressman, Susan B; Lipton, Richard B; Pullman, Seth; Saunders-Pullman, Rachel

2016-01-01

Pre-clinical markers of Parkinson's Disease (PD) are needed, and to be relevant in pre-clinical disease, they should be quantifiably abnormal in early disease as well. Handwriting is impaired early in PD and can be evaluated using computerized analysis of drawn spirals, capturing kinematic, dynamic, and spatial abnormalities and calculating indices that quantify motor performance and disability. Digitized spiral drawing correlates with motor scores and may be more sensitive in detecting early changes than subjective ratings. However, whether changes in spiral drawing are abnormal compared with controls and whether changes are detected in early PD are unknown. 138 PD subjects (50 with early PD) and 150 controls drew spirals on a digitizing tablet, generating x, y, z (pressure) data-coordinates and time. Derived indices corresponded to overall spiral execution (severity), shape and kinematic irregularity (second order smoothness, first order zero-crossing), tightness, mean speed and variability of spiral width. Linear mixed effect adjusted models comparing these indices and cross-validation were performed. Receiver operating characteristic analysis was applied to examine discriminative validity of combined indices. All indices were significantly different between PD cases and controls, except for zero-crossing. A model using all indices had high discriminative validity (sensitivity = 0.86, specificity = 0.81). Discriminative validity was maintained in patients with early PD. Spiral analysis accurately discriminates subjects with PD and early PD from controls supporting a role as a promising quantitative biomarker. Further assessment is needed to determine whether spiral changes are PD specific compared with other disorders and if present in pre-clinical PD.

Digitized Spiral Drawing: A Possible Biomarker for Early Parkinson’s Disease

PubMed Central

San Luciano, Marta; Wang, Cuiling; Ortega, Roberto A.; Yu, Qiping; Boschung, Sarah; Soto-Valencia, Jeannie; Bressman, Susan B.; Lipton, Richard B.; Pullman, Seth; Saunders-Pullman, Rachel

2016-01-01

Introduction Pre-clinical markers of Parkinson’s Disease (PD) are needed, and to be relevant in pre-clinical disease, they should be quantifiably abnormal in early disease as well. Handwriting is impaired early in PD and can be evaluated using computerized analysis of drawn spirals, capturing kinematic, dynamic, and spatial abnormalities and calculating indices that quantify motor performance and disability. Digitized spiral drawing correlates with motor scores and may be more sensitive in detecting early changes than subjective ratings. However, whether changes in spiral drawing are abnormal compared with controls and whether changes are detected in early PD are unknown. Methods 138 PD subjects (50 with early PD) and 150 controls drew spirals on a digitizing tablet, generating x, y, z (pressure) data-coordinates and time. Derived indices corresponded to overall spiral execution (severity), shape and kinematic irregularity (second order smoothness, first order zero-crossing), tightness, mean speed and variability of spiral width. Linear mixed effect adjusted models comparing these indices and cross-validation were performed. Receiver operating characteristic analysis was applied to examine discriminative validity of combined indices. Results All indices were significantly different between PD cases and controls, except for zero-crossing. A model using all indices had high discriminative validity (sensitivity = 0.86, specificity = 0.81). Discriminative validity was maintained in patients with early PD. Conclusion Spiral analysis accurately discriminates subjects with PD and early PD from controls supporting a role as a promising quantitative biomarker. Further assessment is needed to determine whether spiral changes are PD specific compared with other disorders and if present in pre-clinical PD. PMID:27732597

Healing of voids in the aluminum metallization of integrated circuit chips

NASA Technical Reports Server (NTRS)

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

1990-01-01

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

Evaluation of Animal-Based Indicators to Be Used in a Welfare Assessment Protocol for Sheep.

PubMed

Richmond, Susan E; Wemelsfelder, Francoise; de Heredia, Ina Beltran; Ruiz, Roberto; Canali, Elisabetta; Dwyer, Cathy M

2017-01-01

Sheep are managed under a variety of different environments (continually outdoors, partially outdoors with seasonal or diurnal variation, continuously indoors) and for different purposes, which makes assessing welfare challenging. This diversity means that resource-based indicators are not particularly useful and, thus, a welfare assessment scheme for sheep, focusing on animal-based indicators, was developed. We focus specifically on ewes, as the most numerous group of sheep present on farm, although many of the indicators may also have relevance to adult male sheep. Using the Welfare Quality ® framework of four Principles and 12 Criteria, we considered the validity, reliability, and feasibility of 46 putative animal-based indicators derived from the literature for these criteria. Where animal-based indicators were potentially unreliably or were not considered feasible, we also considered the resource-based indicators of access to water, stocking density, and floor slipperiness. With the exception of the criteria "Absence of prolonged thirst," we suggest at least one animal-based indicator for each welfare criterion. As a minimum, face validity was available for all indicators; however, for many, we found evidence of convergent validity and discriminant validity (e.g., lameness as measured by gait score, body condition score). The reliability of most of the physical and health measures has been tested in the field and found to be appropriate for use in welfare assessment. However, for the majority of the proposed behavioral indicators (lying synchrony, social withdrawal, postures associated with pain, vocalizations, stereotypy, vigilance, response to surprise, and human approach test), this still needs to be tested. In conclusion, the comprehensive assessment of sheep welfare through largely animal-based measures is supported by the literature through the use of indicators focusing on specific aspects of sheep biology. Further work is required for some indicators to ensure that measures are reliable when used in commercial settings.

Evaluation of Animal-Based Indicators to Be Used in a Welfare Assessment Protocol for Sheep

PubMed Central

Richmond, Susan E.; Wemelsfelder, Francoise; de Heredia, Ina Beltran; Ruiz, Roberto; Canali, Elisabetta; Dwyer, Cathy M.

2017-01-01

Sheep are managed under a variety of different environments (continually outdoors, partially outdoors with seasonal or diurnal variation, continuously indoors) and for different purposes, which makes assessing welfare challenging. This diversity means that resource-based indicators are not particularly useful and, thus, a welfare assessment scheme for sheep, focusing on animal-based indicators, was developed. We focus specifically on ewes, as the most numerous group of sheep present on farm, although many of the indicators may also have relevance to adult male sheep. Using the Welfare Quality® framework of four Principles and 12 Criteria, we considered the validity, reliability, and feasibility of 46 putative animal-based indicators derived from the literature for these criteria. Where animal-based indicators were potentially unreliably or were not considered feasible, we also considered the resource-based indicators of access to water, stocking density, and floor slipperiness. With the exception of the criteria “Absence of prolonged thirst,” we suggest at least one animal-based indicator for each welfare criterion. As a minimum, face validity was available for all indicators; however, for many, we found evidence of convergent validity and discriminant validity (e.g., lameness as measured by gait score, body condition score). The reliability of most of the physical and health measures has been tested in the field and found to be appropriate for use in welfare assessment. However, for the majority of the proposed behavioral indicators (lying synchrony, social withdrawal, postures associated with pain, vocalizations, stereotypy, vigilance, response to surprise, and human approach test), this still needs to be tested. In conclusion, the comprehensive assessment of sheep welfare through largely animal-based measures is supported by the literature through the use of indicators focusing on specific aspects of sheep biology. Further work is required for some indicators to ensure that measures are reliable when used in commercial settings. PMID:29322048

The electromagnetic environment in CFC structures

NASA Technical Reports Server (NTRS)

Hardwick, C. J.; Haigh, S. J.

1991-01-01

Extensive measurements of induced voltages and currents were made using a CFC (carbon fiber composites) horizontal stabilizer from the A320 as a test bed. The work was done to investigate the efficacy of various protection schemes to reduce the magnitudes of the induced voltages and validate a computer program INDCAL. Results indicate that a good understanding of the various induced voltage mechanisms including the long wave effect due to current redistribution was obtained.

Resilience in a reborn nation: Validation of the Lithuanian Resilience Scale for Adults (RSA).

PubMed

Hilbig, Jan; Viliūnienė, Rima; Friborg, Oddgeir; Pakalniškienė, Vilmantė; Danilevičiūtė, Vita

2015-07-01

Resilience, as an ability to withstand or rebound from crisis or adversity, is becoming an increasingly significant concept in health promotion and well-being. Individuals exhibiting resilience use skills or resources flexibly to solve situational demands. The Resilience Scale for Adults (RSA) may be used to assess protective resources, and the aim of the present study was to validate the Lithuanian translation. The translated RSA was administered to a clinical (n=125) and a non clinical sample (n=499) to examine the discriminant validity of the RSA items with a confirmatory factor analysis, the internal consistency as well as construct validity by correlating it with the Quick Psycho-Affective Symptoms Scan (QPASS). The internal consistency, the test-retest stability and the factor structure were replicated as adequate, thus indicating good psychometric properties and support of discriminant validity. Females reported more resilience resources for the domains of social competence, family cohesion and social resources compared to men. The RSA subscales correlated negatively with the QPASS scores, and patients reported significantly less resilience resources than non-patients, thus indicating construct validity. Valid psychometric tools for research purposes and routine every-day use are urgently needed in Lithuania, a young nation still under numerous challenges due to social, economic and political transitions. The RSA represents a reliable and valid tool for assessing protective factors. Assessing resilience factors may extend the understanding of factors relevant for mental health problems as well as treatment prognosis beyond the capabilities of mere symptom oriented approaches. Copyright © 2015 Elsevier Inc. All rights reserved.

Measuring suicidality using the personality assessment inventory: a convergent validity study with federal inmates.

PubMed

Patry, Marc W; Magaletta, Philip R

2015-02-01

Although numerous studies have examined the psychometric properties and clinical utility of the Personality Assessment Inventory in correctional contexts, only two studies to date have specifically focused on suicide ideation. This article examines the convergent validity of the Suicide Ideation Scale and the Suicide Potential Index on the Personality Assessment Inventory in a large, nontreatment sample of male and female federal inmates (N = 1,120). The data indicated robust validity support for both the Suicide Ideation Scale and Suicide Potential Index, which were each correlated with a broad group of validity indices representing multiple assessment modalities. Recommendations for future research to build upon these findings through replication and extension are made. © The Author(s) 2014.

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

NASA Astrophysics Data System (ADS)

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

2016-09-01

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

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

PubMed

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

2013-09-01

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

Design of a robust control law for the Vega launcher ballistic phase

NASA Astrophysics Data System (ADS)

Valli, Monica; Lavagna, Michèle R.; Panozzo, Thomas

2012-02-01

This work presents the design of a robust control law, and the related control system architecture, for the Vega launcher ballistic phase, taking into account the complete six degrees of freedom dynamics. To gain robustness a non-linear control approach has been preferred: more specifically the Lyapunov's second stability theorem has been exploited, being a very powerful tool to guarantee asymptotic stability of the controlled dynamics. The dynamics of Vega's actuators has also been taken into account. The system performance has been checked and analyzed by numerical simulations run on real mission data for different operational and configuration scenarios, and the effectiveness of the synthesized control highlighted: in particular scenarios including a wide range of composite's inertial configurations performing various typologies of maneuvers have been run. The robustness of the controlled dynamics has been validated by 100 cases Monte Carlo analysis campaign: the containment of the dispersion for the controlled variables - say the composite roll, yaw and pitch angles - confirmed the wide validity and generality of the proposed control law. This paper will show the theoretical approach and discuss the obtained results.

Translation and validation of the Canadian diabetes risk assessment questionnaire in China.

PubMed

Guo, Jia; Shi, Zhengkun; Chen, Jyu-Lin; Dixon, Jane K; Wiley, James; Parry, Monica

2018-01-01

To adapt the Canadian Diabetes Risk Assessment Questionnaire for the Chinese population and to evaluate its psychometric properties. A cross-sectional study was conducted with a convenience sample of 194 individuals aged 35-74 years from October 2014 to April 2015. The Canadian Diabetes Risk Assessment Questionnaire was adapted and translated for the Chinese population. Test-retest reliability was conducted to measure stability. Criterion and convergent validity of the adapted questionnaire were assessed using 2-hr 75 g oral glucose tolerance tests and the Finnish Diabetes Risk Scores, respectively. Sensitivity and specificity were evaluated to establish its predictive validity. The test-retest reliability was 0.988. Adequate validity of the adapted questionnaire was demonstrated by positive correlations found between the scores and 2-hr 75 g oral glucose tolerance tests (r = .343, p < .001) and with the Finnish Diabetes Risk Scores (r = .738, p < .001). The area under receiver operating characteristic curve was 0.705 (95% CI .632, .778), demonstrating moderate diagnostic value at a cutoff score of 30. The sensitivity was 73%, with a positive predictive value of 57% and negative predictive value of 78%. Our results provided evidence supporting the translation consistency, content validity, convergent validity, criterion validity, sensitivity, and specificity of the translated Canadian Diabetes Risk Assessment Questionnaire with minor modifications. This paper provides clinical, practical, and methodological information on how to adapt a diabetes risk calculator between cultures for public health nurses. © 2017 Wiley Periodicals, Inc.

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

PubMed

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

2007-11-01

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

Post-Flash Validation of the new ACS/WFC Subarrays

NASA Astrophysics Data System (ADS)

Bellini, A.; Grogin, N. A.; Lim, P. L.; Golimowski, D.

2017-05-01

We made use of the new ACS/WFC subarray images of CAL-14410, taken taken with a large range of flash exposure times (0.1-30 seconds), to probe the temporal stability of the reference flash file and to validate the current post-flash correction pipeline of CALACS and ACS DESTRIPE PLUS on the new subarray modes. No statistically-significant deviations are found between the new post-flashed subarray exposures and the flash reference file, indicating that the LED lamp used to post-flash ACS images has been stable over several years. The current calibration pipelines (both CALACS and ACS DESTRIPE PLUS can be successfully used with the new subarray modes.

French-Canadian translation and validation of four questionnaires assessing hearing impairment and handicap.

PubMed

Vincent, Claude; Gagné, Jean-Pierre; Leroux, Tony; Clothier, Audrey; Larivière, Marianne; Dumont, Frédéric S; Gendron, Martine

2017-04-01

Questionnaires evaluating hearing impairment are available in English but there is a need for French standardised questionnaires for researchers as well as for audiologists and other clinicians. The objective of this study is to describe the translation and validation of four questionnaires that assess different aspects of hearing impairment and handicap among elders with hearing loss, by comparing the main score and psychometric evaluation of original and French-Canadian (FC) versions of the World Health Organization Disability Assessment Scale II (WHO-DAS II), the Screening Test for Hearing Problems (STHP), the Abbreviated Profile of Hearing Aid Benefit (APHAB) and the Measure of Audiologic Rehabilitation Self-Efficacy for Hearing Aids (MARS-HA). Vallerand method: translation and back-translation by two translators, revision by a committee of experts and pre-tested with five bilingual older participants. Participants (n = 29) were 65 years of age or older including 21 with hearing aids. The psychometric properties (internal consistency, temporal stability after four weeks) indicate good reliability for most of the translated questionnaires and their subscales, especially the WHO-DAS II. The translations in FC of two hearing loss and two hearing aid questionnaires were validated. It is recommended to pursue the demonstration for temporal stability for the STHP.

A rapid quantification method for the screening indicator for β-thalassemia with near-infrared spectroscopy

NASA Astrophysics Data System (ADS)

Chen, Jiemei; Peng, Lijun; Han, Yun; Yao, Lijun; Zhang, Jing; Pan, Tao

2018-03-01

Near-infrared (NIR) spectroscopy combined with chemometrics was applied to rapidly analyse haemoglobin A2 (HbA2) for β-thalassemia screening in human haemolysate samples. The relative content indicator HbA2 was indirectly quantified by simultaneous analysis of two absolute content indicators (Hb and Hb • HbA2). According to the comprehensive prediction effect of the multiple partitioning of calibration and prediction sets, the parameters were optimized to achieve modelling stability, and the preferred models were validated using the samples not involved in modelling. Savitzky-Golay smoothing was firstly used for the spectral pretreatment. The absorbance optimization partial least squares (AO-PLS) was used to eliminate high-absorption wave-bands appropriately. The equidistant combination PLS (EC-PLS) was further used to optimize wavelength models. The selected optimal models were I = 856 nm, N = 16, G = 1 and F = 6 for Hb and I = 988 nm, N = 12, G = 2 and F = 5 for Hb • HbA2. Through independent validation, the root-mean-square errors and correlation coefficients for prediction (RMSEP, RP) were 3.50 g L- 1 and 0.977 for Hb and 0.38 g L- 1 and 0.917 for Hb • HbA2, respectively. The predicted values of relative percentage HbA2 were further calculated, and the calculated RMSEP and RP were 0.31% and 0.965, respectively. The sensitivity and specificity for β-thalassemia both reached 100%. Therefore, the prediction of HbA2 achieved high accuracy for distinguishing β-thalassemia. The local optimal models for single parameter and the optimal equivalent model sets were proposed, providing more models to match possible constraints in practical applications. The NIR analysis method for the screening indicator of β-thalassemia was successfully established. The proposed method was rapid, simple and promising for thalassemia screening in a large population.

Towards muscle-specific meat color stability of Chinese Luxi yellow cattle: A proteomic insight into post-mortem storage.

PubMed

Wu, Wei; Yu, Qian-Qian; Fu, Yu; Tian, Xiao-Jing; Jia, Fei; Li, Xing-Min; Dai, Rui-Tong

2016-09-16

Searching for potential predictors of meat color is a challenging task for the meat industry. In this study, the relationship between meat color parameters and the sarcoplasmic proteome of M. longissimuss lumborum (LL) and M. psoas major (PM) from Chinese Luxi yellow cattle during post-mortem storage (0, 5, 10 and 15days) were explored with the aid of the integrated proteomics and bioinformatics approaches. Meat color attributes revealed that LL displayed better color stability than PM during storage. Furthermore, sarcoplasmic proteins of these two muscles were compared between days 5, 10, 15 and day 0. Several proteins were closely correlated with meat color attributes and they were muscle-specific and responsible for the meat color stability at different storage periods. Glycerol-3-phosphate dehydrogenase, fructose-bisphosphate aldolase A isoform, glycogen phosphorylase, peroxiredoxin-2, phosphoglucomutase-1, superoxide dismutase [Cu-Zn], heat shock cognate protein (71kDa) might serve as the candidate predictors of meat color stability during post-mortem storage. In addition, bioinformatics analyses indicated that more proteins were involved in glycolytic metabolism of LL, which contributed to better meat color stability of LL than PM. The present results could provide a proteomic insight into muscle-specific meat color stability of Chinese Luxi yellow cattle during post-mortem storage. Copyright © 2015 Elsevier B.V. All rights reserved.

Quantitative characterization of non-classic polarization of cations on clay aggregate stability.

PubMed

Hu, Feinan; Li, Hang; Liu, Xinmin; Li, Song; Ding, Wuquan; Xu, Chenyang; Li, Yue; Zhu, Longhui

2015-01-01

Soil particle interactions are strongly influenced by the concentration, valence and ion species and the pH of the bulk solution, which will also affect aggregate stability and particle transport. In this study, we investigated clay aggregate stability in the presence of different alkali ions (Li+, Na+, K+, and Cs+) at concentrations from10-5 to 10-1 mol L-1. Strong specific ion effects on clay aggregate stability were observed, and showed the order Cs+>K+>Na+>Li+. We found that it was not the effects of ion size, hydration, and dispersion forces in the cation-surface interactions but strong non-classic polarization of adsorbed cations that resulted in these specific effects. In this study, the non-classic dipole moments of each cation species resulting from the non-classic polarization were estimated. By comparing non-classic dipole moments with classic values, the observed dipole moments of adsorbed cations were up to 104 times larger than the classic values for the same cation. The observed non-classic dipole moments sharply increased with decreasing electrolyte concentration. We conclude that strong non-classic polarization could significantly suppress the thickness of the diffuse layer, thereby weakening the electric field near the clay surface and resulting in improved clay aggregate stability. Even though we only demonstrated specific ion effects on aggregate stability with several alkali ions, our results indicate that these effects could be universally important in soil aggregate stability.

Quantitative Characterization of Non-Classic Polarization of Cations on Clay Aggregate Stability

PubMed Central

Hu, Feinan; Li, Hang; Liu, Xinmin; Li, Song; Ding, Wuquan; Xu, Chenyang; Li, Yue; Zhu, Longhui

2015-01-01

Soil particle interactions are strongly influenced by the concentration, valence and ion species and the pH of the bulk solution, which will also affect aggregate stability and particle transport. In this study, we investigated clay aggregate stability in the presence of different alkali ions (Li+, Na+, K+, and Cs+) at concentrations from10−5 to 10−1 mol L−1. Strong specific ion effects on clay aggregate stability were observed, and showed the order Cs+>K+>Na+>Li+. We found that it was not the effects of ion size, hydration, and dispersion forces in the cation–surface interactions but strong non-classic polarization of adsorbed cations that resulted in these specific effects. In this study, the non-classic dipole moments of each cation species resulting from the non-classic polarization were estimated. By comparing non-classic dipole moments with classic values, the observed dipole moments of adsorbed cations were up to 104 times larger than the classic values for the same cation. The observed non-classic dipole moments sharply increased with decreasing electrolyte concentration. We conclude that strong non-classic polarization could significantly suppress the thickness of the diffuse layer, thereby weakening the electric field near the clay surface and resulting in improved clay aggregate stability. Even though we only demonstrated specific ion effects on aggregate stability with several alkali ions, our results indicate that these effects could be universally important in soil aggregate stability. PMID:25874864

Measuring progress in maternal and newborn health care in Mexico: validating indicators of health system contact and quality of care.

PubMed

Blanc, Ann K; Diaz, Claudia; McCarthy, Katharine J; Berdichevsky, Karla

2016-08-30

The majority of births in Mexico take place in a health facility and are attended by a skilled birth attendant, yet maternal mortality has not declined to anticipated levels. Coverage estimates of skilled attendance and other maternal and newborn interventions often rely on women's self-report through a population-based survey, the accuracy of which is not well established. We used a facility-based design to validate women's report of skilled birth attendance, as well as other key elements of maternal, newborn intrapartum, and immediate postnatal care. Women's reports of labor and delivery care were collected by exit interview prior to hospital discharge and were compared against direct observation by a trained third party in a Mexican public hospital (n = 597). For each indicator, validity was assessed at the individual level using the area under the receiver operating curve (AUC) and at the population level using the inflation factor (IF). Five of 47 indicators met both validation criteria (AUC > 0.60 and 0.75 < IF < 1.25): urine sample screen, injection or IV medication received during labor, before the birth of the baby (i.e., uterotonic for either induction or augmentation of labor), episiotomy, excessive bleeding, and receipt of blood products. An additional 9 indicators met criteria for the AUC and 18 met criteria for the IF. A skilled attendant indicator had high sensitivity (90.1 %: 95 % CI: 87.1-92.5 %), low specificity (14.0 %: 95 % CI: 5.8-26.7 %) and was suitable for population-level estimation only. Women are able to give valid reports on some aspects of the content of care, although questions regarding the indication for interventions are less likely to be known. Questions that include technical terms or refer to specific time periods tended to have lower response levels. A key aspect of efforts to improve maternal and newborn health requires valid measurement of women's access to maternal and newborn health interventions and the quality of such services. Additional work on improving measurement of population coverage indicators is warranted.

ISO/IEC 17025 Sysmex R-500 hematology reticulocyte analyzer validation.

PubMed

Dimopoulou, H A; Theodoridis, T; Galea, V; Christopoulou-Cokkinou, V; Spyridaki, M-H E; Georgakopoulos, C G

2007-01-01

The Sysmex R-500 (R-500) Hematology Analyzer is a bench-top system appropriate for the analysis of limited batches of blood samples. The R-500 provides percentage proportional (RET%), absolute reticulocyte (RET#), and absolute red blood cell (RBC#) counts. The system was validated at the Doping Control Laboratory of Athens, according to the International Committee for Standardization in Hematology, International Standards Organization (ISO/IEC) 17025, and World Antidoping Agency (WADA) specifications. The instrument calibration was performed according to the manufacturer and validation parameters comprised linearity, precision, uncertainty (intermediate and long-term precision), comparability, effect of drift, carryover, stability, and accuracy. The linearity and the comparability studies for RET#, RET%, and RBC# were expressed in regression factors (R2) and coefficients of correlation [r(x, y)], respectively. For the precision studies, the coefficients of variation for RET#, RET%, and RBC# were 9.49%, 9.83%, and <1.5%, respectively. For the intermediate precision studies, the coefficients of variation for RET#, RET%, and RBC# were 3.1%, 3.6%, and 0.6%, respectively. Carryover was found to be negligible. Sample stability was demonstrated at both room temperature and at 4 degrees C over a 24-hour period. Comparability studies for the R-500 were performed using a Sysmex SE-9500. The total evaluation led to the conclusion that the R-500 is an accurate and precise analyzer and because of to its relatively limited size, it can be considered a portable instrument, capable to be used in sports competition and training sites, where doping control and health tests are conducted. The analytical methodology of RET% measurement by the R-500 has been incorporated into the Doping Control Laboratory of Athens' Scope of Accreditation according to the ISO/IEC 17025 and WADA specifications.

Validity Evidence for Games as Assessment Environments. CRESST Report 773

ERIC Educational Resources Information Center

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

2010-01-01

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

Evaluation of thermal expansion coefficient of carbon fiber reinforced composites using electronic speckle interferometry.

PubMed

Dong, Chengzhi; Li, Kai; Jiang, Yuxi; Arola, Dwayne; Zhang, Dongsheng

2018-01-08

An optical system for measuring the coefficient of thermal expansion (CTE) of materials has been developed based on electronic speckle interferometry. In this system, the temperature can be varied from -60°C to 180°C with a Peltier device. A specific specimen geometry and an optical arrangement based on the Michelson interferometer are proposed to measure the deformation along two orthogonal axes due to temperature changes. The advantages of the system include its high sensitivity and stability over the whole range of measurement. The experimental setup and approach for estimating the CTE was validated using an Aluminum alloy. Following this validation, the system was applied for characterizing the CTE of carbon fiber reinforced composite (CFRP) laminates. For the unidirectional fiber reinforced composites, the CTE varied with fiber orientation and exhibits anisotropic behavior. By stacking the plies with specific angles and order, the CTE of a specific CFRP was constrained to a low level with minimum variation temperature. The optical system developed in this study can be applied to CTE measurement for engineering and natural materials with high accuracy.

Mass spectrometric characterization of the hypoxia-inducible factor (HIF) stabilizer drug candidate BAY 85-3934 (molidustat) and its glucuronidated metabolite BAY-348, and their implementation into routine doping controls.

PubMed

Dib, Josef; Mongongu, Cynthia; Buisson, Corinne; Molina, Adeline; Schänzer, Wilhelm; Thuss, Uwe; Thevis, Mario

2017-01-01

The development of new therapeutics potentially exhibiting performance-enhancing properties implicates the risk of their misuse by athletes in amateur and elite sports. Such drugs necessitate preventive anti-doping research for consideration in sports drug testing programmes. Hypoxia-inducible factor (HIF) stabilizers represent an emerging class of therapeutics that allows for increasing erythropoiesis in patients. BAY 85-3934 is a novel HIF stabilizer, which is currently undergoing phase-2 clinical trials. Consequently, the comprehensive characterization of BAY 85-3934 and human urinary metabolites as well as the implementation of these analytes into routine doping controls is of great importance. The mass spectrometric behaviour of the HIF stabilizer drug candidate BAY 85-3934 and a glucuronidated metabolite (BAY-348) were characterized by electrospray ionization-(tandem) mass spectrometry (ESI-MS(/MS)) and multiple-stage mass spectrometry (MS n ). Subsequently, two different laboratories established different analytical approaches (one each) enabling urine sample analyses by employing either direct urine injection or solid-phase extraction. The methods were cross-validated for the metabolite BAY-348 that is expected to represent an appropriate target analyte for human urine analysis. Two test methods allowing for the detection of BAY-348 in human urine were applied and cross-validated concerning the validation parameters specificity, linearity, lower limit of detection (LLOD; 1-5 ng/mL), ion suppression/enhancement (up to 78%), intra- and inter-day precision (3-21%), recovery (29-48%), and carryover. By means of ten spiked test urine samples sent blinded to one of the participating laboratories, the fitness-for-purpose of both assays was provided as all specimens were correctly identified applying both testing methods. As no post-administration study samples were available, analyses of authentic urine specimens remain desirable. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

ICH guidance in practice: validated reversed-phase HPLC method for the determination of active mangiferin from extracts of Mangifera indica Linn.

PubMed

Gowda, Nagaraj; Kumar, Pradeep; Panghal, Surender; Rajshree, Mashru

2010-02-01

This study presents the development and validation of a reversed-phase liquid chromatographic method for the determination of mangiferin (MGN) in alcoholic extracts of mangifera indica. A Lichrospher 100 C(18)-ODS (250 x 4.6 mm, 5 microm size) (Merck, Whitehouse Station, NJ) prepacked column and a mobile phase of potassium dihydrogen orthophosphate (0.01M) pH 2.7 +/- 0.2-acetonitrile (15:85, v/v) with the flow rate of 1 mL/min was used. MGN detection was achieved at a wavelength monitored at 254 nm with SPD-M 10A vp PDA detector or SPD 10AD vp UV detector in combination with class LC 10A software. The proposed method was validated as prescribed by International Conference on Harmonization (ICH) with respect to linearity, specificity, accuracy, precision, stability, and quantification. The method validation was realized using alcoholic extracts and raw materials of leaves and barks. All the validation parameters were within the acceptable limits, and the developed analytical method can successfully be applied for MGN determination.

Photosynthetic characteristics and estimated growth rates indicate grazing is the proximate control of primary production in the equatorial Pacific

NASA Technical Reports Server (NTRS)

Cullen, John J.; Lewis, Marlon R.; Davis, Curtiss O.; Barber, Richard T.

1992-01-01

Macronutrients persist in the surface layer of the equatorial Pacific because the production of phytoplankton is limited; the nature of this limitation has yet to be resolved. Measurements of photosynthesis as a function of irradiance (P-I) provide information on the control of primary productivity, a question of great biogeochemical importance. Accordingly, P-I was measured in the equatorial Pacific along 150 deg W, during February-March 1988. Diel variability of P-I showed a pattern consistent with nocturnal vertical mixing in the upper 20 m followed by diurnal stratification, causing photoinhibition near the surface at midday. Otherwise, the distribution of photosynthetic parameters with depth and the stability of P-I during simulated in situ incubations over 2 days demonstrated that photoadaptation was nearly complete at the time of sampling: photoadaptation had not been effectively countered by upwelling or vertical mixing. Measurements of P-I and chlorophyll during manipulations of trace elements showed that simple precautions to minimize contamination were sufficient to obtain valid rate measurements and that the specific growth rates of phytoplankton were fairly high in situ, a minimum of 0.6/d. Diel variability of beam attenuation also indicated high specific growth rates of phytoplankton and a strong coupling of production with grazing. It appears that grazing is the proximate control on the standing crop of phytoplankton. Nonetheless, the supply of a trace nutrient such as iron might ultimately regulate productivity by influencing species composition and food-web structure.

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

DTIC Science & Technology

2001-07-01

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

Utility measures of health-related quality of life in patients treated for benign paroxysmal positional vertigo.

PubMed

Roberts, Richard A; Abrams, Harvey; Sembach, Melanie K; Lister, Jennifer J; Gans, Richard E; Chisolm, Theresa Hnath

2009-06-01

Comparing the effects of different disorders and interventions on health-related quality of life (HRQoL) is important for healthcare policy and accountability. There are two basic approaches to measure HRQoL: questionnaires derived from psychometrics and preference-based measures or utilities derived from econometrics. While disease-specific HRQoL questionnaires, such as the Dizziness Handicap Inventory (DHI), are important because they focus on the impact of a specific problem and its treatments (i.e., vestibular disorders), economic comparisons of the impacts of diseases/disorders and their treatments are typically based on utility assessment. The utility measures for audiology application (UMAA) were developed to measure utilities for various audiologic conditions using a standard computer. The purpose of this study was to determine if the UMAA provides stable, valid, and sensitive utility measures of the effects of benign paroxysmal positional vertigo (BPPV) and its treatment on HRQoL. It was hypothesized that utilities, as measured by the UMAA, would indicate improvement in HRQoL post-treatment for BPPV comparable to a disease-specific health status measure (DHI). The UMAA incorporates three techniques to measure utility: rating scale, standard gamble, and time tradeoff. A utility is a cardinal measure of strength of preference and is measured on a continuum basis from 0.0 (incapacitating dizziness) to 1.0 (no dizziness). Fifty-two adults with BPPV of the posterior semicircular canal completed the UMAA and DHI before treatment and again post-treatment. A subgroup of 15 participants completed the UMAA on two occasions before treatment to assess test-retest stability and to establish critical difference values. Results from this investigation demonstrate that utilities as measured through the UMAA are stable, valid, and comparable to the DHI. Post-treatment utilities were also significantly higher than pretreatment utilities, indicating that the utilities, as measured through the UMAA, are sensitive to improvement in HRQoL after BPPV treatment. Utilities as measured through the UMAA seem sensitive to changes in HRQoL after treatment of BPPV. Since the UMAA can be used to measure patient preference (i.e., utility), it may be useful for comparison of specific audiologic conditions, such as BPPV, to nonaudiologic conditions, such as cardiovascular disease and kidney disease.

Further Validation of the Conner's Adult Attention Deficit/Hyperactivity Rating Scale Infrequency Index (CII) for Detection of Non-Credible Report of Attention Deficit/Hyperactivity Disorder Symptoms.

PubMed

Cook, Carolyn M; Bolinger, Elizabeth; Suhr, Julie

2016-06-01

Attention deficit/hyperactivity disorder (ADHD) can be easily presented in a non-credible manner, through non-credible report of ADHD symptoms and/or by non-credible performance on neuropsychological tests. While most studies have focused on detection of non-credible performance using performance validity tests, there are few studies examining the ability to detect non-credible report of ADHD symptoms. We provide further validation data for a recently developed measure of non-credible ADHD symptom report, the Conner's Adult ADHD Rating Scales (CAARS) Infrequency Index (CII). Using archival data from 86 adults referred for concerns about ADHD, we examined the accuracy of the CII in detecting extreme scores on the CAARS and invalid reporting on validity indices of the Minnesota Multiphasic Personality Inventory-2 Restructured Format (MMPI-2-RF). We also examined the accuracy of the CII in detecting non-credible performance on standalone and embedded performance validity tests. The CII was 52% sensitive to extreme scores on CAARS DSM symptom subscales (with 97% specificity) and 20%-36% sensitive to invalid responding on MMPI-2-RF validity scales (with near 90% specificity), providing further evidence for the interpretation of the CII as an indicator of non-credible ADHD symptom report. However, the CII detected only 18% of individuals who failed a standalone performance validity test (Word Memory Test), with 87.8% specificity, and was not accurate in detecting non-credible performance using embedded digit span cutoffs. Future studies should continue to examine how best to assess for non-credible symptom report in ADHD referrals. © The Author 2016. Published by Oxford University Press. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

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

PubMed

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

2015-01-01

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

Validation of a Self-Report Questionnaire Assessing the Bodily and Physiological Sensations of Orgasm.

PubMed

Dubray, Samantha; Gérard, Marina; Beaulieu-Prévost, Dominic; Courtois, Frédérique

2017-02-01

Despite a plethora of research on sexual functioning during the past decades, the field is still lacking standardized measurements specifically characterizing orgasm. Although several validated tools are available to assess sexual function in healthy and clinical populations, items on orgasm are limited to frequency or dichotomous responses. A neurophysiologic model of orgasm developed from previous research in able-bodied and spinally injured populations offers a promising framework for the construction of a new questionnaire. To develop and validate a brief self-report measurement of orgasm by the assessment of bodily and physiologic sensations perceived during climax by able-bodied individuals. Although the currently available tool focuses on the phenomenological sensations associated with climax, the goal of this questionnaire was to capture the more specific genital and extragenital sensations associated with orgasm. The current Bodily Sensations of Orgasm questionnaire and the Orgasm Rating Scale. Data from previous research conducted on individuals with spinal cord injury and the available empirical literature provided a pool of 45 items organized into four categories, which were reviewed by an expert panel. Upon review, a 28-item questionnaire was created and administered to a community sample of 227 participants, including men and women, 18 to 73 years old. Exploratory factor analyses supported the four-factor model, in which orgasm is comprised of extragenital sensations, genital sensations and spasms, nociceptive sensations, and sweating responses. Overall, a high degree of internal consistency was found for the final 22-item questionnaire (Cronbach α = 0.87), with individual reliability coefficients showing moderate to high internal consistency (r = 0.65-0.79) for each dimension. Overall temporal stability of the measurement was acceptable (r = 0.74). Using the Orgasm Rating Scale, satisfying convergent validity was confirmed, thereby indicating that the two measurements are complementary. The Bodily Sensations of Orgasm questionnaire allows for a brief evaluation of the physical and physiologic sensations associated with orgasm. Findings also suggest perceptual differences between men and women with regard to climax, with women reporting a larger repertoire of climactic sensations during orgasm. Copyright © 2016 International Society for Sexual Medicine. Published by Elsevier Inc. All rights reserved.

Fitness-Specific Epistemic Beliefs, Effort Regulation, Outcomes, and Indices of Motivation in High School Physical Education

ERIC Educational Resources Information Center

Lodewyk, Ken R.; Gao, Zan

2013-01-01

Epistemic beliefs are deeply held convictions about the nature of knowledge, knowing, and learning. In this study, approximately 500 ninth and tenth-grade physical education (PE) students completed fitness-specific measures assessing their epistemic beliefs in the simplicity and stability of knowledge and the speed of its acquisition along with…

Development and validation of a hydrophilic interaction chromatography-mass spectrometry assay for taurine and methionine in matrices rich in carbohydrates.

PubMed

de Person, Marine; Hazotte, Aurélie; Elfakir, Claire; Lafosse, Michel

2005-07-22

A new procedure based on hydrophilic interaction chromatography coupled to tandem mass spectrometry (ionisation process by pneumatically assisted electrospray in negative ion mode), is developed and validated for the simultaneous determination of underivatised taurine and methionine in beverages rich in carbohydrates such as energy drinks. No initial clean-up procedure and no sample derivatisation are required. Satisfactory analysis was obtained on an Astec apHera NH2 (150 mm x 4.6 mm; 5 microm) column with methanol-water (60/40) as mobile phase. The method was validated in terms of specificity, detection limits, linearity, accuracy, precision and stability, using threonine as internal standard. The potential effects of matrix and endogenous amino acid content were also examined. The limits of detection in the beverage varied from 20 microg L(-1) for taurine to 50 micro L(-1) for methionine.

Experimental and theoretical studies of the colloidal stability of nanoparticles-a general interpretation based on stability maps.

PubMed

Segets, Doris; Marczak, Renata; Schäfer, Stefan; Paula, Carolin; Gnichwitz, Jan-Frederik; Hirsch, Andreas; Peukert, Wolfgang

2011-06-28

The current work addresses the understanding of the stabilization of nanoparticles in suspension. Specifically, we study ZnO in ethanol for which the influence of particle size and reactant ratio as well as surface coverage on colloidal stability in dependence of the purification progress was investigated. The results revealed that the well-known ζ-potential determines not only the colloidal stability but also the surface coverage of acetate groups bound to the particle surface. The acetate groups act as molecular spacers between the nanoparticles and prevent agglomeration. Next to DLVO calculations based on the theory of Derjaguin, Landau, Verwey and Overbeek using a core-shell model we find that the stability is better understood in terms of dimensionless numbers which represent attractive forces as well as electrostatic repulsion, steric effects, transport properties, and particle concentration. Evaluating the colloidal stability in dependence of time by means of UV-vis absorption measurements a stability map for ZnO is derived. From this map it becomes clear that the dimensionless steric contribution to colloidal stability scales with a stability parameter including dimensionless repulsion and attraction as well as particle concentration and diffusivity of the particles according to a power law with an exponent of -0.5. Finally, we show that our approach is valid for other stabilizing molecules like cationic dendrons and is generally applicable for a wide range of other material systems within the limitations of vanishing van der Waals forces in refractive index matched situations, vanishing ζ-potential and systems without a stabilizing shell around the particle surface.

[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.

The 406 MHz ELT/EPIRBs. [Emergency Locator Transmitters/Emergency Position Indicating Radio Beacons (ELT/EPIRB)

NASA Technical Reports Server (NTRS)

Flatow, F. S.; Gal, C.; Hayes, E. J.

1984-01-01

Specifications for the COSPAS/SARSAT beacons are presented and related design considerations are discussed. Critical design aspects having significant impact on cost and performance are highlighted. Among these is the oscillator, whose frequency drift specifications require stabilization by ovens or digital control. Design options are presented and their impact on cost and performance assessed. Beacon designs developed to meet COSPAS/SARSAT specifications are shown.

Aeroservoelastic Model Validation and Test Data Analysis of the F/A-18 Active Aeroelastic Wing

NASA Technical Reports Server (NTRS)

Brenner, Martin J.; Prazenica, Richard J.

2003-01-01

Model validation and flight test data analysis require careful consideration of the effects of uncertainty, noise, and nonlinearity. Uncertainty prevails in the data analysis techniques and results in a composite model uncertainty from unmodeled dynamics, assumptions and mechanics of the estimation procedures, noise, and nonlinearity. A fundamental requirement for reliable and robust model development is an attempt to account for each of these sources of error, in particular, for model validation, robust stability prediction, and flight control system development. This paper is concerned with data processing procedures for uncertainty reduction in model validation for stability estimation and nonlinear identification. F/A-18 Active Aeroelastic Wing (AAW) aircraft data is used to demonstrate signal representation effects on uncertain model development, stability estimation, and nonlinear identification. Data is decomposed using adaptive orthonormal best-basis and wavelet-basis signal decompositions for signal denoising into linear and nonlinear identification algorithms. Nonlinear identification from a wavelet-based Volterra kernel procedure is used to extract nonlinear dynamics from aeroelastic responses, and to assist model development and uncertainty reduction for model validation and stability prediction by removing a class of nonlinearity from the uncertainty.

Optimization of Processing Parameters for Extraction of Amylase Enzyme from Dragon (Hylocereus polyrhizus) Peel Using Response Surface Methodology

PubMed Central

Abdul Manap, Mohd Yazid; Zohdi, Norkhanani

2014-01-01

The main goal of this study was to investigate the effect of extraction conditions on the enzymatic properties of thermoacidic amylase enzyme derived from dragon peel. The studied extraction variables were the buffer-to-sample (B/S) ratio (1 : 2 to 1 : 6, w/w), temperature (−18°C to 25°), mixing time (60 to 180 seconds), and the pH of the buffer (2.0 to 8.0). The results indicate that the enzyme extraction conditions exhibited the least significant (P < 0.05) effect on temperature stability. Conversely, the extraction conditions had the most significant (P < 0.05) effect on the specific activity and pH stability. The results also reveal that the main effect of the B/S ratio, followed by its interaction with the pH of the buffer, was significant (P < 0.05) among most of the response variables studied. The optimum extraction condition caused the amylase to achieve high enzyme activity (648.4 U), specific activity (14.2 U/mg), temperature stability (88.4%), pH stability (85.2%), surfactant agent stability (87.2%), and storage stability (90.3%). PMID:25050403

Fuzzy-logic based strategy for validation of multiplex methods: example with qualitative GMO assays.

PubMed

Bellocchi, Gianni; Bertholet, Vincent; Hamels, Sandrine; Moens, W; Remacle, José; Van den Eede, Guy

2010-02-01

This paper illustrates the advantages that a fuzzy-based aggregation method could bring into the validation of a multiplex method for GMO detection (DualChip GMO kit, Eppendorf). Guidelines for validation of chemical, bio-chemical, pharmaceutical and genetic methods have been developed and ad hoc validation statistics are available and routinely used, for in-house and inter-laboratory testing, and decision-making. Fuzzy logic allows summarising the information obtained by independent validation statistics into one synthetic indicator of overall method performance. The microarray technology, introduced for simultaneous identification of multiple GMOs, poses specific validation issues (patterns of performance for a variety of GMOs at different concentrations). A fuzzy-based indicator for overall evaluation is illustrated in this paper, and applied to validation data for different genetically modified elements. Remarks were drawn on the analytical results. The fuzzy-logic based rules were shown to be applicable to improve interpretation of results and facilitate overall evaluation of the multiplex method.

Psychometric evaluation of commonly used game-specific skills tests in rugby: A systematic review

PubMed Central

Oorschot, Sander; Chiwaridzo, Matthew; CM Smits-Engelsman, Bouwien

2017-01-01

Objectives To (1) give an overview of commonly used game-specific skills tests in rugby and (2) evaluate available psychometric information of these tests. Methods The databases PubMed, MEDLINE CINAHL and Africa Wide information were systematically searched for articles published between January 1995 and March 2017. First, commonly used game-specific skills tests were identified. Second, the available psychometrics of these tests were evaluated and the methodological quality of the studies assessed using the Consensus-based Standards for the selection of health Measurement Instruments checklist. Studies included in the first step had to report detailed information on the construct and testing procedure of at least one game-specific skill, and studies included in the second step had additionally to report at least one psychometric property evaluating reliability, validity or responsiveness. Results 287 articles were identified in the first step, of which 30 articles met the inclusion criteria and 64 articles were identified in the second step of which 10 articles were included. Reactive agility, tackling and simulated rugby games were the most commonly used tests. All 10 studies reporting psychometrics reported reliability outcomes, revealing mainly strong evidence. However, all studies scored poor or fair on methodological quality. Four studies reported validity outcomes in which mainly moderate evidence was indicated, but all articles had fair methodological quality. Conclusion Game-specific skills tests indicated mainly high reliability and validity evidence, but the studies lacked methodological quality. Reactive agility seems to be a promising domain, but the specific tests need further development. Future high methodological quality studies are required in order to develop valid and reliable test batteries for rugby talent identification. Trial registration number PROSPERO CRD42015029747. PMID:29259812

Parental Flooding During Conflict: A Psychometric Evaluation of a New Scale

PubMed Central

Del Vecchio, Tamara; Lorber, Michael F.; Slep, Amy M. Smith; Malik, Jill; Heyman, Richard E.; Foran, Heather M.

2016-01-01

Parents who are overwhelmed by the intensity and aversive nature of child negative affect — those who are experiencing flooding — may be less likely to react effectively and instead may focus on escaping the aversive situation, disciplining either overly permissively or punitively to escape quickly from child negative affect. However, there are no validated self-report measures of the degree to which parents experience flooding, impeding the exploration of these relations. Thus, we created and evaluated the Parent Flooding scale (PFS), assessing the extent to which parents believe their children's negative affect during parent-child conflicts is unexpected, overwhelming and distressing. We studied its factorial validity, reliability, and concurrent validity in a community sample of 453 couples with 3- to 7-year-old children (51.9% girls) recruited via random digit dialing. Confirmatory factor analyses indicated a one-factor solution with excellent internal consistency. Test-retest stability over an average of 5.6 months was high. Concurrent validity was suggested by the associations of flooding with parents’ aggression toward their children, overreactive and lax discipline, parenting satisfaction, and parents’ anger, as well as with child externalizing behavior and negative affect. Incrementally concurrent validity analyses indicated that flooding was a unique predictor of mothers’ and fathers’ overreactive discipline and fathers’ parent-child aggression and lax discipline, over and above the contributions of parents’ anger and children's negative affect. The present results support the psychometric validity of the PFS. PMID:26909682

Cross-cultural adaptation and validation of the Peripheral Artery Questionnaire: Korean version for patients with peripheral vascular diseases.

PubMed

Lee, Ji Hyun; Cho, Kyoung Im; Spertus, John; Kim, Seong Man

2012-08-01

The Peripheral Artery Questionnaire (PAQ), as developed in US English, is a validated scale to evaluate the health status of patients with peripheral artery disease (PAD). The aim of this study was to translate the PAQ into Korean and to evaluate its reliability and validity. A multi-step process of forward-translation, reconciliation, consultation with the developer, back-translation and proofreading was conducted. The test-retest reliability was evaluated at a 2-week interval using the intra-class correlation coefficient (ICC). The validity was assessed by identifying associations between Korean PAQ (KPAQ) scores and Korean Health Assessment Questionnaire (KHAQ) scores. A total of 100 PAD patients were enrolled: 63 without and 37 with severe claudication. The reliability of the KPAQ was adequate, with an ICC of 0.71. There were strong correlations between KPAQ's subscales. Cronbach's alpha for the summary score was 0.94, indicating good internal consistency and congruence with the original US version. The validity was supported by a significant correlation between the total KHAQ score and KPAQ physical function, stability, symptom, social limitation and quality of life scores (r = -0.24 to -0.90; p < 0.001) as well as between the KHAQ walking subscale and the KPAQ physical function score (r = -0.55, p < 0.001). Our results indicate that the KPAQ is a reliable, valid instrument to evaluate the health status of Korean patients with PAD.

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

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

PubMed Central

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

2017-01-01

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

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.

On-Line Robust Modal Stability Prediction using Wavelet Processing

NASA Technical Reports Server (NTRS)

Brenner, Martin J.; Lind, Rick

1998-01-01

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

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…

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.

Molecular insights into the mechanism of thermal stability of actinomycete mannanase.

PubMed

Kumagai, Yuya; Uraji, Misugi; Wan, Kun; Okuyama, Masayuki; Kimura, Atsuo; Hatanaka, Tadashi

2016-09-01

Streptomyces thermolilacinus mannanase (StMan), which requires Ca(2+) for its enhanced thermal stability and hydrolysis activity, possesses two Ca(2+) -binding sites in loop6 and loop7. We evaluated the function of the Ca(2+) -binding site in loop7 and the hydrogen bond between residues Ser247 in loop6 and Asp279 in loop7. The Ca(2+) -binding in loop7 was involved only in thermal stability. Mutations of Ser247 or Asp279 retained the Ca(2+) -binding ability; however, mutants showed less thermal stability than StMan. Phylogenetic analysis indicated that most glycoside hydrolase family 5 subfamily 8 mannanases could be stabilized by Ca(2+) ; however, the mechanism of StMan thermal stability was found to be quite specific in some actinomycete mannanases. © 2016 Federation of European Biochemical Societies.

Stability of HAMLET--a kinetically trapped alpha-lactalbumin oleic acid complex.

PubMed

Fast, Jonas; Mossberg, Ann-Kristin; Svanborg, Catharina; Linse, Sara

2005-02-01

The stability toward thermal and urea denaturation was measured for HAMLET (human alpha-lactalbumin made lethal to tumor cells) and alpha-lactalbumin, using circular dichroism and fluorescence spectroscopy as well as differential scanning calorimetry. Under all conditions examined, HAMLET appears to have the same or lower stability than alpha-lactalbumin. The largest difference is seen for thermal denaturation of the calcium free (apo) forms, where the temperature at the transition midpoint is 15 degrees C lower for apo HAMLET than for apo alpha-lactalbumin. The difference becomes progressively smaller as the calcium concentration increases. Denaturation of HAMLET was found to be irreversible. Samples of HAMLET that have been renatured after denaturation have lost the specific biological activity toward tumor cells. Three lines of evidence indicate that HAMLET is a kinetic trap: (1) It has lower stability than alpha-lactalbumin, although it is a complex of alpha-lactalbumin and oleic acid; (2) its denaturation is irreversible and HAMLET is lost after denaturation; (3) formation of HAMLET requires a specific conversion protocol.

An application of the LC-LSTM framework to the self-esteem instability case.

PubMed

Alessandri, Guido; Vecchione, Michele; Donnellan, Brent M; Tisak, John

2013-10-01

The present research evaluates the stability of self-esteem as assessed by a daily version of the Rosenberg (Society and the adolescent self-image, Princeton University Press, Princeton, 1965) general self-esteem scale (RGSE). The scale was administered to 391 undergraduates for five consecutive days. The longitudinal data were analyzed using the integrated LC-LSTM framework that allowed us to evaluate: (1) the measurement invariance of the RGSE, (2) its stability and change across the 5-day assessment period, (3) the amount of variance attributable to stable and transitory latent factors, and (4) the criterion-related validity of these factors. Results provided evidence for measurement invariance, mean-level stability, and rank-order stability of daily self-esteem. Latent state-trait analyses revealed that variances in scores of the RGSE can be decomposed into six components: stable self-esteem (40 %), ephemeral (or temporal-state) variance (36 %), stable negative method variance (9 %), stable positive method variance (4 %), specific variance (1 %) and random error variance (10 %). Moreover, latent factors associated with daily self-esteem were associated with measures of depression, implicit self-esteem, and grade point average.

Stability analysis of implicit time discretizations for the Compton-scattering Fokker-Planck equation

NASA Astrophysics Data System (ADS)

Densmore, Jeffery D.; Warsa, James S.; Lowrie, Robert B.; Morel, Jim E.

2009-09-01

The Fokker-Planck equation is a widely used approximation for modeling the Compton scattering of photons in high energy density applications. In this paper, we perform a stability analysis of three implicit time discretizations for the Compton-Scattering Fokker-Planck equation. Specifically, we examine (i) a Semi-Implicit (SI) scheme that employs backward-Euler differencing but evaluates temperature-dependent coefficients at their beginning-of-time-step values, (ii) a Fully Implicit (FI) discretization that instead evaluates temperature-dependent coefficients at their end-of-time-step values, and (iii) a Linearized Implicit (LI) scheme, which is developed by linearizing the temperature dependence of the FI discretization within each time step. Our stability analysis shows that the FI and LI schemes are unconditionally stable and cannot generate oscillatory solutions regardless of time-step size, whereas the SI discretization can suffer from instabilities and nonphysical oscillations for sufficiently large time steps. With the results of this analysis, we present time-step limits for the SI scheme that prevent undesirable behavior. We test the validity of our stability analysis and time-step limits with a set of numerical examples.

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.

Brief screening for mild cognitive impairment: validation of the Brazilian version of the Montreal cognitive assessment.

PubMed

Memória, Cláudia M; Yassuda, Mônica S; Nakano, Eduardo Y; Forlenza, Orestes V

2013-01-01

The Montreal Cognitive Assessment (MoCA) is a brief cognitive schedule that has been developed for the screening of patients with Mild Cognitive Impairment (MCI). MCI is recognized as a high-risk state for Alzheimer's disease. The aim of the present study is to examine the reliability and validity of the Brazilian version of the MoCA test (MoCA-BR) in a sample of older individuals with at least 4 years of education. The MoCA-BR was administered to 112 older adults who were classified into three diagnostic groups according to their cognitive state (Alzheimer's disease, n = 28; MCI, n = 43; normal controls, n = 41). This procedure was based on clinical and neuropsychological data. The performance in the MoCA-BR was compared with the Mini-mental state examination (MMSE) and the Cambridge Cognitive Examination. Diagnostic accuracy was examined with the receiver operating characteristic (ROC) curve analyses. Cronbach's alpha for the MoCA-BR was 0.75. Temporal stability (retesting after 3 months) using intraclass correlation coefficient was 0.75 (p < 0.001). The sensitivity and specificity of the MoCA-BR for MCI were 81% and 77%, respectively, with a cut-off score of 25 points. The area under the ROC curve for predicting MCI was 0.82 ± 0.06. The present results indicate that the MoCA-BR maintains its core diagnostic properties rendering it a valid and reliable tool for the screening of MCI among older individuals with at least 4 years of education. Copyright © 2012 John Wiley & Sons, Ltd.

Trait sexual motivation questionnaire: concept and validation.

PubMed

Stark, Rudolf; Kagerer, Sabine; Walter, Bertram; Vaitl, Dieter; Klucken, Tim; Wehrum-Osinsky, Sina

2015-04-01

Trait sexual motivation defines a psychological construct that reflects the long-lasting degree of motivation for sexual activities, which is assumed to be the result of biological and sociocultural influences. With this definition, it shares commonalities with other sexuality-related constructs like sexual desire, sexual drive, sexual needs, and sexual compulsivity. The Trait Sexual Motivation Questionnaire (TSMQ) was developed in order to measure trait sexual motivation with its different facets. Several steps were conducted: First, items were composed assessing sexual desire, the effort made to gain sex, as well as specific sexual behaviors. Factor analysis of the data of a first sample (n = 256) was conducted. Second, the factor solution was verified by a confirmatory factor analysis in a second sample (n = 498) and construct validity was demonstrated. Third, the temporal stability of the TSMQ was tested in a third study (n = 59). Questionnaire data. The exploratory and confirmatory factor analyses revealed that trait sexual motivation is best characterized by four subscales: Solitary Sexuality, Importance of Sex, Seeking Sexual Encounters, and Comparison with Others. It could be shown that the test quality of the questionnaire is high. Most importantly for the trait concept, the retest reliability after 1 year was r = 0.87. Our results indicate that the TSMQ is indeed a suitable tool for measuring long-lasting sexual motivation with high test quality and high construct validity. A future differentiation between trait and state sexual motivation might be helpful for clinical as well as forensic research. © 2015 International Society for Sexual Medicine.

Weight concerns scale applied to college students: comparison between pencil-and-paper and online formats.

PubMed

Dias, Juliana Chioda Ribeiro; Maroco, João; Campos, Juliana Alvares Duarte Bonini

2015-03-01

Online data collection is becoming increasingly common and has some advantages compared to traditional paper-and-pencil formats, such as reducing loss of data, increasing participants' privacy, and decreasing the effect of social desirability. However, the validity and reliability of this administration format must be established before results can be considered acceptable. The aim of this study was to evaluate the validity, reliability, and equivalence of paper-and-pencil and online versions of the Weight Concerns Scale (WCS) when applied to Brazilian university students. A crossover design was used, and the Portuguese version of the WCS (in both paper-and-pencil and online formats) was completed by 100 college students. The results indicated adequate fit in both formats. The simultaneous fit of data for both groups was excellent, with strong invariance between models. Adequate convergent validity, internal consistency, and mean score equivalence of the WCS in both formats were observed. Thus, the WCS presented adequate reliability and validity in both administration formats, with equivalence/stability between answers.

Dependence and physical exercise: Spanish validation of the Exercise Dependence Scale-Revised (EDS-R).

PubMed

Sicilia, Alvaro; González-Cutre, David

2011-05-01

The purpose of this study was to validate the Spanish version of the Exercise Dependence Scale-Revised (EDS-R). To achieve this goal, a sample of 531 sport center users was used and the psychometric properties of the EDS-R were examined through different analyses. The results supported both the first-order seven-factor model and the higher-order model (seven first-order factors and one second-order factor). The structure of both models was invariant across age. Correlations among the subscales indicated a related factor model, supporting construct validity of the scale. Alpha values over .70 (except for Reduction in Other Activities) and suitable levels of temporal stability were obtained. Users practicing more than three days per week had higher scores in all subscales than the group practicing with a frequency of three days or fewer. The findings of this study provided reliability and validity for the EDS-R in a Spanish context.

Dual Wavelength RP-HPLC Method for Simultaneous Determination of Two Antispasmodic Drugs: An Application in Pharmaceutical and Human Serum.

PubMed

Hasan, Najmul; Chaiharn, Mathurot; Khan, Sauleha; Khalid, Hira; Sher, Nawab; Siddiqui, Farhan Ahmed; Siddiqui, Muhammad Zain

2013-01-01

A reverse phase stability indicating HPLC method for simultaneous determination of two antispasmodic drugs in pharmaceutical parenteral dosage forms (injectable) and in serum has been developed and validated. Mobile phase ingredients consist of Acetonitrile : buffer : sulfuric acid 0.1 M (50 : 50 : 0.3 v/v/v), at flow rate 1.0 mL/min using a Hibar μ Bondapak ODS C18 column monitored at dual wavelength of 266 nm and 205 nm for phloroglucinol and trimethylphloroglucinol, respectively. The drugs were subjected to stress conditions of hydrolysis (oxidation, base, acid, and thermal degradation). Oxidation degraded the molecule drastically while there was not so much significant effect of other stress conditions. The calibration curve was linear with a correlation coefficient of 0.9999 and 0.9992 for PG and TMP, respectively. The drug recoveries fall in the range of 98.56% and 101.24% with 10 pg/mL and 33 pg/mL limit of detection and limit of quantification for both phloroglucinol and trimethylphloroglucinol. The method was validated in accordance with ICH guidelines and was applied successfully to quantify the amount of trimethylphloroglucinol and phloroglucinol in bulk, injectable form and physiological fluid. Forced degradation studies proved the stability indicating abilities of the method.

Does early childhood callous-unemotional behavior uniquely predict behavior problems or callous-unemotional behavior in late childhood?

PubMed Central

Waller, Rebecca; Dishion, Thomas J.; Shaw, Daniel S.; Gardner, Frances; Wilson, Melvin N.; Hyde, Luke W.

2016-01-01

Callous unemotional (CU) behavior has been linked to behavior problems in children and adolescents. However, few studies have examined whether CU behavior in early childhood predicts behavior problems or CU behavior in late childhood. This study examined whether indicators of CU behavior at ages 2–4 predicted aggression, rule-breaking, and CU behavior across informants at age 9.5. To test the unique predictive and convergent validity of CU behavior in early childhood, we accounted for stability in behavior problems and method effects to rule out the possibility that rater biases inflated the magnitude of any associations found. Cross-informant data were collected from a multi-ethnic, high-risk sample (N = 731; female = 49%) at ages 2–4 and again at age 9.5. From age 3, CU behavior uniquely predicted aggression and rule-breaking across informants. There were also unique associations between CU behavior assessed at ages 3 and 4 and CU behavior assessed at age 9.5. Findings demonstrate that early-childhood indicators of CU behavior account for unique variance in later childhood behavior problems and CU behavior, taking into account stability in behavior problems over time and method effects. Convergence with a traditional measure of CU behavior in late childhood provides support for the construct validity of a brief early childhood measure of CU behavior. PMID:27598253

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.

Transcriptional expression of type-I interferon response genes and stability of housekeeping genes in the human endometrium and endometriosis.

PubMed

Vestergaard, Anna L; Knudsen, Ulla B; Munk, Torben; Rosbach, Hanne; Martensen, Pia M

2011-04-01

Endometriosis is a painful chronic female disease defined by the presence of endometrial tissue implants in ectopic (Ec) locations. The pathogenesis is much debated, and type-I interferons (IFNs) could be involved. The expression of genes of the type-I IFN response were profiled by a specific PCR array of RNA obtained from Ec and eutopic (Eu) endometrium collected from nine endometriosis patients and nine healthy control women. Transcriptional expression levels of selected IFN-regulated and housekeeping genes (HKGs) were investigated by real-time quantitative reverse transcriptase PCR (qRT-PCR). Stably expressed HKGs for valid normalization of transcriptional studies of endometrium and endometriosis have not yet been published. Here, seven HKGs were evaluated for stability using the GeNorm and NormFinder software. A normalization factor based on HMBS, TBP and YWHAZ expression was suitable for normalization of qRT-PCR studies of Eu versus Ec endometrium. In the endometrial cell lines HEC1A, HEC1B, Ishikawa and RL95-2, HMBS and HPRT1 were the most stably expressed. The IFN-specific PCR array indicated significantly different expression of the genes BST2, COL16A1, HOXB2 and ISG20 between the endometrial tissue types. However, by correctly normalized qRT-PCR, levels of BST2, COL16A1 and the highly type-I IFN-stimulated genes ISG12A and 6-16 displayed insignificant variations. Conversely, HOXB2 and ISG20 transcriptions were significantly reduced in endometriosis lesions compared with endometrium from endometriosis patients and healthy controls. In conclusion, appropriate HKGs for normalization of qRT-PCR studies of endometrium and endometriosis have been identified here. Abolished expression of ISG20 and HOX genes could be important in endometriosis.

Assigning crystallographic electron densities with free energy calculations—The case of the fluoride channel Fluc

PubMed Central

2018-01-01

Approximately 90% of the structures in the Protein Data Bank (PDB) were obtained by X-ray crystallography or electron microscopy. Whereas the overall quality of structure is considered high, thanks to a wide range of tools for structure validation, uncertainties may arise from density maps of small molecules, such as organic ligands, ions or water, which are non-covalently bound to the biomolecules. Even with some experience and chemical intuition, the assignment of such disconnected electron densities is often far from obvious. In this study, we suggest the use of molecular dynamics (MD) simulations and free energy calculations, which are well-established computational methods, to aid in the assignment of ambiguous disconnected electron densities. Specifically, estimates of (i) relative binding affinities, for instance between an ion and water, (ii) absolute binding free energies, i.e., free energies for transferring a solute from bulk solvent to a binding site, and (iii) stability assessments during equilibrium simulations may reveal the most plausible assignments. We illustrate this strategy using the crystal structure of the fluoride specific channel (Fluc), which contains five disconnected electron densities previously interpreted as four fluoride and one sodium ion. The simulations support the assignment of the sodium ion. In contrast, calculations of relative and absolute binding free energies as well as stability assessments during free MD simulations suggest that four of the densities represent water molecules instead of fluoride. The assignment of water is compatible with the loss of these densities in the non-conductive F82I/F85I mutant of Fluc. We critically discuss the role of the ion force fields for the calculations presented here. Overall, these findings indicate that MD simulations and free energy calculations are helpful tools for modeling water and ions into crystallographic density maps. PMID:29771936

Validation of Bioreactor and Human-on-a-Chip Devices for Chemical Safety Assessment.

PubMed

Rebelo, Sofia P; Dehne, Eva-Maria; Brito, Catarina; Horland, Reyk; Alves, Paula M; Marx, Uwe

2016-01-01

Equipment and device qualification and test assay validation in the field of tissue engineered human organs for substance assessment remain formidable tasks with only a few successful examples so far. The hurdles seem to increase with the growing complexity of the biological systems, emulated by the respective models. Controlled single tissue or organ culture in bioreactors improves the organ-specific functions and maintains their phenotypic stability for longer periods of time. The reproducibility attained with bioreactor operations is, per se, an advantage for the validation of safety assessment. Regulatory agencies have gradually altered the validation concept from exhaustive "product" to rigorous and detailed process characterization, valuing reproducibility as a standard for validation. "Human-on-a-chip" technologies applying micro-physiological systems to the in vitro combination of miniaturized human organ equivalents into functional human micro-organisms are nowadays thought to be the most elaborate solution created to date. They target the replacement of the current most complex models-laboratory animals. Therefore, we provide here a road map towards the validation of such "human-on-a-chip" models and qualification of their respective bioreactor and microchip equipment along a path currently used for the respective animal models.

With Reference to Reference Genes: A Systematic Review of Endogenous Controls in Gene Expression Studies.

PubMed

Chapman, Joanne R; Waldenström, Jonas

2015-01-01

The choice of reference genes that are stably expressed amongst treatment groups is a crucial step in real-time quantitative PCR gene expression studies. Recent guidelines have specified that a minimum of two validated reference genes should be used for normalisation. However, a quantitative review of the literature showed that the average number of reference genes used across all studies was 1.2. Thus, the vast majority of studies continue to use a single gene, with β-actin (ACTB) and/or glyceraldehyde 3-phosphate dehydrogenase (GAPDH) being commonly selected in studies of vertebrate gene expression. Few studies (15%) tested a panel of potential reference genes for stability of expression before using them to normalise data. Amongst studies specifically testing reference gene stability, few found ACTB or GAPDH to be optimal, whereby these genes were significantly less likely to be chosen when larger panels of potential reference genes were screened. Fewer reference genes were tested for stability in non-model organisms, presumably owing to a dearth of available primers in less well characterised species. Furthermore, the experimental conditions under which real-time quantitative PCR analyses were conducted had a large influence on the choice of reference genes, whereby different studies of rat brain tissue showed different reference genes to be the most stable. These results highlight the importance of validating the choice of normalising reference genes before conducting gene expression studies.

Validity and reliability of three commonly used quality of life measures in a large European population of coronary heart disease patients.

PubMed

De Smedt, Delphine; Clays, Els; Doyle, Frank; Kotseva, Kornelia; Prugger, Christof; Pająk, Andrzej; Jennings, Catriona; Wood, David; De Bacquer, Dirk

2013-09-01

To investigate the validity and reliability of the EuroQol-5D (EQ-5D), the 12-item Short-Form Health Survey (SF-12v2), and the Hospital Anxiety and Depression Scale (HADS) in a stable coronary population. Cross-sectional study EUROASPIRE III. Quality of life data (QoL) were available on 8745 patients hospitalized for coronary artery bypass graft (CABG), percutaneous coronary intervention (PCI), acute myocardial infarction (AMI), or myocardial ischemia. They were interviewed and examined at least 6 months after their hospital admission. Reliability and validity of the 3 instruments were tested. Internal consistency, and discriminative, convergent, criterion and construct validity were assessed. Cronbach's alpha indicated good internal consistency for all measures (0.73 to 0.87). Discriminative validity analyses confirmed significant QoL differences between known groups: age, gender, educational level. In addition, all hypothesized correlations between QoL constructs (convergent validity) and items (criterion validity) were confirmed with significant correlations. Confirmatory factor analyses indicated good construct validity for HADS and SF-12v2. On country-specific level, results were roughly similar. The EQ-5D as well as the SF-12v2 and the HADS are reliable and valid instruments for use in a stable coronary population, both on aggregate European level and on country-specific level. However, our results must be generalized with caution, because EUROASPIRE III patients might not be representative for all patients with stable coronary heart disease. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

Development and validation of an administrative case definition for inflammatory bowel diseases

PubMed Central

Rezaie, Ali; Quan, Hude; Fedorak, Richard N; Panaccione, Remo; Hilsden, Robert J

2012-01-01

BACKGROUND: A population-based database of inflammatory bowel disease (IBD) patients is invaluable to explore and monitor the epidemiology and outcome of the disease. In this context, an accurate and validated population-based case definition for IBD becomes critical for researchers and health care providers. METHODS: IBD and non-IBD individuals were identified through an endoscopy database in a western Canadian health region (Calgary Health Region, Calgary, Alberta). Subsequently, using a novel algorithm, a series of case definitions were developed to capture IBD cases in the administrative databases. In the second stage of the study, the criteria were validated in the Capital Health Region (Edmonton, Alberta). RESULTS: A total of 150 IBD case definitions were developed using 1399 IBD patients and 15,439 controls in the development phase. In the validation phase, 318,382 endoscopic procedures were searched and 5201 IBD patients were identified. After consideration of sensitivity, specificity and temporal stability of each validated case definition, a diagnosis of IBD was assigned to individuals who experienced at least two hospitalizations or had four physician claims, or two medical contacts in the Ambulatory Care Classification System database with an IBD diagnostic code within a two-year period (specificity 99.8%; sensitivity 83.4%; positive predictive value 97.4%; negative predictive value 98.5%). An alternative case definition was developed for regions without access to the Ambulatory Care Classification System database. A novel scoring system was developed that detected Crohn disease and ulcerative colitis patients with a specificity of >99% and a sensitivity of 99.1% and 86.3%, respectively. CONCLUSION: Through a robust methodology, a reproducible set of criteria to capture IBD patients through administrative databases was developed. The methodology may be used to develop similar administrative definitions for chronic diseases. PMID:23061064

Engineering Proteins for Thermostability with iRDP Web Server

PubMed Central

Ghanate, Avinash; Ramasamy, Sureshkumar; Suresh, C. G.

2015-01-01

Engineering protein molecules with desired structure and biological functions has been an elusive goal. Development of industrially viable proteins with improved properties such as stability, catalytic activity and altered specificity by modifying the structure of an existing protein has widely been targeted through rational protein engineering. Although a range of factors contributing to thermal stability have been identified and widely researched, the in silico implementation of these as strategies directed towards enhancement of protein stability has not yet been explored extensively. A wide range of structural analysis tools is currently available for in silico protein engineering. However these tools concentrate on only a limited number of factors or individual protein structures, resulting in cumbersome and time-consuming analysis. The iRDP web server presented here provides a unified platform comprising of iCAPS, iStability and iMutants modules. Each module addresses different facets of effective rational engineering of proteins aiming towards enhanced stability. While iCAPS aids in selection of target protein based on factors contributing to structural stability, iStability uniquely offers in silico implementation of known thermostabilization strategies in proteins for identification and stability prediction of potential stabilizing mutation sites. iMutants aims to assess mutants based on changes in local interaction network and degree of residue conservation at the mutation sites. Each module was validated using an extensively diverse dataset. The server is freely accessible at http://irdp.ncl.res.in and has no login requirements. PMID:26436543

Engineering Proteins for Thermostability with iRDP Web Server.

PubMed

Panigrahi, Priyabrata; Sule, Manas; Ghanate, Avinash; Ramasamy, Sureshkumar; Suresh, C G

2015-01-01

Engineering protein molecules with desired structure and biological functions has been an elusive goal. Development of industrially viable proteins with improved properties such as stability, catalytic activity and altered specificity by modifying the structure of an existing protein has widely been targeted through rational protein engineering. Although a range of factors contributing to thermal stability have been identified and widely researched, the in silico implementation of these as strategies directed towards enhancement of protein stability has not yet been explored extensively. A wide range of structural analysis tools is currently available for in silico protein engineering. However these tools concentrate on only a limited number of factors or individual protein structures, resulting in cumbersome and time-consuming analysis. The iRDP web server presented here provides a unified platform comprising of iCAPS, iStability and iMutants modules. Each module addresses different facets of effective rational engineering of proteins aiming towards enhanced stability. While iCAPS aids in selection of target protein based on factors contributing to structural stability, iStability uniquely offers in silico implementation of known thermostabilization strategies in proteins for identification and stability prediction of potential stabilizing mutation sites. iMutants aims to assess mutants based on changes in local interaction network and degree of residue conservation at the mutation sites. Each module was validated using an extensively diverse dataset. The server is freely accessible at http://irdp.ncl.res.in and has no login requirements.

Determination of colonoscopy indication from administrative claims data.

PubMed

Ko, Cynthia W; Dominitz, Jason A; Neradilek, Moni; Polissar, Nayak; Green, Pam; Kreuter, William; Baldwin, Laura-Mae

2014-04-01

Colonoscopy outcomes, such as polyp detection or complication rates, may differ by procedure indication. To develop methods to classify colonoscopy indications from administrative data, facilitating study of colonoscopy quality and outcomes. We linked 14,844 colonoscopy reports from the Clinical Outcomes Research Initiative, a national repository of endoscopic reports, to the corresponding Medicare Carrier and Outpatient File claims. Colonoscopy indication was determined from the procedure reports. We developed algorithms using classification and regression trees and linear discriminant analysis (LDA) to classify colonoscopy indication. Predictor variables included ICD-9CM and CPT/HCPCS codes present on the colonoscopy claim or in the 12 months prior, patient demographics, and site of colonoscopy service. Algorithms were developed on a training set of 7515 procedures, then validated using a test set of 7329 procedures. Sensitivity was lowest for identifying average-risk screening colonoscopies, varying between 55% and 86% for the different algorithms, but specificity for this indication was consistently over 95%. Sensitivity for diagnostic colonoscopy varied between 77% and 89%, with specificity between 55% and 87%. Algorithms with classification and regression trees with 7 variables or LDA with 10 variables had similar overall accuracy, and generally lower accuracy than the algorithm using LDA with 30 variables. Algorithms using Medicare claims data have moderate sensitivity and specificity for colonoscopy indication, and will be useful for studying colonoscopy quality in this population. Further validation may be needed before use in alternative populations.

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

PubMed

Buchholz, Bernhard; Kallweit, Sören; Ebert, Volker

2016-12-30

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

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

PubMed Central

Buchholz, Bernhard; Kallweit, Sören; Ebert, Volker

2016-01-01

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

Incidence of foot rotation, pelvic crest unleveling, and supine leg length alignment asymmetry and their relationship to self-reported back pain.

PubMed

Knutson, Gary A

2002-02-01

To determine the incidence of pelvic unleveling, foot rotation, and supine leg length alignment asymmetry in a nonclinical population and to examine the validity (sensitivity, specificity, positive and negative predictive values) of these visual tests and their relationship to self-reported back pain. Volunteers answered a questionnaire regarding back pain and were then examined by a chiropractor who was unaware of the status of their back pain. Seventy-four unscreened volunteers answered the questionnaire. The association of visual tests with back pain and their validity indices; Visual Analogue Scale ratings. Fifty-one percent (n = 74) of volunteers examined had supine leg length alignment asymmetry (LLA). Pain intensity on a Visual Analogue Scale was significantly higher (P <.001) for those demonstrating supine LLA than for those without LLA. Those with back pain and recurrent back pain were significantly (P <.001) more likely to have supine LLA. The validity indices of the supine leg check showed acceptable levels for sensitivity (74%), specificity (78%), and positive predictive value (82%) [corrected] in recurrent back pain. Findings also indicated a high incidence of supine LLA in volunteers with chronic back pain (85%). The results indicated that, in this group of volunteers, the supine leg length alignment check had clinical validity as a stand-alone test for recurring back pain. Further testing on a larger, statistically defined cross-section of the population is recommended.

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

PubMed

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

2017-01-01

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

Clinical Validation of the Nursing Outcome "Swallowing Status" in People with Stroke: Analysis According to the Classical and Item Response Theories.

PubMed

Oliveira-Kumakura, Ana Railka de Souza; de Araujo, Thelma Leite; Costa, Alice Gabrielle de Sousa; Cavalcante, Tahissa Frota; Lopes, Marcos Venícios de Oliveira; Carvalho, Emilia Campos

2017-09-19

To validate clinically the nursing outcome "Swallowing status". The adjustment of the nursing outcome was investigated according to the Classical and Item Response Theories. The models were compared regarding information loss, goodness-of-fit, and differential item functioning. Stability and internal consistency were examined. The nursing outcome has the best fit in the generalized partial credit model with different discrimination parameters. Strong correlations among the scores of each indicator were observed. There was no differential item functioning of the outcome indicators. The scale presented high internal consistency (Cronbach's α = .954) and stability (and > .800). This study presents a valid nursing outcome. Most accurate monitoring of sensitivity to an intervention. Validar clinicamente o resultado de enefermagem "Estado da Deglutição". MÉTODOS: O ajustamento do resultado foi investigado de acordo com as teorias Clássica e de Resposta ao Item. Os modelos foram comparados assumindo parâmetros de itens cruzados de igual discriminação. Investigaram-se as propriedades de bondade do ajuste, funcionamento diferencial dos itens, estabilidade e consistência interna. O resultado se ajustou melhor a partir do Modelo de crédito parcial generalizado, o qual demonstrou unidimensionalidade do resultado e forte correlação entre os escores de cada indicador. Não houve funcionamento diferencial dos indicadores. A consistência interna para a escala global (Cronbach's α = .954) e a estabilidade (>.800) mantiveram-se elevadas. CONCLUSÃO: O estudo apresenta um resultado de enfermagem válido. RELEVÂNCIA PARA A PRÁTICA CLÍNICA: Maior acurácia para monitorar a sensibilidade da intervenção. © 2017 NANDA International, Inc.

The Stability of Medicinal Plant microRNAs in the Herb Preparation Process.

PubMed

Xie, Wenyan; Melzig, Matthias F

2018-04-16

Herbal medicine is now globally accepted as a valid alternative system of pharmaceutical therapies. Various studies around the world have been initiated to develop scientific evidence-based herbal therapies. Recently, the therapeutic potential of medicinal plant derived miRNAs has attracted great attraction. MicroRNAs have been indicated as new bioactive ingredients in medicinal plants. However, the stability of miRNAs during the herbal preparation process and their bioavailability in humans remain unclear. Viscum album L. (European mistletoe) has been widely used in folk medicine for the treatment of cancer and cardiovascular diseases. Our previous study has indicated the therapeutic potential of mistletoe miRNAs by using bioinformatics tools. To evaluate the stability of these miRNAs, various mistletoe extracts that mimic the clinical medicinal use as well as traditional folk medicinal use were prepared. The mistletoe miRNAs including miR166a-3p, miR159a, miR831-5p, val-miR218 and val-miR11 were quantified by stem-loop qRT-PCR. As a result, miRNAs were detectable in the majority of the extracts, indicating that consumption of medicinal plant preparations might introduce miRNAs into mammals. The factors that might cause miRNA degradation include ultrasonic treatment, extreme heat, especially RNase treatment, while to be associated with plant molecules (e.g., proteins, exosomes) might be an efficient way to protect miRNAs against degradation. Our study confirmed the stability of plant derived miRNAs during herb preparations, suggesting the possibility of functionally intact medicinal plant miRNAs in mammals.

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.

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.

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

PubMed

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

2016-01-01

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

The latency validation of the optical link for the ATLAS Liquid Argon Calorimeter Phase-I trigger upgrade

NASA Astrophysics Data System (ADS)

Deng, B.; Xiao, L.; Zhao, X.; Baker, E.; Gong, D.; Guo, D.; He, H.; Hou, S.; Liu, C.; Liu, T.; Sun, Q.; Thomas, J.; Wang, J.; Xiang, A. C.; Yang, D.; Ye, J.; Zhou, W.

2018-05-01

Two optical data link data transmission Application Specific Integrated Circuits (ASICs), the baseline and its backup, have been designed for the ATLAS Liquid Argon (LAr) Calorimeter Phase-I trigger upgrade. The latency of each ASIC and that of its corresponding receiver implemented in a back-end Field-Programmable Gate Array (FPGA) are critical specifications. In this paper, we present the latency measurements and simulation of two ASICs. The measurement results indicate that both ASICs achieve their design goals and meet the latency specifications. The consistency between the simulation and measurements validates the ASIC latency characterization.

Perceived match or mismatch on the Gottman conflict styles: associations with relationship outcome variables.

PubMed

Busby, Dean M; Holman, Thomas B

2009-12-01

Gottman has proposed that there are 3 functional styles of conflict management in couple relationships, labeled Avoidant, Validating, and Volatile, and 1 dysfunctional style, labeled Hostile. Using a sample of 1,983 couples in a committed relationship, we test the association of perceived matches or mismatches on these conflict styles with relationship outcome variables. The results indicate that 32% of the participants perceive there is a mismatch with their conflict style and that of their partner. The Volatile-Avoidant mismatch was particularly problematic and was associated with more stonewalling, relationship problems, and lower levels of relationship satisfaction and stability than the Validating matched style and than other mismatched styles. The most problematic style was the Hostile style. Contrary to existing assumptions by Gottman, the 3 matched functional styles were not equivalent, as the Validating Style was associated with substantially better results on relationship outcome measures than the Volatile and Avoidant styles.

The Career and Work Adaptability Questionnaire (CWAQ): a first contribution to its validation.

PubMed

Nota, Laura; Ginevra, Maria Cristina; Soresi, Salvatore

2012-12-01

Over the last decade, occupational changes have the rapidly changing job market has begun to demand that people more actively construct their professional lives and acquire career adaptability. The aim of the present study was to develop a specific, new instrument, "Career and Work Adaptability", to assess degree of adaptability in adolescents planning their futures. We conducted three studies, the first of which aimed to formulate the instrument's items and to verify its factor structure; the second study confirmed the instrument's multidimensional structure and evaluated its discriminant validity; the third study was conducted to verify the factorial structure's across-gender invariance and to evaluate its stability over time. Our results showed that the instrument is an effective and multidimensional instrument for accurately measuring career adaptability. Specifically, it can serve as a useful vocational guidance tool in analyzing adolescents' career adaptability. Copyright © 2012 The Foundation for Professionals in Services for Adolescents. Published by Elsevier Ltd. All rights reserved.

Evaluation of vegetation indices for rangeland biomass estimation in the Kimberley area of Western Australia

NASA Astrophysics Data System (ADS)

Mundava, C.; Helmholz, P.; Schut, A. G. T.; Corner, R.; McAtee, B.; Lamb, D. W.

2014-09-01

The objective of this paper is to test the relationships between Above Ground Biomass (AGB) and remotely sensed vegetation indices for AGB assessments in the Kimberley area in Western Australia. For 19 different sites, vegetation indices were derived from eight Landsat ETM+ scenes over a period of two years (2011-2013). The sites were divided into three groups (Open plains, Bunch grasses and Spinifex) based on similarities in dominant vegetation types. Dry and green biomass fractions were measured at these sites. Single and multiple regression relationships between vegetation indices and green and total AGB were calibrated and validated using a "leave site out" cross validation. Four tests were compared: (1) relationships between AGB and vegetation indices combining all sites; (2) separate relationships per site group; (3) multiple regressions including selected vegetation indices per site group; and (4) as in 3 but including rainfall and elevation data. Results indicate that relationships based on single vegetation indices are moderately accurate for green biomass in wide open plains covered with annual grasses. The cross-validation results for green AGB improved for a combination of indices for the Open plains and Bunch grasses sites, but not for Spinifex sites. When rainfall and elevation data are included, cross validation improved slightly with a Q2 of 0.49-0.72 for Open plains and Bunch grasses sites respectively. Cross validation results for total AGB were moderately accurate (Q2 of 0.41) for Open plains but weak or absent for other site groups despite good calibration results, indicating strong influence of site-specific factors.

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…

Stability of Prednisone in Oral Mix Suspending Vehicle.

PubMed

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

2015-01-01

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

A validity assessment of the Progress out of Poverty Index (PPI)™.

PubMed

Desiere, Sam; Vellema, Wytse; D'Haese, Marijke

2015-04-01

Development organisations need easy-to-use and quick-to-implement indicators to quantify poverty when requested to measure program impact. In this paper we assess the validity of the Progress out of Poverty Index (PPI)™, a country-specific indicator based on ten closed questions on directly observable household characteristics, by its compliance to the SMART criteria. Each response receives a pre-determined score, such that the sum of these scores can be converted into the likelihood the household is living below the poverty line. We focus on the PPI scorecard for Rwanda, which was validated using two national household surveys conducted in 2005/06 and 2010/11. The PPI is Specific, Measurable, Available cost effectively, and Timely available. Yet, its Relevance depends on the way it is used. Although it accurately distinguishes poor from non-poor households, making it a useful reporting tool, its limited sensitivity to changes in poverty status restricts its usefulness for evaluating the impact of development projects. Copyright © 2014 Elsevier Ltd. All rights reserved.

Computational Design and Discovery of Ni-Based Alloys and Coatings: Thermodynamic Approaches Validated by Experiments

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

Liu, Zi-Kui; Gleeson, Brian; Shang, Shunli

This project developed computational tools that can complement and support experimental efforts in order to enable discovery and more efficient development of Ni-base structural materials and coatings. The project goal was reached through an integrated computation-predictive and experimental-validation approach, including first-principles calculations, thermodynamic CALPHAD (CALculation of PHAse Diagram), and experimental investigations on compositions relevant to Ni-base superalloys and coatings in terms of oxide layer growth and microstructure stabilities. The developed description included composition ranges typical for coating alloys and, hence, allow for prediction of thermodynamic properties for these material systems. The calculation of phase compositions, phase fraction, and phase stabilities,more » which are directly related to properties such as ductility and strength, was a valuable contribution, along with the collection of computational tools that are required to meet the increasing demands for strong, ductile and environmentally-protective coatings. Specifically, a suitable thermodynamic description for the Ni-Al-Cr-Co-Si-Hf-Y system was developed for bulk alloy and coating compositions. Experiments were performed to validate and refine the thermodynamics from the CALPHAD modeling approach. Additionally, alloys produced using predictions from the current computational models were studied in terms of their oxidation performance. Finally, results obtained from experiments aided in the development of a thermodynamic modeling automation tool called ESPEI/pycalphad - for more rapid discovery and development of new materials.« less

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

NASA Astrophysics Data System (ADS)

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

2015-06-01

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

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

PubMed

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

2015-06-15

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

Radionuclide Incorporation and Long Term Performance of Apatite Waste Forms

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

Wang, Jianwei; Lian, Jie; Gao, Fei

2016-01-04

This project aims to combines state-of-the-art experimental and characterization techniques with atomistic simulations based on density functional theory (DFT) and molecular dynamics (MD) simulations. With an initial focus on long-lived I-129 and other radionuclides such as Cs, Sr in apatite structure, specific research objectives include the atomic scale understanding of: (1) incorporation behavior of the radionuclides and their effects on the crystal chemistry and phase stability; (2) stability and microstructure evolution of designed waste forms under coupled temperature and radiation environments; (3) incorporation and migration energetics of radionuclides and release behaviors as probed by DFT and molecular dynamics (MD) simulations;more » and (4) chemical durability as measured in dissolution experiments for long term performance evaluation and model validation.« less

AKAP200 promotes Notch stability by protecting it from Cbl/lysosome-mediated degradation in Drosophila melanogaster.

PubMed

Bala Tannan, Neeta; Collu, Giovanna; Humphries, Ashley C; Serysheva, Ekatherina; Weber, Ursula; Mlodzik, Marek

2018-01-01

AKAP200 is a Drosophila melanogaster member of the "A Kinase Associated Protein" family of scaffolding proteins, known for their role in the spatial and temporal regulation of Protein Kinase A (PKA) in multiple signaling contexts. Here, we demonstrate an unexpected function of AKAP200 in promoting Notch protein stability. In Drosophila, AKAP200 loss-of-function (LOF) mutants show phenotypes that resemble Notch LOF defects, including eye patterning and sensory organ specification defects. Through genetic interactions, we demonstrate that AKAP200 interacts positively with Notch in both the eye and the thorax. We further show that AKAP200 is part of a physical complex with Notch. Biochemical studies reveal that AKAP200 stabilizes endogenous Notch protein, and that it limits ubiquitination of Notch. Specifically, our genetic and biochemical evidence indicates that AKAP200 protects Notch from the E3-ubiquitin ligase Cbl, which targets Notch to the lysosomal pathway. Indeed, we demonstrate that the effect of AKAP200 on Notch levels depends on the lysosome. Interestingly, this function of AKAP200 is fully independent of its role in PKA signaling and independent of its ability to bind PKA. Taken together, our data indicate that AKAP200 is a novel tissue specific posttranslational regulator of Notch, maintaining high Notch protein levels and thus promoting Notch signaling.

Soil organic matter stability as indicated by compound-specific radiocarbon analyses

NASA Astrophysics Data System (ADS)

van der Voort, Tessa Sophia; Zell, Claudia; Hagedorn, Frank; McIntyre, Cameron; Eglinton, Timothy Ian

2017-04-01

Carbon storage in soils is increasingly recognized as a key ecosystem function, and molecular-level analyses could be a valuable potential indicator of this storage potential. In this framework, radiocarbon constitutes a powerful tool for unraveling soil carbon dynamics on both decadal as well as centennial and millennial timescales. In this study, we look at the radiocarbon signature of specific compounds (fatty acids and n-alkanes) in two forested ecosystems (temperate and pre-alpine) with the aim of attaining a better understanding of soil organic carbon stability on a molecular level. Radiocarbon dating of the fatty acids and n-alkanes has been coupled to abundance data of these compounds and additionally lignin phenols. We hypothesize that potentially, these long-chain apolar compounds could be a representative indicator of the mineral-bound soil organic carbon pool. These well-studied sites are part of the Long-Term Forest Ecosystem Research (LWF) program of the Swiss Federal Institute for Forest, Snow and Landscape research (WSL). Therefore, a wide suite of ancillary climatic and textural data is available for these sites. Initial results show a wide range of ages in the specific compounds which constitute a much larger range than the ages indicated by the density fractions done on the same samples. Overall, this study explores the use of molecular-level indicators to study soil organic matter dynamics, which could help assess the overall potential vulnerability of soil carbon in various ecosystems.

Reverse transcription quantitative real-time polymerase chain reaction reference genes in the spared nerve injury model of neuropathic pain: validation and literature search.

PubMed

Piller, Nicolas; Decosterd, Isabelle; Suter, Marc R

2013-07-10

The reverse transcription quantitative real-time polymerase chain reaction (RT-qPCR) is a widely used, highly sensitive laboratory technique to rapidly and easily detect, identify and quantify gene expression. Reliable RT-qPCR data necessitates accurate normalization with validated control genes (reference genes) whose expression is constant in all studied conditions. This stability has to be demonstrated.We performed a literature search for studies using quantitative or semi-quantitative PCR in the rat spared nerve injury (SNI) model of neuropathic pain to verify whether any reference genes had previously been validated. We then analyzed the stability over time of 7 commonly used reference genes in the nervous system - specifically in the spinal cord dorsal horn and the dorsal root ganglion (DRG). These were: Actin beta (Actb), Glyceraldehyde-3-phosphate dehydrogenase (GAPDH), ribosomal proteins 18S (18S), L13a (RPL13a) and L29 (RPL29), hypoxanthine phosphoribosyltransferase 1 (HPRT1) and hydroxymethylbilane synthase (HMBS). We compared the candidate genes and established a stability ranking using the geNorm algorithm. Finally, we assessed the number of reference genes necessary for accurate normalization in this neuropathic pain model. We found GAPDH, HMBS, Actb, HPRT1 and 18S cited as reference genes in literature on studies using the SNI model. Only HPRT1 and 18S had been once previously demonstrated as stable in RT-qPCR arrays. All the genes tested in this study, using the geNorm algorithm, presented gene stability values (M-value) acceptable enough for them to qualify as potential reference genes in both DRG and spinal cord. Using the coefficient of variation, 18S failed the 50% cut-off with a value of 61% in the DRG. The two most stable genes in the dorsal horn were RPL29 and RPL13a; in the DRG they were HPRT1 and Actb. Using a 0.15 cut-off for pairwise variations we found that any pair of stable reference gene was sufficient for the normalization process. In the rat SNI model, we validated and ranked Actb, RPL29, RPL13a, HMBS, GAPDH, HPRT1 and 18S as good reference genes in the spinal cord. In the DRG, 18S did not fulfill stability criteria. The combination of any two stable reference genes was sufficient to provide an accurate normalization.

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

NASA Technical Reports Server (NTRS)

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

1984-01-01

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

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.

Enhanced thermal stability of RuO2/polyimide interface for flexible device applications

NASA Astrophysics Data System (ADS)

Music, Denis; Schmidt, Paul; Chang, Keke

2017-09-01

We have studied the thermal stability of RuO2/polyimide (Kapton) interface using experimental and theoretical methods. Based on calorimetric and spectroscopic analyses, this inorganic-organic system does not exhibit any enthalpic peaks as well as all bonds in RuO2 and Kapton are preserved up to 500 °C. In addition, large-scale density functional theory based molecular dynamics, carried out in the same temperature range, validates the electronic structure and points out that numerous Ru-C and a few Ru-O covalent/ionic bonds form across the RuO2/Kapton interface. This indicates strong adhesion, but there is no evidence of Kapton degradation upon thermal excitation. Furthermore, RuO2 does not exhibit any interfacial bonds with N and H in Kapton, providing additional evidence for the thermal stability notion. It is suggested that the RuO2/Kapton interface is stable due to aromatic architecture of Kapton. This enhanced thermal stability renders Kapton an appropriate polymeric substrate for RuO2 containing systems in various applications, especially for flexible microelectronic and energy devices.

Prediction of incidence and stability of alcohol use disorders by latent internalizing psychopathology risk profiles in adolescence and young adulthood.

PubMed

Behrendt, Silke; Bühringer, Gerhard; Höfler, Michael; Lieb, Roselind; Beesdo-Baum, Katja

2017-10-01

Comorbid internalizing mental disorders in alcohol use disorders (AUD) can be understood as putative independent risk factors for AUD or as expressions of underlying shared psychopathology vulnerabilities. However, it remains unclear whether: 1) specific latent internalizing psychopathology risk-profiles predict AUD-incidence and 2) specific latent internalizing comorbidity-profiles in AUD predict AUD-stability. To investigate baseline latent internalizing psychopathology risk profiles as predictors of subsequent AUD-incidence and -stability in adolescents and young adults. Data from the prospective-longitudinal EDSP study (baseline age 14-24 years) were used. The study-design included up to three follow-up assessments in up to ten years. DSM-IV mental disorders were assessed with the DIA-X/M-CIDI. To investigate risk-profiles and their associations with AUD-outcomes, latent class analysis with auxiliary outcome variables was applied. AUD-incidence: a 4-class model (N=1683) was identified (classes: normative-male [45.9%], normative-female [44.2%], internalizing [5.3%], nicotine dependence [4.5%]). Compared to the normative-female class, all other classes were associated with a higher risk of subsequent incident alcohol dependence (p<0.05). AUD-stability: a 3-class model (N=1940) was identified with only one class (11.6%) with high probabilities for baseline AUD. This class was further characterized by elevated substance use disorder (SUD) probabilities and predicted any subsequent AUD (OR 8.5, 95% CI 5.4-13.3). An internalizing vulnerability may constitute a pathway to AUD incidence in adolescence and young adulthood. In contrast, no indication for a role of internalizing comorbidity profiles in AUD-stability was found, which may indicate a limited importance of such profiles - in contrast to SUD-related profiles - in AUD stability. Copyright © 2017 Elsevier B.V. All rights reserved.

Validation and use of three complementary analytical methods (LC-FLS, LC-MS/MS and ICP-MS) to evaluate the pharmacokinetics, biodistribution and stability of motexafin gadolinium in plasma and tissues.

PubMed

Miles, Dale R; Mesfin, Mimi; Mody, Tarak D; Stiles, Mark; Lee, Jean; Fiene, John; Denis, Bernie; Boswell, Garry W

2006-05-01

Liquid chromatography-fluorescence (LC-FLS), liquid chromatography-tandem mass spectrometry (LC-MS/MS) and inductively coupled plasma-mass spectrometry (ICP-MS) methods were developed and validated for the evaluation of motexafin gadolinium (MGd, Xcytrin) pharmacokinetics and biodistribution in plasma and tissues. The LC-FLS method exhibited the greatest sensitivity (0.0057 microg mL(-1)), and was used for pharmacokinetic, biodistribution, and protein binding studies with small sample sizes or low MGd concentrations. The LC-MS/MS method, which exhibited a short run time and excellent selectivity, was used for routine clinical plasma sample analysis. The ICP-MS method, which measured total Gd, was used in conjunction with LC methods to assess MGd stability in plasma. All three methods were validated using human plasma. The LC-FLS method was also validated using plasma, liver and kidneys from mice and rats. All three methods were shown to be accurate, precise and robust for each matrix validated. For three mice, the mean (standard deviation) concentration of MGd in plasma/tissues taken 5 hr after dosing with 23 mg kg(-1) MGd was determined by LC-FLS as follows: plasma (0.025+/-0.002 microg mL(-1)), liver (2.89+/-0.45 microg g(-1)), and kidney (6.09+/-1.05 microg g(-1)). Plasma samples from a subset of patients with brain metastases from extracranial tumors were analyzed using both LC-MS/MS and ICP-MS methods. For a representative patient, > or = 90% of the total Gd in plasma was accounted for as MGd over the first hour post dosing. By 24 hr post dosing, 63% of total Gd was accounted for as MGd, indicating some metabolism of MGd.

Development and evaluation of a PCR-based assay kit for authentication of Zaocys dhumnades in traditional Chinese medicine.

PubMed

Zhang, Xiaomei; Zhou, Tingting; Yu, Wenjing; Ai, Jinxia; Wang, Xuesong; Gao, Lijun; Yuan, Guangxin; Li, Mingcheng

2018-01-01

We developed a kind of Zaocys dhumnades DNA test kit and it's indexes including specificity, sensitivity and stability were evaluated and compared with the method recorded in Chinese Pharmacopoeia (2010 edition). The bioinformatics technology was used to design primers, sequencing and blast, in conjunction with PCR technology based on the characteristics of Z. dhumnades cytochrome b (Cyt b) gene. The efficiency of nucleic acid extraction by the kit was done in accordance with Pharmacopoeia method. The kit stability results proved effective after repeated freezing and thawing 20 times. The sensitivity results indicated that the lowest amount detected by the kit was 0. 025 g of each specimen. The specificity test of the kit was 100% specific. All repeatability tests indicated the same results when conducted three times. Compared with the method recorded in Chinese Pharmacopoeia, the PCR-based assay kit by our team developed is accurate, effective in identification of Z. dhumnades, it is simple and fast, demonstrating a broad prospect in quality inspection of Z. dhumnades in the future.

The Turkish Adaptation of the Ten-Item Personality Inventory

PubMed Central

ATAK, Hasan

2013-01-01

Introduction Personality is one of the important domains of psychology, and it is an integration of emotional, cognitive, social and physical properties. In this study, we aimed to assess the applicability of the “Ten-Item Personality Inventory (TIPI)” which measures five basic personality traits in Turkish young people. Method Data from a total of 420 participants - 208 male (49.1%) and 212 female (50.9%) - were employed for the validity and reliability analyses. Of the participants, 230 (54,8%; mean age: 23.2 years; sd=1.6) were university students and the rest were not (n=190; 45.2%; mean age: 23.4 years; df=1.7). The mean age of the participants was 22.1 years (df=1.3), ranging from 18 to 25 years. Results Language validity (correlations between 0.92 and 0.97), exploratory factor analysis yielded 10 items and five-factor model explaining 65.21% of the variance. Confirmatory factor analyses (χ2/df: 2.20, GFI=0.95, AGFI=0.92, CFI=0.93, NNFI=0.91, RMR=0.04, and RMSEA=0.03), item analysis, and convergent validity results indicated that a five-factor solution with 10 items met the criteria standards for adequacy of fit among Turkish young people. The internal consistency (Openness to Experiences 0.83, Agreeableness 0.81, Emotional Stability 0.83, Conscientiousness 0.84, and Extraversion 0.86) and test-retest stability (=54; Openness to Experiences 0.89, Agreeableness 0.87, Emotional Stability 0.89, Conscientiousness 0.87, and Extraversion 0.88) revealed a moderate to acceptable reliabilities. Conclusion The results demonstrated that the TIPI could be used in studies that evaluate personality in Turkish young people. PMID:28360563

Stability analysis and stabilization strategies for linear supply chains

NASA Astrophysics Data System (ADS)

Nagatani, Takashi; Helbing, Dirk

2004-04-01

Due to delays in the adaptation of production or delivery rates, supply chains can be dynamically unstable with respect to perturbations in the consumption rate, which is known as “bull-whip effect”. Here, we study several conceivable production strategies to stabilize supply chains, which is expressed by different specifications of the management function controlling the production speed in dependence of the stock levels. In particular, we will investigate, whether the reaction to stock levels of other producers or suppliers has a stabilizing effect. We will also demonstrate that the anticipation of future stock levels can stabilize the supply system, given the forecast horizon τ is long enough. To show this, we derive linear stability conditions and carry out simulations for different control strategies. The results indicate that the linear stability analysis is a helpful tool for the judgement of the stabilization effect, although unexpected deviations can occur in the non-linear regime. There are also signs of phase transitions and chaotic behavior, but this remains to be investigated more thoroughly in the future.

Full-field measurement of micromotion around a cementless femoral stem using micro-CT imaging and radiopaque markers.

PubMed

Malfroy Camine, V; Rüdiger, H A; Pioletti, D P; Terrier, A

2016-12-08

A good primary stability of cementless femoral stems is essential for the long-term success of total hip arthroplasty. Experimental measurement of implant micromotion with linear variable differential transformers is commonly used to assess implant primary stability in pre-clinical testing. But these measurements are often limited to a few distinct points at the interface. New techniques based on micro-computed tomography (micro-CT) have recently been introduced, such as Digital Volume Correlation (DVC) or markers-based approaches. DVC is however limited to measurement around non-metallic implants due to metal-induced imaging artifacts, and markers-based techniques are confined to a small portion of the implant. In this paper, we present a technique based on micro-CT imaging and radiopaque markers to provide the first full-field micromotion measurement at the entire bone-implant interface of a cementless femoral stem implanted in a cadaveric femur. Micromotion was measured during compression and torsion. Over 300 simultaneous measurement points were obtained. Micromotion amplitude ranged from 0 to 24µm in compression and from 0 to 49µm in torsion. Peak micromotion was distal in compression and proximal in torsion. The technique bias was 5.1µm and its repeatability standard deviation was 4µm. The method was thus highly reliable and compared well with results obtained with linear variable differential transformers (LVDTs) reported in the literature. These results indicate that this micro-CT based technique is perfectly relevant to observe local variations in primary stability around metallic implants. Possible applications include pre-clinical testing of implants and validation of patient-specific models for pre-operative planning. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

PubMed

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

2002-06-01

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

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

NASA Astrophysics Data System (ADS)

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

2017-11-01

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

Validation and Reliability of the Portuguese Version of the Michigan Neuropathy Screening Instrument.

PubMed

Barbosa, Margarida; Saavedra, Ana; Severo, Milton; Maier, Christoph; Carvalho, Davide

2017-04-01

Diabetic peripheral neuropathy is very common in the diabetic population. Early screening for foot pathology is of the utmost importance. The Michigan Neuropathy Screening Instrument (MNSI) is an easy, brief, and noninvasive screening tool. The aim of this study was to validate the semantics and characteristics of both sections of the Portuguese translation of the MNSI for Portuguese diabetic patients. A cross-sectional study was performed on 87 type 1 and 2 diabetic patients at our outpatient endocrinology department. The final sample was composed of 76 patients. Nerve conduction studies were requested, but only a subsample of 42 patients agreed to participate in them. The scale was internally consistent (Cronbach's alpha > 0.70 in section A, or a clinical history questionnaire and a physical examination [section B]), and the scores of both sections were positively correlated (r = 0.70; P < 0.001). With regard to stability, MNSI scores between test/retest showed high stability (intraclass correlation coefficient = 0.91). The receiver-operating characteristic (ROC) demonstrated its validity, with ROC curve values for section A, section B, and sections A + B of 0.913, 0.798, and 0.906 respectively. Considering a cut off of ≥ 3 in section A and of ≥ 2 in section B, we obtained a sensitivity of 100% and 86%; a specificity of 64% and 61%; a positive predictive value of 80% and 73%; and a negative predictive value of 100% and 79%, respectively. The Portuguese MNSI is a reliable and valid tool for screening diabetic neuropathy. © 2016 World Institute of Pain.

Development of the outcome expectancy scale for self-care among periodontal disease patients.

PubMed

Kakudate, Naoki; Morita, Manabu; Fukuhara, Shunichi; Sugai, Makoto; Nagayama, Masato; Isogai, Emiko; Kawanami, Masamitsu; Chiba, Itsuo

2011-12-01

The theory of self-efficacy states that specific efficacy expectations affect behaviour. Two types of efficacy expectations are described within the theory. Self-efficacy expectations are the beliefs in the capacity to perform a specific behaviour. Outcome expectations are the beliefs that carrying out a specific behaviour will lead to a desired outcome. To develop and examine the reliability and validity of an outcome expectancy scale for self-care (OESS) among periodontal disease patients. A 34-item scale was tested on 101 patients at a dental clinic. Accuracy was improved by item analysis, and internal consistency and test-retest stability were investigated. Concurrent validity was tested by examining associations of the OESS score with the self-efficacy scale for self-care (SESS) score and plaque index score. Construct validity was examined by comparing OESS scores between periodontal patients at initial visit (group 1) and those continuing maintenance care (group 2). Item analysis identified 13 items for the OESS. Factor analysis extracted three factors: social-, oral- and self-evaluative outcome expectancy. Cronbach's alpha coefficient for the OESS was 0.90. A significant association was observed between test and retest scores, and between the OESS and SESS and plaque index scores. Further, group 2 had a significantly higher mean OESS score than group 1. We developed a 13-item OESS with high reliability and validity which may be used to assess outcome expectancy for self-care. A patient's psychological condition with regard to behaviour and affective status can be accurately evaluated using the OESS with SESS. © 2011 Blackwell Publishing Ltd.

Music psychopathology. II. Assessment of musical expression.

PubMed

Steinberg, R; Raith, L

1985-01-01

A short polarity profile which was well suited for the assessment of the musical expression of performances recorded from mentally ill patients and controls is described. 9 out of 12 polarities showed sufficient differentiating qualities, ranging from professional to poor amateur performances. Only 3 polarities had to be reformulated. The assessments of the 3 experts had a high interrater reliability and retest stability. The very significant correlation between the results of the experts and 50 independent subjects indicates the validity of the experiment.

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…

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

DOE PAGES

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

2015-07-30

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

Aromatic proteinaceous surfactants stabilize long-lived gas microbubbles from natural sources

NASA Technical Reports Server (NTRS)

Darrigo, J. S.

1981-01-01

Three different types of protein-specific chemical tests were performed on long-lived gas microbubbles derived from aqueous solutions of agarose powder and from filtered aqueous extracts of Hawaiian forest soil. The separate protein-specific tests involved use of either 0.3% (w/v) ninhydrin, 100 microM methylene blue dye, or 0.7-1.0 M 2-hydroxy-5-nitrobenzyl bromide. The chemical test results obtained with each of the two natural substances, i.e., agarose powder and Hawaiian forest soil, were very similar and indicate that the biological surfactants which surround and stabilize long-lived gas microbubbles are proteinaceous compounds that contain, and whose surface activity depends upon, aromatic amino acid residues, particularly tryptophan.

VALUE - A Framework to Validate Downscaling Approaches for Climate Change Studies

NASA Astrophysics Data System (ADS)

Maraun, Douglas; Widmann, Martin; Gutiérrez, José M.; Kotlarski, Sven; Chandler, Richard E.; Hertig, Elke; Wibig, Joanna; Huth, Radan; Wilke, Renate A. I.

2015-04-01

VALUE is an open European network to validate and compare downscaling methods for climate change research. VALUE aims to foster collaboration and knowledge exchange between climatologists, impact modellers, statisticians, and stakeholders to establish an interdisciplinary downscaling community. A key deliverable of VALUE is the development of a systematic validation framework to enable the assessment and comparison of both dynamical and statistical downscaling methods. Here, we present the key ingredients of this framework. VALUE's main approach to validation is user-focused: starting from a specific user problem, a validation tree guides the selection of relevant validation indices and performance measures. Several experiments have been designed to isolate specific points in the downscaling procedure where problems may occur: what is the isolated downscaling skill? How do statistical and dynamical methods compare? How do methods perform at different spatial scales? Do methods fail in representing regional climate change? How is the overall representation of regional climate, including errors inherited from global climate models? The framework will be the basis for a comprehensive community-open downscaling intercomparison study, but is intended also to provide general guidance for other validation studies.

VALUE: A framework to validate downscaling approaches for climate change studies

NASA Astrophysics Data System (ADS)

Maraun, Douglas; Widmann, Martin; Gutiérrez, José M.; Kotlarski, Sven; Chandler, Richard E.; Hertig, Elke; Wibig, Joanna; Huth, Radan; Wilcke, Renate A. I.

2015-01-01

VALUE is an open European network to validate and compare downscaling methods for climate change research. VALUE aims to foster collaboration and knowledge exchange between climatologists, impact modellers, statisticians, and stakeholders to establish an interdisciplinary downscaling community. A key deliverable of VALUE is the development of a systematic validation framework to enable the assessment and comparison of both dynamical and statistical downscaling methods. In this paper, we present the key ingredients of this framework. VALUE's main approach to validation is user- focused: starting from a specific user problem, a validation tree guides the selection of relevant validation indices and performance measures. Several experiments have been designed to isolate specific points in the downscaling procedure where problems may occur: what is the isolated downscaling skill? How do statistical and dynamical methods compare? How do methods perform at different spatial scales? Do methods fail in representing regional climate change? How is the overall representation of regional climate, including errors inherited from global climate models? The framework will be the basis for a comprehensive community-open downscaling intercomparison study, but is intended also to provide general guidance for other validation studies.

Persian language version of the "Tinnitus Handicap Inventory": translation, standardization, validity and reliability.

PubMed

Mahmoudian, Saeid; Shahmiri, Elaheh; Rouzbahani, Masoumeh; Jafari, Zahra; Keyhani, Mohammad; Rahimi, Farzad; Mahmoudian, Guiti; Akbarvand, Leila; Barzegar, Gholamreza; Farhadi, Mohammad

2011-01-01

Tinnitus is a debilitating condition that is widespread yet difficult to successfully diagnose and treat. This symptom can seriously affect the individual's life quality. The aim of current study was to compose and validate a Persian version of the Tinnitus Handicap Inventory (THI-P). The linguistic validation of the original version of THI into Persian version (THI-P) included translation, back translation and data gathering. The THI-P was administered to 112 tinnitus subjects. Age, gender, medical history and tinnitus characteristics were recorded as baseline information. All participants complained of chronic unilateral or bilateral subjective idiopathic tinnitus lasting for at least 6 months before consulting about their tinnitus. There was no significant difference between gender, age, hearing impairment and total score and subscales of THI-P. Pearson product-moment correlations revealed adequate test-retest reliability for the THI-P (r = 0.96). Cronbach's-alpha coefficient indicated adequate internal stability of the THI-P (r= 0.943), with a total item correction varying between r=0.939 and r=0.944, indicating its reproducibility. The present study proved the internal consistency/ coherency of the Persian version of THI (THI-P). This provides satisfactory application in clinical/research environments.

In silico selection of expression reference genes with demonstrated stability in barley among a diverse set of tissues and cultivars

USDA-ARS?s Scientific Manuscript database

Premise of the study: Reference genes are selected based on the assumption of temporal and spatial expression stability and on their widespread use in model species. They are often used in new target species without validation, presumed as stable. For barley, reference gene validation is lacking, bu...

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

PubMed

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

2011-03-25

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

Validation of the shortened Perceived Medical Condition Self-Management Scale in patients with chronic disease.

PubMed

Wild, Marcus G; Ostini, Remo; Harrington, Magdalena; Cavanaugh, Kerri L; Wallston, Kenneth A

2018-05-21

Self-efficacy, or perceived competence, has been identified as an important factor in self-management behaviors and health outcomes in patients with chronic disease. Measures of self-management self-efficacy are currently available for multiple forms of chronic disease. One established measure is the 8-item Perceived Medical Condition Self-Management Scale (PMCSMS). This study investigated the use of the PMCSMS in samples of patients with a chronic disease to develop an abbreviated version of the scale that could be more readily used in clinical contexts or in large population health cohort studies. The PMCSMS was administered as either a generic scale or as a disease-specific scale. The results of analyses using item response theory and classical test theory methods indicated that using 4 items of the scale resulted in similar internal consistency (α = .70-0.90) and temporal stability (test-retest r = .75 after 2 to 4 weeks) to the 8-item PMCSMS (r = .81 after 2 to 4 weeks). The 4 items selected had the greatest discriminability among participants (α parameters = 2.49-3.47). Scores from both versions also demonstrated similar correlations with related constructs such as health literacy (r = .13-0.29 vs. 0.14-0.27), self-rated health (r = .17-0.48 vs. 0.26-0.50), social support (r = .21-0.32 vs. 0.25-0.34), and medication adherence (r = .20-0.24 vs. 0.20-0.25). The results of this study indicate that 4-item PMCSMS scores are equally valid but more efficient, and have the potential to be beneficial for both research and clinical applications. (PsycINFO Database Record (c) 2018 APA, all rights reserved).

Development and Validation of an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) Method for Quantitative Analysis of Platinum in Plasma, Urine, and Tissues.

PubMed

Zhang, Ti; Cai, Shuang; Forrest, Wai Chee; Mohr, Eva; Yang, Qiuhong; Forrest, M Laird

2016-09-01

Cisplatin, a platinum chemotherapeutic, is one of the most commonly used chemotherapeutic agents for many solid tumors. In this work, we developed and validated an inductively coupled plasma mass spectrometry (ICP-MS) method for quantitative determination of platinum levels in rat urine, plasma, and tissue matrices including liver, brain, lungs, kidney, muscle, heart, spleen, bladder, and lymph nodes. The tissues were processed using a microwave accelerated reaction system (MARS) system prior to analysis on an Agilent 7500 ICP-MS. According to the Food and Drug Administration guidance for industry, bioanalytical validation parameters of the method, such as selectivity, accuracy, precision, recovery, and stability were evaluated in rat biological samples. Our data suggested that the method was selective for platinum without interferences caused by other presenting elements, and the lower limit of quantification was 0.5 ppb. The accuracy and precision of the method were within 15% variation and the recoveries of platinum for all tissue matrices examined were determined to be 85-115% of the theoretical values. The stability of the platinum-containing solutions, including calibration standards, stock solutions, and processed samples in rat biological matrices was investigated. Results indicated that the samples were stable after three cycles of freeze-thaw and for up to three months. © The Author(s) 2016.

Development and Validation of an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) Method for Quantitative Analysis of Platinum in Plasma, Urine, and Tissues

PubMed Central

Zhang, Ti; Cai, Shuang; Forrest, Wai Chee; Mohr, Eva; Yang, Qiuhong; Forrest, M. Laird

2016-01-01

Cisplatin, a platinum chemotherapeutic, is one of the most commonly used chemotherapeutic agents for many solid tumors. In this work, we developed and validated an inductively coupled plasma mass spectrometry (ICP-MS) method for quantitative determination of platinum levels in rat urine, plasma, and tissue matrices including liver, brain, lungs, kidney, muscle, heart, spleen, bladder, and lymph nodes. The tissues were processed using a microwave accelerated reaction system (MARS) system prior to analysis on an Agilent 7500 ICP-MS. According to the Food and Drug Administration guidance for industry, bioanalytical validation parameters of the method, such as selectivity, accuracy, precision, recovery, and stability were evaluated in rat biological samples. Our data suggested that the method was selective for platinum without interferences caused by other presenting elements, and the lower limit of quantification was 0.5 ppb. The accuracy and precision of the method were within 15% variation and the recoveries of platinum for all tissue matrices examined were determined to be 85–115% of the theoretical values. The stability of the platinum-containing solutions, including calibration standards, stock solutions, and processed samples in rat biological matrices was investigated. Results indicated that the samples were stable after three cycles of freeze–thaw and for up to three months. PMID:27527103

Translation and psychometric evaluation of Persian versions of Burn Specific Pain Anxiety Scale and Impact of Event Scale.

PubMed

Ghezeljeh, Tahereh Najafi; Ardebili, Fatimah Mohades; Rafii, Forough; Hagani, Hamid

2013-09-01

Burn as a traumatic life incident manifests severe pain and psychological problems. Specific instruments are needed to evaluate burn patients' psychological issues related to the injury. The aim of this study was to translate and evaluate the reliability and validity of the Persian versions of Impact of Burn Specific Pain Anxiety scale (BSPAS) and Impact of Event Scale (IES). In this cross-sectional study, convenience sampling method was utilized to select 55 Iranian hospitalized burn patients. Combined translation was utilized for translating scales. Alpha cronbach, item-total correlation, convergent and discriminative validity were evaluated. The Cronbach's α for both BSPAS- and IES-Persian version was 0.96. Item-total correlation coefficients ranged from 0.70 to 0.90. Convergent construct validity was confirmed by indicating high correlation between the scales designed to measure the same concepts. The mean score of BSPAS- and IES-Persian version was lower for individuals with a lower TBSA burn percentage which assessed discriminative construct validity of scales. BSPAS- and IES-Persian version showed high internal consistency and good validity for the assessment of burn psychological outcome in hospitalized burn patients. Future studies are needed to determine repeatability, factor structure, sensitivity and specificity of the scales. Copyright © 2013 Elsevier Ltd and ISBI. All rights reserved.

The Johns Hopkins Fall Risk Assessment Tool: A Study of Reliability and Validity.

PubMed

Poe, Stephanie S; Dawson, Patricia B; Cvach, Maria; Burnett, Margaret; Kumble, Sowmya; Lewis, Maureen; Thompson, Carol B; Hill, Elizabeth E

Patient falls and fall-related injury remain a safety concern. The Johns Hopkins Fall Risk Assessment Tool (JHFRAT) was developed to facilitate early detection of risk for anticipated physiologic falls in adult inpatients. Psychometric properties in acute care settings have not yet been fully established; this study sought to fill that gap. Results indicate that the JHFRAT is reliable, with high sensitivity and negative predictive validity. Specificity and positive predictive validity were lower than expected.

Genetic and epigenetic stability of cryopreserved and cold-stored hops (Humulus lupulus L.).

PubMed

Peredo, Elena L; Arroyo-García, Rosa; Reed, Barbara M; Revilla, M Angeles

2008-12-01

Conventional cold storage and cryopreservation methods for hops (Humulus lupulus L.) are available but, to our knowledge, the genetic and epigenetic stability of the recovered plants have not been tested. This study analyzed 51 accessions of hop using the molecular techniques, Random Amplified DNA Polymorphism (RAPD) and Amplified Fragment Length Polymorphism (AFLP), revealing no genetic variation among greenhouse-grown controls and cold stored or cryopreserved plants. Epigenetic stability was evaluated using Methylation Sensitive Amplified Polymorphism (MSAP). Over 36% of the loci were polymorphic when the cold and cryo-treated plants were compared to greenhouse plants. The main changes were demethylation events and they were common to the cryopreserved and cold stored plants indicating the possible effect of the in vitro establishment process, an essential step in both protocols. Protocol-specific methylation patterns were also detected indicating that both methods produced epigenetic changes in plants following cold storage and cryopreservation.

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

PubMed Central

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

2015-01-01

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

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.

Development and validation of a selective, sensitive and stability indicating UPLC-MS/MS method for rapid, simultaneous determination of six process related impurities in darunavir drug substance.

PubMed

A, Vijaya Bhaskar Reddy; Yusop, Zulkifli; Jaafar, Jafariah; Aris, Azmi B; Majid, Zaiton A; Umar, Khalid; Talib, Juhaizah

2016-09-05

In this study a sensitive and selective gradient reverse phase UPLC-MS/MS method was developed for the simultaneous determination of six process related impurities viz., Imp-I, Imp-II, Imp-III, Imp-IV, Imp-V and Imp-VI in darunavir. The chromatographic separation was performed on Acquity UPLC BEH C18 (50 mm×2.1mm, 1.7μm) column using gradient elution of acetonitrile-methanol (80:20, v/v) and 5.0mM ammonium acetate containing 0.01% formic acid at a flow rate of 0.4mL/min. Both negative and positive electrospray ionization (ESI) modes were operated simultaneously using multiple reaction monitoring (MRM) for the quantification of all six impurities in darunavir. The developed method was fully validated following ICH guidelines with respect to specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision, robustness and sample solution stability. The method was able to quantitate Imp-I, Imp-IV, Imp-V at 0.3ppm and Imp-II, Imp-III, and Imp-VI at 0.2ppm with respect to 5.0mg/mL of darunavir. The calibration curves showed good linearity over the concentration range of LOQ to 250% for all six impurities. The correlation coefficient obtained was >0.9989 in all the cases. The accuracy of the method lies between 89.90% and 104.60% for all six impurities. Finally, the method has been successfully applied for three formulation batches of darunavir to determine the above mentioned impurities, however no impurity was found beyond the LOQ. This method is a good quality control tool for the trace level quantification of six process related impurities in darunavir during its synthesis. Copyright © 2016 Elsevier B.V. All rights reserved.

English translation and validation of the SarQoL®, a quality of life questionnaire specific for sarcopenia.

PubMed

Beaudart, Charlotte; Edwards, Mark; Moss, Charlotte; Reginster, Jean-Yves; Moon, Rebecca; Parsons, Camille; Demoulin, Christophe; Rizzoli, René; Biver, Emmanuel; Dennison, Elaine; Bruyere, Olivier; Cooper, Cyrus

2017-03-01

the first quality of life questionnaire specific to sarcopenia, the SarQoL®, has recently been developed and validated in French. To extend the availability and utilisation of this questionnaire, its translation and validation in other languages is necessary. the purpose of this study was therefore to translate the SarQoL® into English and validate the psychometric properties of this new version. cross-sectional. Hertfordshire, UK. in total, 404 participants of the Hertfordshire Cohort Study, UK. the translation part was articulated in five stages: (i) two initial translations from French to English; (ii) synthesis of the two translations; (iii) backward translations; (iv) expert committee to compare the backward translations with the original questionnaire and (v) pre-test. To validate the English SarQoL®, we assessed its validity (discriminative power, construct validity), reliability (internal consistency, test-retest reliability) and floor/ceiling effects. the SarQoL® questionnaire was translated without any major difficulties. Results indicated a good discriminative power (lower score of quality of life for sarcopenic subjects, P = 0.01), high internal consistency (Cronbach's alpha of 0.88), consistent construct validity (high correlations found with domains related to mobility, usual activities, vitality, physical function and low correlations with domains related to anxiety, self-care, mental health and social problems) and excellent test-retest reliability (intraclass coefficient correlation of 0.95, 95%CI 0.92-0.97). Moreover, no floor/ceiling has been found. a valid SarQoL® English questionnaire is now available and can be used with confidence to better assess the disease burden associated with sarcopenia. It could also be used as a treatment outcome indicator in research. © The Author 2016. Published by Oxford University Press on behalf of the British Geriatrics Society.

Development and validation of the Questionnaire of Stressful Life Events (QSLE).

PubMed

Butjosa, Anna; Gómez-Benito, Juana; Myin-Germeys, Inez; Barajas, Ana; Baños, Iris; Usall, Judith; Grau, Norma; Granell, Luis; Sola, Andrea; Carlson, Janina; Dolz, Montserrat; Sánchez, Bernardo; Haro, Josep Maria; Ochoa, Susana

2017-12-01

Stressful life events (SLEs) are important indicators prior to the onset of first-episode psychosis (FEP). Although there are well-validated interviews and self-reports for assessing SLE on proximate events, unfortunately there are no instruments to assess SLE covering an entire lifetime. This study includes detailed specific items of childhood, adolescence, and adulthood focused on the presence of SLE, emotional impact (stressfulness), and the age at which the event occurred. Our research describes 2 studies designed to develop and validate a new scale to assess SLE: the Questionnaire of Stressful Life Events (QSLE). In Study 1, an over-inclusive item pool was generated based on review of group of experts at Parc Sanitari Sant Joan de Déu and content validity was examined by an Expert Survey. The whole scale represents the content domain. In Study 2, item-level analyses revealed good distributional properties, intra-rater reliability, and convergent and discriminant validity. In the sensitivity and specificity analysis, 18 items had high relevance in the discriminability between patients with FEP and healthy controls. We note that there was an AUC of 0.676, indicating a good predictor. Using 7 as a cutoff to predict an individual as a patient would yield a sensitivity of 64.8% and a specificity of 65%. Overall, the QSLE displayed satisfactory psychometric characteristics in a Spanish population. These results suggest that QSLE gives us the opportunity to investigate childhood, adolescent, and adult life events by measuring the stress and age at the moment on a continuous scale. Copyright © 2017 Elsevier Ltd. All rights reserved.

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.

Review of alternative fuels data bases

NASA Technical Reports Server (NTRS)

Harsha, P. T.; Edelman, R. B.

1983-01-01

Based on an analysis of the interaction of fuel physical and chemical properties with combustion characteristics and indicators, a ranking of the importance of various fuel properties with respect to the combustion process was established. This ranking was used to define a suite of specific experiments whose objective is the development of an alternative fuels design data base. Combustion characteristics and indicators examined include droplet and spray formation, droplet vaporization and burning, ignition and flame stabilization, flame temperature, laminar flame speed, combustion completion, soot emissions, NOx and SOx emissions, and the fuels' thermal and oxidative stability and fouling and corrosion characteristics. Key fuel property data is found to include composition, thermochemical data, chemical kinetic rate information, and certain physical properties.

Cultural adaptation and validation of the "Kidney Disease and Quality of Life--Short Form (KDQOL-SF™) version 1.3" questionnaire in Egypt.

PubMed

Abd ElHafeez, Samar; Sallam, Sunny A; Gad, Zahira M; Zoccali, Carmine; Torino, Claudia; Tripepi, Giovanni; ElWakil, Hala S; Awad, Noha M

2012-12-13

Health Related Quality of Life (HRQOL) instruments need disease and country specific validation. In Arab countries, there is no specific validated questionnaire for assessment of HRQOL in chronic kidney disease (CKD) patients. The aim of this study was to present an Arabic translation, adaptation, and the subsequent validation of the kidney disease quality of life-short form (KDQOL-SFTM) version 1.3 questionnaire in a representative series of Egyptian CKD patients. KDQOL-SFTM version 1.3 was translated into Arabic by two independent translators, and then subsequently translated back into English. After translation disparities were reconciled, the final Arabic questionnaire was tested by interviewing 100 pre-dialysis CKD (stage 1-4) patients randomly selected from outpatients attending the Nephrology clinic at the Main Alexandria University Hospital. Test re-test reliability was performed, with a subsample of 50 consecutive CKD patients, by two interviews 7 days apart and internal consistency estimated by Cronbach's α. Discriminant, concept, and construct validity were assessed. All items of SF-36 met the criterion for internal consistency and were reproducible. Of the 10 kidney disease targeted scales, only three had Cronbach's α <0.7: quality of social interaction (0.23), work status (0.28), and cognitive function (0.60). All disease specific scales were reproducible. Results from discriminant validity showed that the study questionnaire could discriminate between patients' subgroups. As for concept validity, the correlation between all domains of the questionnaire with overall health ratewas significant for all domains except for the work status, sexual function, emotional wellbeing, and role emotional. Furthermore, the correlation between the disease specific domains and the two composite summaries of SF-36 (physical and mental composite summaries) was significant for all domains except for sexual function with mental composite summary. Construct validity was indicated by the observation that the majority of the domains of the kidney disease targeted scale of KDQOL-SFTM 1.3 were significantly inter-correlated. Finally, principal component analysis of the kidney disease targeted scale indicated that this part of the questionnaire could be summarized into 10 factors that together explained 70.9% of the variance. The results suggest that this Arabic version of the KDQOL-SFTM 1.3 questionnaire is a valid and reliable tool for use in Egyptian patients with CKD.

Improving the sensitivity and specificity of a bioanalytical assay for the measurement of certolizumab pegol.

PubMed

Smeraglia, John; Silva, John-Paul; Jones, Kieran

2017-08-01

In order to evaluate placental transfer of certolizumab pegol (CZP), a more sensitive and selective bioanalytical assay was required to accurately measure low CZP concentrations in infant and umbilical cord blood. Results & methodology: A new electrochemiluminescence immunoassay was developed to measure CZP levels in human plasma. Validation experiments demonstrated improved selectivity (no matrix interference observed) and a detection range of 0.032-5.0 μg/ml. Accuracy and precision met acceptance criteria (mean total error ≤20.8%). Dilution linearity and sample stability were acceptable and sufficient to support the method. The electrochemiluminescence immunoassay was validated for measuring low CZP concentrations in human plasma. The method demonstrated a more than tenfold increase in sensitivity compared with previous assays, and improved selectivity for intact CZP.

Spectroscopic characterization and quantitative determination of atorvastatin calcium impurities by novel HPLC method

NASA Astrophysics Data System (ADS)

Gupta, Lokesh Kumar

2012-11-01

Seven process related impurities were identified by LC-MS in the atorvastatin calcium drug substance. These impurities were identified by LC-MS. The structure of impurities was confirmed by modern spectroscopic techniques like 1H NMR and IR and physicochemical studies conducted by using synthesized authentic reference compounds. The synthesized reference samples of the impurity compounds were used for the quantitative HPLC determination. These impurities were detected by newly developed gradient, reverse phase high performance liquid chromatographic (HPLC) method. The system suitability of HPLC analysis established the validity of the separation. The analytical method was validated according to International Conference of Harmonization (ICH) with respect to specificity, precision, accuracy, linearity, robustness and stability of analytical solutions to demonstrate the power of newly developed HPLC method.

Advanced stability indicating chemometric methods for quantitation of amlodipine and atorvastatin in their quinary mixture with acidic degradation products

NASA Astrophysics Data System (ADS)

Darwish, Hany W.; Hassan, Said A.; Salem, Maissa Y.; El-Zeany, Badr A.

2016-02-01

Two advanced, accurate and precise chemometric methods are developed for the simultaneous determination of amlodipine besylate (AML) and atorvastatin calcium (ATV) in the presence of their acidic degradation products in tablet dosage forms. The first method was Partial Least Squares (PLS-1) and the second was Artificial Neural Networks (ANN). PLS was compared to ANN models with and without variable selection procedure (genetic algorithm (GA)). For proper analysis, a 5-factor 5-level experimental design was established resulting in 25 mixtures containing different ratios of the interfering species. Fifteen mixtures were used as calibration set and the other ten mixtures were used as validation set to validate the prediction ability of the suggested models. The proposed methods were successfully applied to the analysis of pharmaceutical tablets containing AML and ATV. The methods indicated the ability of the mentioned models to solve the highly overlapped spectra of the quinary mixture, yet using inexpensive and easy to handle instruments like the UV-VIS spectrophotometer.

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

PubMed

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

2016-02-01

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

LC-MS/MS method for the determination of clodronate in human plasma.

PubMed

Hasan, Mahmoud; Schumacher, Gitta; Seekamp, Anne; Taedken, Tobias; Siegmund, Werner; Oswald, Stefan

2014-11-01

Clodronate belongs to the class of bisphosphonates which are used for the treatment of bone disorders. Due to its high polarity it has a low and highly variable oral bioavailability which results in low plasma concentrations and requires sensitive bioanalytical methods to characterize its pharmacokinetics in human. Here, we describe for the first time the development and validation of a LC-MS/MS assay for the quantification of clodronate in human plasma. The bisphosphonate was isolated from the biological matrix by protein precipitation using perchloric acid (10%), and derivatized with trimethylorthoacetate prior sample clean-up with liquid-liquid extraction using methyl tert-butyl ether. The chromatography was performed using an isocratic elution with ammonium acetate 5mM (85% v/v, pH 3.8) and acetonitrile (15% v/v) as mobile phase with a flow rate of 300μl/min on a reversed-phase column (Supelco Ascentis(®), C18) temporized at 50°C. The mass spectrometric detection was done using the API4000 triple quadruple mass spectrometer monitoring the mass/charge transitions 301.0/145 for clodronate and 305.2/137.1 for the internal standard etidronate. The analytical range was set to 5-800ng/ml, allowing an evaluation of the plasma concentration-time profiles of clodronate for approximately 7-8 half-life (∼24h). The method was validated according to current FDA/EMA guidelines on bioanalytical method validation with respect to specificity, linearity, intra- and inter-day accuracy and precision, matrix effect, recovery as well as stability. The precision of the assay was 0.6-6.9% and 0.6-8.1% for the intra-day and inter-day variability, respectively. The intra-day and inter-day accuracy (error) was 0.6-8.8% and 2.2-4.5%. The recovery of the analyte was low (2-3%) but reproducible over the entire validation range and sufficient to monitor the target concentrations in human plasma. The drug was shown to be stable in plasma at room temperature for at least 3h (96.0±6%) and for at least 24h when stored in the cooled autosampler at 4°C (102.4±4.5%). Clodronate can also undergo up to three freeze-thaw cycles without impaired stability. Thus, the method was shown to possess sufficient specificity, sensitivity, accuracy, precision and stability to measure plasma concentrations of clodronate. Finally, the developed method was successfully applied to study the clodronate serum levels in a pharmacokinetic study in healthy volunteers. Copyright © 2014 Elsevier B.V. All rights reserved.

International ring trial for the validation of an event-specific Golden Rice 2 quantitative real-time polymerase chain reaction method.

PubMed

Jacchia, Sara; Nardini, Elena; Bassani, Niccolò; Savini, Christian; Shim, Jung-Hyun; Trijatmiko, Kurniawan; Kreysa, Joachim; Mazzara, Marco

2015-05-27

This article describes the international validation of the quantitative real-time polymerase chain reaction (PCR) detection method for Golden Rice 2. The method consists of a taxon-specific assay amplifying a fragment of rice Phospholipase D α2 gene, and an event-specific assay designed on the 3' junction between transgenic insert and plant DNA. We validated the two assays independently, with absolute quantification, and in combination, with relative quantification, on DNA samples prepared in haploid genome equivalents. We assessed trueness, precision, efficiency, and linearity of the two assays, and the results demonstrate that both the assays independently assessed and the entire method fulfill European and international requirements for methods for genetically modified organism (GMO) testing, within the dynamic range tested. The homogeneity of the results of the collaborative trial between Europe and Asia is a good indicator of the robustness of the method.

Structural and Functional Analysis of an mRNP Complex That Mediates the High Stability of Human β-Globin mRNA

PubMed Central

Yu, Jia; Russell, J. Eric

2001-01-01

Human globins are encoded by mRNAs exhibiting high stabilities in transcriptionally silenced erythrocyte progenitors. Unlike α-globin mRNA, whose stability is enhanced by assembly of a specific messenger RNP (mRNP) α complex on its 3′ untranslated region (UTR), neither the structure(s) nor the mechanism(s) that effects the high-level stability of human β-globin mRNA has been identified. The present work describes an mRNP complex assembling on the 3′ UTR of the β-globin mRNA that exhibits many of the properties of the stability-enhancing α complex. The β-globin mRNP complex is shown to contain one or more factors homologous to αCP, a 39-kDa RNA-binding protein that is integral to α-complex assembly. Sequence analysis implicates a specific 14-nucleotide pyrimidine-rich track within its 3′ UTR as the site of β-globin mRNP assembly. The importance of this track to mRNA stability is subsequently verified in vivo using mice expressing human β-globin transgenes that contain informative mutations in this region. In combination, the in vitro and in vivo analyses indicate that the high stabilities of the α- and β-globin mRNAs are maintained through related mRNP complexes that may share a common regulatory pathway. PMID:11486027

The needs of siblings of children with a life-threatening illness, part 2: Psychometric validation of the IBesFEMS.

PubMed

Olivier d'avignon, Marianne; Dumont, Serge; Valois, Pierre; Cohen, S Robin

2017-02-01

Life-threatening illnesses in children have a significant impact on the lives of their brothers and sisters. Consequently, special attention must be paid to the specific needs of these siblings to help them cope with their situations. To address this issue, we developed an inventory of the needs of the adolescent siblings of severely ill children, the Inventaire des Besoins de la Fratrie d'Enfants Malades Sévèrement (IBesFEMS) [Needs Inventory for Siblings of Critically Ill Children]. The present article describes a preliminary validation study of this new instrument. In a prospective cohort study, the 48-item instrument was administered via a website or paper to 58 siblings. Our study revealed that the measure has an estimated internal consistency of 0.96 and a temporal stability intraclass correlation coefficient (ICC) of 0.86 (p < 0.01). Its convergence validity is also satisfactory. Our findings suggest that the IBesFEMS is highly relevant for pediatric palliative care clinicians and researchers. Future studies should investigate its factorial structure and predictive validities.

Development and Validation of New Discriminative Dissolution Method for Carvedilol Tablets

PubMed Central

Raju, V.; Murthy, K. V. R.

2011-01-01

The objective of the present study was to develop and validate a discriminative dissolution method for evaluation of carvedilol tablets. Different conditions such as type of dissolution medium, volume of dissolution medium and rotation speed of paddle were evaluated. The best in vitro dissolution profile was obtained using Apparatus II (paddle), 50 rpm, 900 ml of pH 6.8 phosphate buffer as dissolution medium. The drug release was evaluated by high-performance liquid chromatographic method. The dissolution method was validated according to current ICH and FDA guidelines using parameters such as the specificity, accuracy, precision and stability were evaluated and obtained results were within the acceptable range. The comparison of the obtained dissolution profiles of three different products were investigated using ANOVA-based, model-dependent and model-independent methods, results showed that there is significant difference between the products. The dissolution test developed and validated was adequate for its higher discriminative capacity in differentiating the release characteristics of the products tested and could be applied for development and quality control of carvedilol tablets. PMID:22923865

Development and validation of a liquid chromatography-isotope dilution tandem mass spectrometry for determination of olanzapine in human plasma and its application to bioavailability study.

PubMed

Zhang, Meng-Qi; Jia, Jing-Ying; Lu, Chuan; Liu, Gang-Yi; Yu, Cheng-Yin; Gui, Yu-Zhou; Liu, Yun; Liu, Yan-Mei; Wang, Wei; Li, Shui-Jun; Yu, Chen

2010-06-01

A simple, reliable and sensitive liquid chromatography-isotope dilution mass spectrometry (LC-ID/MS) was developed and validated for quantification of olanzapine in human plasma. Plasma samples (50 microL) were extracted with tert-butyl methyl ether and isotope-labeled internal standard (olanzapine-D3) was used. The chromatographic separation was performed on XBridge Shield RP 18 (100 mm x 2.1 mm, 3.5 microm, Waters). An isocratic program was used at a flow rate of 0.4 m x min(-1) with mobile phase consisting of acetonitrile and ammonium buffer (pH 8). The protonated ions of analytes were detected in positive ionization by multiple reactions monitoring (MRM) mode. The plasma method, with a lower limit of quantification (LLOQ) of 0.1 ng x mL(-1), demonstrated good linearity over a range of 0.1 - 30 ng x mL(-1) of olanzapine. Specificity, linearity, accuracy, precision, recovery, matrix effect and stability were evaluated during method validation. The validated method was successfully applied to analyzing human plasma samples in bioavailability study.

Comparing Generic and Condition-Specific Preference-Based Measures in Epilepsy: EQ-5D-3L and NEWQOL-6D.

PubMed

Mulhern, Brendan; Pink, Joshua; Rowen, Donna; Borghs, Simon; Butt, Thomas; Hughes, Dyfrig; Marson, Antony; Brazier, John

2017-04-01

There is debate about the psychometric characteristics of the three-level EuroQol five-dimensional questionnaire (EQ-5D-3L) for use in epilepsy. In response to the concerns, an epilepsy-specific preference-based measure (NEWQOL-6D) was developed. The psychometric characteristics of the NEWQOL-6D, however, have not been assessed. To investigate the validity and responsiveness of the EQ-5D-3L and the Quality of Life in Newly Diagnosed Epilepsy Instrument-six dimensions (NEWQOL-6D) for use in the assessment of treatments for newly diagnosed focal epilepsy. The analysis used data from the Standard And New Antiepileptic Drugs trial including patients with focal epilepsy. We assessed convergent validity using correlations, and known-group validity across different epilepsy and general health severity indicators using analysis of variance and effect sizes. The responsiveness of the measures to change over time was assessed using standardized response means. We also assessed agreement between the measures. There was some level of convergence and agreement between the measures in terms of utility score but divergence in the concepts measured by the descriptive systems. Both instruments displayed known-group validity, with significant differences between severity groups, and generally slightly larger effect sizes for the NEWQOL-6D across the epilepsy-specific indicators. Evidence for responsiveness was less clear, with small to moderate standardized response means demonstrating different levels of change across different indicators. There was an overall tendency for the NEWQOL-6D to better reflect differences across groups, but this does not translate into large absolute utility differences. Both the EQ-5D-3L and the NEWQOL-6D show some evidence of validity for providing utility values for economic evaluations in newly diagnosed focal epilepsy. Copyright © 2017 International Society for Pharmacoeconomics and Outcomes Research (ISPOR). Published by Elsevier Inc. All rights reserved.

An overview of self-administered health literacy instruments.

PubMed

O Neill, Braden; Gonçalves, Daniela; Ricci-Cabello, Ignacio; Ziebland, Sue; Valderas, Jose

2014-01-01

With the increasing recognition of health literacy as a worldwide research priority, the development and refinement of indices to measure the construct is an important area of inquiry. Furthermore, the proliferation of online resources and research means that there is a growing need for self-administered instruments. We undertook a systematic overview to identify all published self-administered health literacy assessment indices to report their content and considerations associated with their administration. A primary aim of this study was to assist those seeking to employ a self-reported health literacy index to select one that has been developed and validated for an appropriate context, as well as with desired administration characteristics. Systematic searches were carried out in four electronic databases, and studies were included if they reported the development and/or validation of a novel health literacy assessment measure. Data were systematically extracted on key characteristics of the instruments: breadth of construct ("generic" vs. "content- or context- specific" health literacy), whether it was an original instrument or a derivative, country of origin, administration characteristics, age of target population (adult vs. pediatric), and evidence for validity. 35 articles met the inclusion criteria. There were 27 original instruments (27/35; 77.1%) and 8 derivative instruments (8/35; 22.9%). 22 indices measured "general" health literacy (22/35; 62.9%) while the remainder measured condition- or context- specific health literacy (13/35; 37.1%). Most health literacy measures were developed in the United States (22/35; 62.9%), and about half had adequate face, content, and construct validity (16/35; 45.7%). Given the number of measures available for many specific conditions and contexts, and that several have acceptable validity, our findings suggest that the research agenda should shift towards the investigation and elaboration of health literacy as a construct itself, in order for research in health literacy measurement to progress.

Clinical composite measures of disease activity and damage used to evaluate patients with systemic lupus erythematosus: A systematic literature review.

PubMed

Castrejón, Isabel; Rúa-Figueroa, Iñigo; Rosario, María Piedad; Carmona, Loreto

2014-01-01

To determine the most appropriate indices to evaluate the disease activity and damage in patients with sytemic lupus erythematosus (SLE). A systematic literature search was performed to identify validation studies of indices used to evaluate disease activity and damage. We collected information for each instrument on every aspect of validation including feasibility, reliability, validity and sensitivity to change using ad hoc forms. A total of 38 articles were included addressing the validation of 6 composite indices to evaluate disease activity (BILAG, ECLAM, SLAM, SLEDAI, LAI and SLAQ); and 3 indices to evaluate damage (SLICC/ACE-DI, LDIQ and BILD). Only the SLAQ, LIDIQ and the BILD were self-administered. Feasibility and internal consistency was only studied in 3 indices (BILAG, SLAQ and SDI) with a Cronbach's α ranging from 0.35 to 0.87. The intra-observer reliability was examined by the intraclass correlation coefficient for BILAG with a result of 0.48 (95%CI: 0,23-0,81) and using analysis of variance for SLAM-R (0,78), SLEDAI (0,33) and the LAI (0,81). The inter-observer feasibility was evaluated using the correlation coefficient for ECLAM (0,90-0,93), the SLAM (0,86) and MEX-SLEDAI (0,97-0,89). The construct validity was examined by means of convergence with other instruments, specifically with global assessment by the physician, with similar results between indices (0,48-0,75). Lastly, responsiveness was tested in all indices except LAI, SDI and LDIQ, with a standardized response mean ranging from 0.12 to 0.75. Although multiple instruments have been validated for use in SLE it was not possible to find direct evidence of which is the most appropriate. BILAG and SLEDAI, with moderate feasibility and low responsiveness, are the 2 indices with a most complete validation and more extensively used. Copyright © 2013 Elsevier España, S.L.U. All rights reserved.

Identification of reference genes for RT-qPCR analysis in peach genotypes with contrasting chilling requirements.

PubMed

Marini, N; Bevilacqua, C B; Büttow, M V; Raseira, M C B; Bonow, S

2017-05-25

Selecting and validating reference genes are the first steps in studying gene expression by reverse transcriptase-quantitative polymerase chain reaction (RT-qPCR). The present study aimed to evaluate the stability of five reference genes for the purpose of normalization when studying gene expression in various cultivars of Prunus persica with different chilling requirements. Flower bud tissues of nine peach genotypes from Embrapa's peach breeding program with different chilling requirements were used, and five candidate reference genes based on the RT-qPCR that were useful for studying the relative quantitative gene expression and stability were evaluated using geNorm, NormFinder, and bestKeeper software packages. The results indicated that among the genes tested, the most stable genes to be used as reference genes are Act and UBQ10. This study is the first survey of the stability of reference genes in peaches under chilling stress and provides guidelines for more accurate RT-qPCR results.

Y balance test has no correlation with the Stability Index of the Biodex Balance System.

PubMed

Almeida, Gabriel Peixoto Leão; Monteiro, Isabel Oliveira; Marizeiro, Débora Fortes; Maia, Laísa Braga; de Paula Lima, Pedro Olavo

2017-02-01

A cross-sectional study design. The Stability Index of the Biodex Balance System (SI-BBS) and Y Balance Test (YBT) has been used in studies assessing postural stability but no studies have verified the association of the YBT with the SI-BBS. To analyze the association of the Y Balance Test (YBT) with the Stability Index of the Biodex Balance System (SI-BBS) to evaluate postural stability. Forty participants who engaged in recreational physical activities, 12 of whom had a history of injury to the lower limbs. Was used the SI-BBS and the anterior, posterolateral, posteromedial, and composite measures of the YBT. The order of execution of the tests and of the lower limbs evaluated was randomized and blind tested by two evaluators. Pearson's correlation coefficient was used to check the strength of the relationship between the distances achieved on the YBT and the SI-BBS. The YBT showed excellent reliability in the anterior, posteromedial, and posterolateral directions. However, the YBT showed no statistically significant correlation with any variables in the SI-BBS, indicating poor validity between YBT and SI-BBS assessments of postural stability in people with and without history of lower limb injuries. The results of this study showed the YBT is not correlated with the SI-BBS as an assessment of postural stability. This finding has implications for researchers and clinicians using YBT results as the only measure of postural stability. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

PubMed

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

2013-12-01

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

Stability of the Medial Olivocochlear Reflex as Measured by Distortion Product Otoacoustic Emissions

PubMed Central

Abdala, Carolina

2015-01-01

Purpose The purpose of this study was to assess the repeatability of a fine-resolution, distortion product otoacoustic emission (DPOAE)–based assay of the medial olivocochlear (MOC) reflex in normal-hearing adults. Method Data were collected during 36 test sessions from 4 normal-hearing adults to assess short-term stability and 5 normal-hearing adults to assess long-term stability. DPOAE level and phase measurements were recorded with and without contralateral acoustic stimulation. MOC reflex indices were computed by (a) noting contralateral acoustic stimulation-induced changes in DPOAE level (both absolute and normalized) at fine-structure peaks, (b) recording the effect as a vector difference, and (c) separating DPOAE components and considering a component-specific metric. Results Analyses indicated good repeatability of all indices of the MOC reflex in most frequency ranges. Short- and long-term repeatability were generally comparable. Indices normalized to a subject's own baseline fared best, showing strong short- and long-term stability across all frequency intervals. Conclusions These results suggest that fine-resolution DPOAE-based measures of the MOC reflex measured at strategic frequencies are stable, and natural variance from day-to-day or week-to-week durations is small enough to detect between-group differences and possibly to monitor intervention-related success. However, this is an empirical question that must be directly tested to confirm its utility. PMID:25320951

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.

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.

How Does the Gibbs Inequality Condition Affect the Stability and Detachment of Floating Spheres from the Free Surface of Water?

PubMed

Feng, Dong-xia; Nguyen, Anh V

2016-03-01

Floating objects on the air-water interfaces are central to a number of everyday activities, from walking on water by insects to flotation separation of valuable minerals using air bubbles. The available theories show that a fine sphere can float if the force of surface tension and buoyancies can support the sphere at the interface with an apical angle subtended by the circle of contact being larger than the contact angle. Here we show that the pinning of the contact line at the sharp edge, known as the Gibbs inequality condition, also plays a significant role in controlling the stability and detachment of floating spheres. Specifically, we truncated the spheres with different angles and used a force sensor device to measure the force of pushing the truncated spheres from the interface into water. We also developed a theoretical modeling to calculate the pushing force that in combination with experimental results shows different effects of the Gibbs inequality condition on the stability and detachment of the spheres from the water surface. For small angles of truncation, the Gibbs inequality condition does not affect the sphere detachment, and hence the classical theories on the floatability of spheres are valid. For large truncated angles, the Gibbs inequality condition determines the tenacity of the particle-meniscus contact and the stability and detachment of floating spheres. In this case, the classical theories on the floatability of spheres are no longer valid. A critical truncated angle for the transition from the classical to the Gibbs inequality regimes of detachment was also established. The outcomes of this research advance our understanding of the behavior of floating objects, in particular, the flotation separation of valuable minerals, which often contain various sharp edges of their crystal faces.

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)

Psychometric Properties of Eating Disorder Instruments in Black and White Young Women: Internal Consistency, Temporal Stability, and Validity

ERIC Educational Resources Information Center

Bardone-Cone, Anna M.; Boyd, Clarissa A.

2007-01-01

Most of the major instruments in the eating disorder field have documented psychometric support only in predominantly White samples. The current study examined the internal consistency, temporal stability, and convergent and discriminant validity of a variety of eating disorder measures in Black (n = 97) and White (n = 179) female undergraduates.…

Bioremediation of Contaminated Lake Sediments and Evaluation of Maturity Indicies as Indicators of Compost Stability

PubMed Central

Rekha, P.; Suman Raj, D. S.; Aparna, C.; Bindu, V. Hima; Anjaneyulu, Y.

2005-01-01

Land contamination is one of the widely addressed problems, which is gaining importance in many developed and developing countries. International efforts are actively envisaged to remediate contaminated sites as a response to adverse health effects. Popular conventional methodologies only transfer the phase of the contaminant involving cost intensive liabilities besides handling risk of the hazardous waste. Physico-chemical methods are effective for specific wastes, but are technically complex and lack public acceptance for land remediation. “Bioremediation”, is one of the emerging low-cost technologies that offer the possibility to destroy various contaminants using natural biological activities. Resultant non -toxic end products due to the microbial activity and insitu applicability of this technology is gaining huge public acceptance. In the present study, composting is demonstrated as a bioremediation methodology for the stabilization of contaminated lake sediments of Hyderabad, A.P, India. Lake sediment contaminated with organics is collected from two stratums – upper (0.25 m) and lower (0.5m) to set up as Pile I (Upper) and Pile II (Lower) in the laboratory. Lime as a pretreatment to the lake sediments is carried out to ensure metal precipitation. The pretreated sediment is then mixed with organic and inorganic fertilizers like cow dung, poultry manure, urea and super phosphate as initial seeding amendments. Bulking agents like sawdust and other micronutrients are provided. Continuous monitoring of process control parameters like pH, moisture content, electrical conductivity, total volatile solids and various forms of nitrogen were carried out during the entire course of the study. The stability of the compost was evaluated by assessing maturity indices like C/N, Cw (water soluble carbon), CNw (Cw/Nw), nitrification index (NH4/NO−3), Cation Exchange Capacity (CEC), germination index, humification ratio, compost mineralization index (ash content/oxidizable carbon), sorption capacity index (CEC/oxidizable carbon). Enzyme activities of agricultural interest like urease, phosphatase, β-glucosidase, dehydrogenase and BAA-hydrolyzing protease, which are involved in the nitrogen, phosphorus and carbon cycles, were also assessed. Total content of macro and micronutrients in the final compost was also determined to assess the fertilizer value. The studies revealed that composting could be applied as a remediation technology after removing the top sediment. The maturity indices that are evaluated from the present study can be used to validate the success of the remediation technology. PMID:16705825

How Low Can You Go? Low Densities of Poly(ethylene glycol) Surfactants Attract Stealth Proteins.

PubMed

Seneca, Senne; Simon, Johanna; Weber, Claudia; Ghazaryan, Arthur; Ethirajan, Anitha; Mailaender, Volker; Morsbach, Svenja; Landfester, Katharina

2018-06-25

It is now well-established that the surface chemistry and "stealth" surface functionalities such as poly(ethylene glycol) (PEG) chains of nanocarriers play an important role to decrease unspecific protein adsorption of opsonizing proteins, to increase the enrichment of specific stealth proteins, and to prolong the circulation times of the nanocarriers. At the same time, PEG chains are used to provide colloidal stability for the nanoparticles. However, it is not clear how the chain length and density influence the unspecific and specific protein adsorption keeping at the same time the stability of the nanoparticles in a biological environment. Therefore, this study aims at characterizing the protein adsorption patterns depending on PEG chain length and density to define limits for the amount of PEG needed for a stealth effect by selective protein adsorption as well as colloidal stability during cell experiments. PEG chains are introduced using the PEGylated Lutensol AT surfactants, which allow easy modification of the nanoparticle surface. These findings indicate that a specific enrichment of stealth proteins already occurs at low PEG concentrations; for the decrease of unspecific protein adsorption and finally the colloidal stability a full surface coverage is advised. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Proline substitution independently enhances H-2D(b) complex stabilization and TCR recognition of melanoma-associated peptides.

PubMed

Uchtenhagen, Hannes; Abualrous, Esam T; Stahl, Evi; Allerbring, Eva B; Sluijter, Marjolein; Zacharias, Martin; Sandalova, Tatyana; van Hall, Thorbald; Springer, Sebastian; Nygren, Per-Åke; Achour, Adnane

2013-11-01

The immunogenicity of H-2D(b) (D(b)) restricted epitopes can be significantly increased by substituting peptide position 3 to a proline (p3P). The p3P modification enhances MHC stability without altering the conformation of the modified epitope allowing for T-cell cross-reactivity with the native peptide. The present study reveals how specific interactions between p3P and the highly conserved MHC heavy chain residue Y159 increase the stability of D(b) in complex with an optimized version of the melanoma-associated epitope gp10025-33 . Furthermore, the p3P modification directly increased the affinity of the D(b)/gp10025-33 -specific T-cell receptor (TCR) pMel. Surprisingly, the enhanced TCR binding was independent from the observed increased stability of the optimized D(b)/gp10025-33 complex and from the interactions formed between p3P and Y159, indicating a direct effect of the p3P modification on TCR recognition. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

EO-1 Hyperion Reflectance Time Series at Calibration and Validation Sites: Stability and Sensitivity to Seasonal Dynamics

NASA Technical Reports Server (NTRS)

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

2013-01-01

This study evaluated Earth Observing 1 (EO-1) Hyperion reflectance time series at established calibration sites to assess the instrument stability and suitability for monitoring vegetation functional parameters. Our analysis using three pseudo-invariant calibration sites in North America indicated that the reflectance time series are devoid of apparent spectral trends and their stability consistently is within 2.5-5 percent throughout most of the spectral range spanning the 12-plus year data record. Using three vegetated sites instrumented with eddy covariance towers, the Hyperion reflectance time series were evaluated for their ability to determine important variables of ecosystem function. A number of narrowband and derivative vegetation indices (VI) closely described the seasonal profiles in vegetation function and ecosystem carbon exchange (e.g., net and gross ecosystem productivity) in three very different ecosystems, including a hardwood forest and tallgrass prairie in North America, and a Miombo woodland in Africa. Our results demonstrate the potential for scaling the carbon flux tower measurements to local and regional landscape levels. The VIs with stronger relationships to the CO2 parameters were derived using continuous reflectance spectra and included wavelengths associated with chlorophyll content and/or chlorophyll fluorescence. Since these indices cannot be calculated from broadband multispectral instrument data, the opportunity to exploit these spectrometer-based VIs in the future will depend on the launch of satellites such as EnMAP and HyspIRI. This study highlights the practical utility of space-borne spectrometers for characterization of the spectral stability and uniformity of the calibration sites in support of sensor cross-comparisons, and demonstrates the potential of narrowband VIs to track and spatially extend ecosystem functional status as well as carbon processes measured at flux towers.