Validation

1月 20, 2015

Application of Total Error Strategy in Validation of Affordable and Accessible UV-Visible Spectrophotometric Methods for Quality Control of Poor Medicines

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http://www.scirp.org/journal/PaperInformation.aspx?PaperID=53326#.VL3BYyzQrzE

ABSTRACT

In the framework of fighting against the poor quality medicines sold in developing countries using classical analytical methods easily accessible in those countries, four UV-Visible spectrophotometric methods for one antimalarial (quinine) and two antibiotics (amoxicillin and metronidazole) have been developed and validated according to the total error strategy using the accuracy profiles as a decision tool. The dosing range was 2 – 10 μg/mL (for quinine sulfate in tablet), 4 – 12 μg/mL (for quinine bichlorhydrate in oral drop-metronidazole benzaote in oral suspension) and 15 – 35 μg/mL (for amoxicillin trihydrate in capsule). The validated methods were then applied in determining the content of some analogous medicines sold in the Democratic Republic of Congo. Thus, the proposed UV-Visible spectrophotometric methods are simple and suitable to quantify quinine, amoxicillin and metronidazole in different pharmaceutical forms.

Cite this paper

Mbinze, J. , Mpasi, J. , Maghe, E. , Kobo, S. , Mwanda, R. , Mulumba, G. , Bolande, J. , Bayebila, T. , Amani, M. , Hubert, P. and Marini, R. (2015) Application of Total Error Strategy in Validation of Affordable and Accessible UV-Visible Spectrophotometric Methods for Quality Control of Poor Medicines. American Journal of Analytical Chemistry, 6, 106-117. doi: 10.4236/ajac.2015.62010.

References

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[24] Boulanger, B., Chiap, P., Dewé, W., Crommen, J. and Hubert, Ph. (2003) An Analysis of the SFSTP Guide on Validation of Chromatographic Bioanalytical Methods: Progresses and Limitations. Journal of Pharmaceutical and Biomedical Analysis, 32, 753-765.
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http://dx.doi.org/10.1016/j.talanta.2005.07.026                                                             eww150120lx

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12月 19, 2014

Development and Validation of a Stability-Indicating RP-HPLC Method for Determination of Darifenacin Hydrobromide in Bulk Drugs

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http://www.scirp.org/journal/PaperInformation.aspx?PaperID=52387#.VJOMGcCAM4

ABSTRACT

An isocratic stability-indicating reversed phase high performance liquid chromatographic method (RP-HPLC) was developed for determination of process related impurities and assay of darifenacin hydrobromide (DRF) in bulk drugs. DRF was subjected to various stress conditions such as hydrolysis (acid, base, and neutral), oxidation, photolysis and thermal degradation as per International Conference on Harmonization (ICH Q1A(R2) and Q1B) prescribed conditions to investigate the stability-indicating ability of the method. Significant degradation was observed during acidic hydrolysis and oxidative stress conditions. The chromatographic separation was accomplished on a Prodigy C8 column (250 × 4.6 mm, 5 μm) with mobile phase consisting of 0.05 M ammonium acetate (pH adjusted to 7.2 by using ammonia solution) and methanol (36% acetonitrile) in 35:65 v/v ratio in an isocratic elution mode at a flow rate of 1.0 mL/min at 25°C. Detection of analytes was carried out using photo diode array detector at a wavelength of 215 nm. The developed LC method was validated with respect to accuracy, linearity, precision, limits of detection and quantitation and robustness as per ICH guidelines.

Cite this paper

Nazeerunnisa, M. , Garikapati, L. and Bethanabhatla, S. (2014) Development and Validation of a Stability-Indicating RP-HPLC Method for Determination of Darifenacin Hydrobromide in Bulk Drugs. American Journal of Analytical Chemistry, 5, 1239-1248. doi: 10.4236/ajac.2014.517130.

References

[1] Hashim, H. and Abrams, P. (2005) Treatment of Overactive Bladder Syndrome and Detrusor over Activity. Reviews in Gynaecological Practice, 5, 243-250.
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[2] Haab, F., Stewart, L. and Dwyer, P. (2004) Darifenacin an M3 Selective Receptor Antagonist, Is an Effective and Well-Tolerated Once-Daily Treatment for Overactive Bladder. European Urology, 45, 420-429.
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[3] Thomas, S., Paul, S.K., Shandilya, S., Agarwal, A., Saxena, N., Awasthi, A.K., Matta, H., Vir, D. and Mathel, C.S. (2012) Identification and Structural Elucidation of Two Process Impurities and Stress Degradants in Darifenacin Hydrobromide Active Pharmaceutical Ingredient by LC-ESI/MSn. Analyst, 137, 3571-3582.
http://dx.doi.org/10.1039/c2an35454c
[4] Murthya, M.V., Krishnaiah, Ch., Srinivas, K., Rao, K.S., Kumar, N.R. and Mukkanti, K. (2013) Development and Validation Of RP-UPLC Method for the Determination of Darifenacin Hydrobromide, Its Related Compounds and Its Degradation Products Using Design of Experiments. Journal of Pharmaceutical and Biomedical Analysis, 72, 40-50.
http://dx.doi.org/10.1016/j.jpba.2012.09.013
[5] Meneghini, L.Z., Junqueira, C., Andrade, A.S., Salazar, F.R., Codevilla, C.F., Froehlich, P.E. and Bergold, A.M. (2011) Chemometric Evaluation of Darifenacin Hydrobromide Using a Stability-Indicating Reversed-Phase LC Method. Journal of Liquid Chromatography & Related Technologies, 34, 2169-2184.
http://dx.doi.org/10.1080/10826076.2011.585486
[6] Murthy, M.V., Ragavacharyulu, K.S.V., Krishnaiah, C., Srinivas, K., Mukkanti, K. and Kumar, N.R. (2009) A Stereo-selective, Stability-Indicating Validated LC-Assay Method for the Separation and Quantification of Darifenacin and Its Enantiomer. Analytical Chemistry: An Indian Journal, 8, 491-493.
[7] Radhakrishnanand, P., Rao, D.V.S. and Himabindu, V. (2008) A Validated LC Method for Determination of the Enantiomeric Purity of Darifenacin in Bulk Drug and Extended Release Tablets. Chromatographia, 68, 1059-1062.
http://dx.doi.org/10.1365/s10337-008-0795-z
[8] Srinivas, K., Reddy, S.R., Reddy, G.M., Dubey, P.K., Chakravarthy, A.K. and Reddy, P.P. (2009) Synthesis and Characterization of Novel and Potential Impurities of Darifenacin, a Potent Muscarinic M3 Receptor Antagonist. Rasayan Journal of Chemistry, 2, 151-155.
[9] Kaye, B., Herron, W.J., Macrae, P.V., Robinson, S., Stopher, D.A., Venn, R.F. and Wild, W. (1996) Rapid, Solid Phase Extraction Technique for the High-Throughput Assay of Darifenacin in Human Plasma. Analytical Chemistry, 68, 1658-1660.
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[11] ICH Q1A (R2) (2003) International Conference on Harmonization, Stability Testing of New Drug Substance and Products.                                                                                                                              eww141219lx
12月 11, 2014

Early Detection of Mild Alzheimer’s Disease in Filipino Elderly: Validation of the Montreal Cognitive Assessment-Philippines (MoCA-P)

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http://www.scirp.org/journal/PaperInformation.aspx?PaperID=52116#.VIkCu8nQrzE

ABSTRACT

Background: The Montreal Cognitive Assessment (MoCA) is a useful instrument employed by clinicians to detect cognitive impairment and diagnose probable Alzheimer’s Disease (AD) while in its early stages. Methods: A cross-sectional study was conducted to determine the diagnostic validity of the Philippine version of the MoCA (MoCA-P) among 1385 community-dwelling Filipino elderly from Marikina City, Metro Manila. Results: 509 controls and 97 elderly with probable AD and a Clinical Dementia Rating (CDR) global score of 0.5 were included in the analysis. Analysis of variance showed that the AD group was older (p < 0.05) and had fewer years of education (p < 0.05). The optimal cut-off score to differentiate controls from those with probable AD was 20/21, with a sensitivity of 0.835 and a specificity of 0.723, and area under the curve (AUC) of 0.89 (p < 0.001). The positive and negative likelihood ratios were 3.01 and 0.23, respectively; and pre- and post-test odds were 0.0951 and 0.2224, respectively. Logistic regression showed that the odds of scoring < 20 on the MoCA-P increased with advancing age and with education at ≤7 years (p < 0.05). Two points are added to the MoCA-P score for those with ≤7 years of education. Conclusion: The MoCA-P is a valid instrument for the early detection of mild AD among the Filipino elderly.

Cite this paper

Dominguez, J. , Soriano, J. , Magpantay, C. , Orquiza, M. , Solis, W. , Reandelar Jr., M. and Joson, M. (2014) Early Detection of Mild Alzheimer’s Disease in Filipino Elderly: Validation of the Montreal Cognitive Assessment-Philippines (MoCA-P). Advances in Alzheimer’s Disease, 3, 160-167. doi: 10.4236/aad.2014.34015.

References

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http://dx.doi.org/10.1016/S0140-6736(05)67889-0
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http://dx.doi.org/10.1177/0891988708316855
[10] Wen, H.B., Zhang, Z.X., Niu, F.S. and Li, L. (2008) The Application of Montreal Cognitive Assessment in Urban Chinese Residents of Beijing. Zonghua Nei Ke Za Zhi (Chinese Journal of Internal Medicine), 47, 36-39.
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[19] Luis, C.A., Keegan, A.P. and Mullan, M. (2009) Cross Validation of the Montreal Cognitive Assessment in Community-Dwelling Older Adults Residing in the Southeastern US. International Journal of Geriatric Psychiatry, 24, 197- 201. http://dx.doi.org/10.1002/gps.2101
[20] Lee, J.Y., Dong, W.L., Cho, S.J., Na, D.L., Jeon, H.J., Kim, S.K., et al. (2008) Brief Screening for Mild Cognitive Impairment in Elderly Outpatient Clinic: Validation of the Korean Version of the Montreal Cognitive Assessment. Journal of Geriatric Psychiatry and Neurology, 21, 104-110.
http://dx.doi.org/10.1177/0891988708316855
[21] Fujiwara, Y., Suzuki, H., Yasunaga, M., Sugiyama, M., Ijuin, M., Sakuma, N., et al. (2010) Brief Screening Tool for Mild Cognitive Impairment in Older Japanese: Validation of the Japanese Version of the Montreal Cognitive Assessment. Geriatrics & Gerontology International, 10, 225-232.
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[22] Memória, C.M., Yassuda, M.S., Nakano, E.Y. and Forlenza, O.V. (2013) Brief Screening for Mild Cognitive Impairment: Validation of the Brazilian Version of the Montreal Cognitive Assessment. International Journal of Geriatric Psychiatry, 28, 34-40. http://dx.doi.org/10.1002/gps.3787
[23] Gomez, F., Zunzunegui, M., Lord, C., Alvarado, B. and Garcia, A. (2013) Applicability of the MoCA-S Test in Populations with Little Education in Colombia. International Journal of Geriatric Psychiatry, 28, 813-820. http://dx.doi.org/10.1002/gps.3885                                                                                            eww141211lx
11月 10, 2014

Rapid and Sensitive CZE Method for Quality Control Analysis of Pharmaceuticals Containing Pseudoephedrine, Triprolidine and Paracetamol

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http://www.scirp.org/journal/PaperInformation.aspx?PaperID=47156#.VGApWGfHRK0

ABSTRACT

A rapid and sensitive CZE (Capillary Zone Electrophoresis) method for pharmaceutical analysis was developed and fully validated. The active compounds: Pseudoephedrine hydrochloride (PSE), Triprolidine hydrochloride (TRI) and Paracetamol (PAR) were separated and quantitatively determined using the tris-borate 30 mM buffer at pH = 9.0 as a Background Electrolyte (BGE). The electrophoretic separation was carried out at 25 kV in an unmodified fused silica capillary of I.D. = 50 μm with a “bubble-cell” for UV detection at 210 nm and 25°C. The separation was reached in about 3 min. After calibration the method was applied for analysis of three commercially available pharmaceutical preparations. The repeatability (RSD%) of migration time (tm) was ranging between 0.47% and 0.90% and of peak areas (A) between 0.63% and 3.64%. The Limit of Detection (LOD) values was of 0.19 μg/mL, 0.31 μg/mL and 0.08 μg/mL for respectively PSE, TRI and PAR. The results obtained in this study showed that the proposed method was useful in routinely analysis of pharmaceuticals.

Cite this paper

Di Berardino, S. and Jasionowska, R. (2014) Rapid and Sensitive CZE Method for Quality Control Analysis of Pharmaceuticals Containing Pseudoephedrine, Triprolidine and Paracetamol. American Journal of Analytical Chemistry, 5, 613-619. doi: 10.4236/ajac.2014.59069.

References

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http://dx.doi.org/10.1039/c1jm11795e
[5] Hegazy, M.A., Khattab, F.E. and Abdelhameed, B.M. (2013) Validated Chromatographic Methods for Determination of Paracetamol, Pseudoephedrine and Cetrizine in Pharmaceutical Formulations. Analytical Chemistry: An Indian Journal, 12, 248-255.
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10月 10, 2014

Validation of the Greek Version of Perceived Stress Questionnaire: Psychometric Properties and Factor Structure in a Population-Based Survey

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http://www.scirp.org/journal/PaperInformation.aspx?PaperID=48880#.VDcrv1fHRK0

Author(s)

Eva Karatza, Dimitra Kourou, Michael Galanakis, Liza Varvogli, Christina Darviri

Affiliation(s)

Postgraduate Course Stress Management and Health Promotion, School of Medicine, University of Athens, Athens, Greece.
Postgraduate Course Stress Management and Health Promotion, School of Medicine, University of Athens, Athens, Greece.
Department of Psychology, Panteion University of Social and Political Sciences, Athens, Greece.
Postgraduate Course Stress Management and Health Promotion, School of Medicine, University of Athens, Athens, Greece.
Postgraduate Course Stress Management and Health Promotion, School of Medicine, University of Athens, Athens, Greece.

ABSTRACT

Perceived Stress Scale (PSQ) adaptation is a measuring tool of perceived stress and evaluation of its psychometric properties, on a population-based survey (Greece). Sample N = 1318 of people has anonymously completed the PSQ, comparing it to the Perceived Stress Scale (PSS) and Depressive, Anxiety and Stress Scale (DASS-21). The factor analysis, has shown that the PSQ includes five main factors (Overload, Worries, Joy, Tension/Fatigue, Harassment), which explain the 54.28% of the phenomenon variance. The Cronbach alpha index was 0.9 approaching the respective reliability factor at the original validation (alpha > 0.9). The test-retest reliability was highly statistically significant with an alpha = +0.86, close to the results of the original validation (r = 0.82). The criterion validity has shown high correlation with the PSS (r = 0.737), plus the fact that the results of the correlation with the DSS-21 (r = 0.597) were satisfactory. The satisfactory results, as it concerns the psychometric properties of the PSQ, make the questionnaire an appropriate measuring tool of the perceived stress of the Greek population.

KEYWORDS

Perceived Stress Questionnaire, Validation, Psychometric Properties, Population-Based Survey

Cite this paper

Karatza, E. , Kourou, D. , Galanakis, M. , Varvogli, L. & Darviri, C. (2014). Validation of the Greek Version of Perceived Stress Questionnaire: Psychometric Properties and Factor Structure in a Population-Based Survey. Psychology, 5, 1268-1284. doi: 10.4236/psych.2014.510139.

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9月 18, 2014

Pedestrian Crash Prediction Models and Validation of Effective Factors on Their Safety (Case Study: Tehran Signalized Intersections)

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http://www.scirp.org/journal/PaperInformation.aspx?PaperID=49798#.VBpYPlfHRK0

Pedestrian Crash Prediction Models and Validation of Effective Factors on Their Safety (Case Study: Tehran Signalized Intersections).

ABSTRACT

The quantity and severity of traffic accidents have increased with the development of machinery life and traffic growth in cities and roads in the past 50 years. Among the road users, pedestrians are the most vulnerable groups to be exposed to high risks. Vehicle crashes with pedestrian are almost inevitable and cause injury or death to pedestrian. Crash investigation and statistical studies indicate that percentage of pedestrian deaths caused by vehicle accidents are much more than all deaths. A considerable amount of accidents occur at signalized and urban intersections which are the intensive crash places. Therefore in this paper appropriate models that could specify safety indicators have been indicated with existing information by characterized parametric and nonparametric variables for twenty signalized intersections. Categories and correlations of variables also have been investigated. Three models including Regression, Poisson, and Negative binomial with defined variables have been determined. T and chi square tests, calibration and comparison of variables have been done by curve fitting. The role of each parameter was specified in pedestrian crashes. Validating models had the following outcomes: Pedestrian crash prediction models were based on none linear relations at intersections. Predictable variables, developing extended linear models and also pedestrian crash prediction are on the basis of Negative binomial distribution which is used due to more data dispersion. As observed, the Negative binomial regression because of its more R2 correlation factor has more validity among other regression models such as linear regression and Poisson. Calibrated models are put into sensitivity analysis to study the effect of each previously mentioned parameter in overall performance. Hence much better perception of future transportation plans can be achieved by development of safety models at planning levels.

Cite this paper

Haghighatpour, P. and Moayedfar, R. (2014) Pedestrian Crash Prediction Models and Validation of Effective Factors on Their Safety (Case Study: Tehran Signalized Intersections). Open Journal of Civil Engineering, 4, 240-254. doi: 10.4236/ojce.2014.43021.
References

 

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eww140918lx
9月 15, 2014

Rapid HPLC Method for Determination of Rebaudioside D in Leaves of Stevia rebaudiana Bertoni Grown in the Southeast of México

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http://www.scirp.org/journal/PaperInformation.aspx?PaperID=49606#.VBZNpaN2W3M

Rapid HPLC Method for Determination of Rebaudioside D in Leaves of Stevia rebaudiana Bertoni Grown in the Southeast of México.

 

 

ABSTRACT

Stevia leaves contain glycosides on which biological activity and sweetening capacity has been reported. Besides the main glycosides—stevioside and rebaudioside A—there are minor glycosides that may contribute to the activity and thus it is important to quantify them. Rebaudioside D is one of the minor glycoside present in S. rebaudiana leaves and there are no reports of a validated method to quantify it. Therefore a simple and sensitive high performance liquid chromatography (HPLC) method was validated for the determination of rebaudioside D in leaves of Stevia rebaudiana B. grown in the southeast of México. HPLC method was performed using a C18 column (250 mm × 4.6 mm, 5 μm) and UV detector set at 210 nm. The mobile phase consisted of 32:68 (v/v) mixture of acetonitrile and sodium phosphate buffer (10 mmol/L, pH 2.6), set to a flow rate of 1.0 ml/min. The calculated parameters were: sensitivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy and precision. The retention time of rebaudioside D was found to be 3.47 min ± 0.04 (S.D.). The calibration curves were linear over the working range (25 – 150 μg/ml), with correlation coefficient ≥0.99 and determination coefficient ≥0.98. The calculated limit of detection (LOD) was 8.53 μg/ml, while the limit of quantitation (LOQ) was 25.85 μg/ml. The percent recoveries of fortified samples were 100% ± 10% and precision relative standard deviation was ≤2.79%. The criteria of validation showed accuracy, linearity, and precision; therefore the method is suitable for quantitative analysis of rebaudioside D in Stevia rebaudiana leaves. Rebaudioside D content (g/100g) in Morita II and Criolla varieties grown in the southeast of Mexico were 0.43 and 0.46, respectively with no significant differences (p > 0.05) between them.

 

 

Cite this paper

Aranda-González, I. , Moguel-Ordoñez, Y. and Betancur-Ancona, D. (2014) Rapid HPLC Method for Determination of Rebaudioside D in Leaves of Stevia rebaudiana Bertoni Grown in the Southeast of México. American Journal of Analytical Chemistry, 5, 813-819. doi: 10.4236/ajac.2014.513090.
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