scholarly journals Statistical method for the determination of equivalence of automated test procedures

2003 ◽  
Vol 25 (6) ◽  
pp. 123-127 ◽  
Author(s):  
K. Rick Lung ◽  
Mary A. Gorko ◽  
Jennifer Llewelyn ◽  
Norman Wiggins
Keyword(s):  
Test Methods ◽  
Test Method ◽  
Content Uniformity ◽  
Solid Dosage Forms ◽  
Test Procedures ◽  
Solid Dosage ◽  
Automated Test ◽  
Student’S T ◽  
Manual Test

In the development of test methods for solid dosage forms, manual test procedures for assay and content uniformity often precede the development of automated test procedures. Since the mode of extraction for automated test methods is often slightly different from that of the manual test method, additional validation of an automated test method is usually required. In addition to compliance with validation guidelines, developers of automated test methods are often asked to demonstrate equivalence between the manual and automated test methods. There are problems associated with using the traditional zero-difference hypothesis tests (such as the Student's t-test) for demonstrating equivalence. The use of the Westlake Interval and Schuirmann's Two One-sided test as more rigorous methods of demonstrating equivalence is discussed.

scholarly journals Validation of a UV Spectrophotometric Method for the Determination of Melatonine in Solid Dosage Forms

2001 ◽  
Vol 84 (5) ◽  
pp. 1352-1357 ◽  
Author(s):  
Renato F Pérez ◽  
Igor G Lemus ◽  
Rony V Bocic ◽  
Mauricio V Pérez ◽  
Rubén García-Madrid
Keyword(s):  
Accurate Method ◽  
The United States ◽  
Dosage Forms ◽  
Content Uniformity ◽  
Solid Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Solid Dosage ◽  
Pharmaceutical Form ◽  
Ph Range

Abstract The aim of the work described in this paper was to provide a fast, easy, inexpensive, precise, and accurate method for the determination of melatonine in solid pharmaceutical dosage forms. The developed method is based on a UV first-derivative spectrophotometric determination, which exhibits excellent linearity in aqueous solutions (r2 = 0.996) for analyte concentrations of 1.5–4.5 mg/dL within a pH range of 5–9. Neither excipients present in the formulation nor indole adulterants, such as tryptophan (up to 5%), interfere with the assay. A study of variation parameters showed that sonication temperature was the main factor for successful determination. At temperatures of <45°C, the sample dissolved completely, and accurate spectrophotometric measurements were obtained. A study was conducted of all the parameters established by the United States Pharmacopeia, 23rd Rev., to validate an analytical method for a solid pharmaceutical form, i.e., linearity, range, accuracy, precision, and specificity. All the parameters were in accordance with the acceptance criteria of the Comité de Guías Oficiales de Validación de la Dirección General de Control de Insumos para la Salud de Méjico. In addition, robustness and content uniformity tests were performed to substantiate the usefulness of the method.

Determination of Aspirin and Salicylic Acid by Reverse-Phase Liquid Chromatography

1987 ◽  
Vol 70 (6) ◽  
pp. 964-966
Author(s):  
Dorothy R Heidemann ◽  
Edward S Schulenberg ◽  
William H Smith
Keyword(s):  
Salicylic Acid ◽  
Dosage Forms ◽  
Solid Dosage Forms ◽  
Reverse Phase ◽  
Solid Dosage ◽  
Reverse Phase Liquid Chromatography ◽  
Sample Extraction ◽  
Phase Liquid ◽  
Phase Column

Abstract Buffered solid dosage forms containing aspirin, magnesium hydroxide, and aluminum hydroxide are blended with acidic ethanol to extract the aspirin and salicylic acid rapidly. The resulting preparation is then immediately injected onto a 4.6 mm x 3 cm 5 (im reverse-phase column. Aspirin and free salicylic acid are determined simultaneously. The run time is <2 min. The total time from the initiation of sample extraction to completion of the separation is <5 min.

Methods to Evaluate Cleaners and Sanitizers

1982 ◽  
Vol 45 (13) ◽  
pp. 1257-1260 ◽  
Author(s):  
DALE L. SCHEUSNER
Keyword(s):  
Test Methods ◽  
Test Method ◽  
Test Results ◽  
Standard Laboratory ◽  
Test Procedures ◽  
Laboratory Methods ◽  
Product Use ◽  
Cellulose Sponge ◽  
Equivalent Test ◽  
Recovery Methods

Methods to evaluate germicides can be grouped into three categories: standard laboratory tests, in-use tests and simulated-use tests. Standard laboratory methods, such as the Available Chlorine Germicidal Equivalent test, are specifically defined for reproducibility in any laboratory by any operator, but the test results often lack relevance to actual product-use conditions. In-use test methods are relevant to product-use; however, in-use test procedures do not permit proper controls to be included in the organism recovery methods. Contact plates give an estimate of organism numbers which is only 25% of the theoretical number of organisms present. Organism recovery using a swab, cellulose sponge or tube sampler give estimates of organisms ranging from 91 to 111% of theoretical. The tube sampler is a 1-in. length of flexible tubing having a 1-in. interior diameter and a smooth end, which can make a water-tight seal on a flat surface. Simulated use testing yields data which are relevant to actual product-use. A cafeteria tray is soiled, inoculated and cleaned in a manner to simulate actual product-use. This test method permits the necessary controls to be used. Tray-test reproducibility is as good as that of the other recovery methods tested and organism recovery is quantitative. The tray test provides a means for determining biological cleaning where the effect of both cleaning and germicidal activity are measured together.

A statistical support for using spectroscopic methods to validate the content uniformity of solid dosage forms

2003 ◽  
Vol 92 (7) ◽  
pp. 1526-1530 ◽  
Author(s):  
Tonglei Li ◽  
Amy D. Donner ◽  
Candice Y. Choi ◽  
Gerard P. Frunzi ◽  
Kenneth R. Morris
Keyword(s):  
Dosage Forms ◽  
Content Uniformity ◽  
Spectroscopic Methods ◽  
Solid Dosage Forms ◽  
Solid Dosage ◽  
Statistical Support
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