A simple, precise, accurate and rapid high performance thin layer chromatographic method has been developed and validated for the estimation of telmisartan and hydrochlorothiazide simultaneously in combined dosage forms. The stationary phase used was precoated silica gel 60F254. The mobile phase used was a mixture of chloroform: methanol: toluene (2:5:5 v/v/v). The detection of spots was carried out at 272 nm. The method was validated in terms of linearity, accuracy, precision and specificity.

Two simple and sensitive visible spectrophotometric methods (A and B) have been developed for the quantitative estimation of nitazoxanide, in bulk drug and pharmaceutical dosage forms. Methods were based on the formation of reddish yellow coloured and green coloured chromogens, which were measured at 544 nm and 715 nm, respectively. The results obtained with the proposed methods are in good agreement with the labelled amounts when tablet dosage forms were analysed.

Valdecoxib is a nonsteroidal antiinflammatory drug, and it is listed in class 2 of biopharmaceutic classification of drugs. Valdecoxib is a poorly water-soluble and highly permeable drug. In the present study a new dissolution medium was developed, as there is no official dissolution medium available in the literature. The composition of the dissolution medium was selected on the basis of solubility data at 37°. Solubility data revealed that addition of surfactant may be suitable as dissolution medium.

Several gaps in current regulatory guidelines that govern the analytical method life cycle for the testing of biopharmaceuticals are identified. Strategic guidance on how to monitor and control the life cycle of an analytical test method is provided in this article. Analytical method transfer, analytical method component equivalency, and analytical method comparability protocols are discussed in light of risk-based strategies for validation extensions. The use of an analytical method maintenance program is suggested to control over time the predictable risk to patients and firm.

The design of pharmaceutical water systems has always been part science and part alchemy, and unfortunately, it is not likely to change in the near future. Daily rhetoric is rife with statements from informed and intelligent people alleging design requirements that do not actually exist.

The problem is that if you do not have documentation from a reliable source that supports or contradicts these statements, they are nearly impossible to refute. As a result, they are often incorporated into system design.

Purpose. A sensitive, robust, and selective liquid chromatographic – tandem mass spectrometric method (LC-MS/MS) was developed and validated for paroxetine quantification in human EDTA plasma. Methods. Sample preparation was based on liquid-liquid extraction using a mixture of ethyl acetate/hexane (50/50; v/v) to extract the drug and internal standard from plasma. Chromatography was performed on a C-18 analytical column and the retention times were 1.6 and 1.7 for paroxetine and fluoxetine (IS), respectively.

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This article is the second of a series of articles detailing the development of near-infrared (NIR) methods for solid dosage-form analysis. Experiments were conducted at the Duquesne University Center for Pharmaceutical Technology to demonstrate a method for developing and validating NIR models for the analysis of active pharmaceutical ingredient (API) content and hardness of a solid dosage form. Robustness and cross-validation testing were used to optimize the API content and hardness models.

Many industry professionals know that analytical testing for biopharmaceuticals for all raw materials, production in-process stages, and final containers must be validated, and they generally understand how this can be achieved. Many of us even understand the basic concepts of laboratory compliance and production process quality. However, how exactly are analytical test method performance and process robustness related and how do they depend on each other? Furthermore, how do we monitor and maintain the accuracy and reliability of analytical methods long after validation completion to ensure the suitability of these methods for measuring process quality?

This article describes a software solution for automating the chromatographic method validation process starting from experimental planning, data acquisition and processing, through final report generation in a seamless manner. All experimental planning and calculations are accomplished within the chromatography data software and, thus, are structurally validated, secure, and audit trailed. Highlights of the software are provided, including benefits to the analyst. The analysis of important method validation characteristics such as linearity, accuracy, and precision is automated. These characteristics and their acceptance criteria can be captured in a method template, which adheres to the company's standard operating procedure. This template method can then be used repeatedly by other scientists in the organization, hence, eliminating the need to create a new experimental plan each time a new validation is conducted

The chromatographic analytical method validation process involves a series of activities that are currently conducted in separate “technology islands” using tools that exist for each activity.This article describes a software program that provides an overarching automation technology for analytical method validation and brings together the individual activities under one integrated-technology platform that is adapted to multiple instruments and data systems.

To ensure compliance with quality and safety standards, the United States, Europe,Japan, and other countries have published compendia, or pharmacopeias, that describe official test methods for many marketed drug products. For example, compendial analytical methods found in United States Pharmacopeia 25 (USP 25) are legally recognized analytical procedures under section 501 (b) of the Federal Food, Drug, and Cosmetic Act. For these compendial methods, USP provides regulatory guidance for method validation (1). In addition, validation of analytical methods is covered by the United States Code of Federal  egulations (CFR). Specific references are 21 CFR 211.165 (e) and 21 CFR 211.194 (a).

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