Method Validation and Transfer

  • Frank J. Diana


Analytical methods used in testing pharmaceutical stability samples need to be validated to the current standards. Often the same methods are employed for release and stability testing which facilitates method validation and allows for the use of initial release data for time zero stability as long as samples are packaged and placed on stability in a reasonably short period of time (typically 30 days). Transfer of these methods between laboratories is also facilitated by the development and validation of the same methods for release and stability testing. Stability testing will typically include appearance and a test for assay and degradation products for all dosage forms. The assay method is typically proven to be stability indicating and specific, meaning that all degradation products and synthetic impurities, known or unknown, as well as inactive components are separated from the active ingredient thereby allowing for the accurate measurement of the strength/potency of the dosage form. Similarly, to accurately measure a degradation product level in finished product, all other degradation products and synthetic impurities should be resolved from the peak of interest. Additional tests are typically performed depending on the dosage form, for example dissolution or drug release for solid dosage forms, pH, preservatives and anti-oxidant content for liquid, topical or parenteral dosage forms.

Method validation is covered in the current Good Manufacturing Practices (cGMPs) under section 211.165(e) which indicates that “The accuracy, sensitivity, specificity, and reproducibility of tests methods …shall be established and documented”. Such validation and documentation may be accomplished in accordance with 211.194(a) (2) which includes the need to “indicate the location of data that establish that the methods used in the testing of the sample meet proper standards of accuracy and reliability as applied to the product tested”. Methods included in recognized standard references such as the current USP/NF are understood to be validated. “The suitability of all testing methods used shall be verified under actual conditions of use” (211.194). For new products for which methods are developed, analytical method validation as described in this chapter will be necessary; for methods already included in the USP, method verification will suffice.


Dosage Form Acceptance Criterion Method Transfer Force Degradation Study Analytical Method Validation 
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Copyright information

© Springer Science+Business Media, LLC 2009

Authors and Affiliations

  1. 1.Endo PharmaceuticalsChadds FordUSA

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