Analytical method validation is the process of demonstrating that an analytical procedure is suitable for its intended purpose. According to the Code of Federal Regulations (CFR), 21 CFR 211.165(e) the accuracy, sensitivity, specificity and reproducibility of test methods employed by the firm shall be established and documented. Typical validation characteristics include, but are not limited to, Specificity, Linearity, Accuracy, Precision (repeatability, intermediate precision, and reproducibility), Range, Quantitation limit and Ruggedness.
A company recently received the following observation:
….. The accuracy, specificity and reproducibility of test methods have not been established.
Specifically, the specificity studies for the assay test methods … “HPLC Analysis for …” and … “HPLC Analysis for …” were inadequate in that the chromatographic separation of impurities and active peaks was not determined. The studies did not include the fortification of known impurities to test samples to optimize the separation of each component observed in the chromatograms. … studies were performed according to document: SOP …, “Drug Product … Study.” The procedure was deficient in that:
a. … concentrations were not specified.
b. The exposure times for … were not provided.
c. The … study did not follow ICH … Stability although ICH and USP guidelines were referenced in document no.: … “Method Selection, Validation and Verification.”
The test methods were used to assay … and … drug products.
For additional information pertaining to method validation, refer to FDA Guidance document: Q2(R1) Validation of Analytical Procedures: Text and Methodology, FDA Guidance document: Guidance for Industry Q3B(R2) Impurities in New Drug Products and FDA Guidance document: Analytical Procedures and Method Validation for Drugs and Biologics.
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