Analytical method validation as per US-FDA (Part.:I)

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Analytical method validation as per US-FDA (Part.:I)

by Amrita Shetty, 03/04/2021

       I.          I. Reference standard & material.:

Standard for use must be suitable.

It should follow storage, usage condition, handling instruction for reference standard to avoid modification & contamination which lead to additional impurities and inaccurate analysis.

This should be supported by qualification test report, certificate of analysis (COA) which include stability protocol, reports, and impurity profile information.

This is often obtained from USP, European Pharmacopeia, Japanese pharmacopeia, World Health organisation or National institute of Standard and technology

The standard for biological product is obtained from CBER.

Reference material suitability is determined is not really captured by Drug product or product release test are

·         Extensive structural identity

·         Potency

·         Purity

·         Impurities

Reference standard new batch before it is use for analysis of drug it must be qualified/calibrated against current reference standard.

For biological reference standard have two tiers

·         Qualifying new reference standard to prevent drift in the quality attribute.

·         Comparison of each new reference standard with primary reference standards it is link to clinical trial material and current manufacturing process.

 

    II.           II. Analytical methods validation.:

A.     1.  Non compendial analytical procedure

It is process for demonstrating that an analytical procedure is suitable for intended purpose.

Before initiating validation studies this analytical procedure must be understood which is based on the optimization studies and scientific-based method development.

 The validation data must be generated under sponsored approved protocol along with cGMP (Current Good Manufacturing practice) with methodology description, acceptance criteria using under qualified instrumentation.

Drug substance, product analyte and mixture of analyte protocol in respective matrices should be developed and executed.

 

B.     2. Validation Characteristic.:

              Specificity

Linearity

Accuracy

Precision (repeatability, intermediate precision and reproducibility)

Range

Quantitation Limit

Detection Limit

·         Sample spike use with target analyte and all known interference have undergone various laboratory stress. Condition & actual product sample is either aged or have stored under accelerated temperature and humidity conditions

·         Data used to establish that the analytical procedure used in testing meet accuracy proper standard and reliability.

·         Data used to establish that the analytical procedure used in testing meet proper standards of accuracy and reliability.

·         Notify the FDA about each condition in an approved application beyond the variation already provide for in the application including change to analytical procedure and established controls.

·         The result of submitted data must have robustness evaluation of method obtained during method development or a part of planned validation study.

C.    3. Compendial analytical procedure

Analytical procedure suitability should be verified under actual condition of use

USP/NF analytical procedure are suitable for the drug product or drug substance included in the submission and generated under a verification protocol.

Verification protocol should include

1.      Compendial methodology to verified with predetermined acceptance criteria

2.      Detail of methodology reagent suitability

·         Equipment component

·         Chromatographic condition

·         Column

·         Detector type

·         Sensitivity of detector signal response

·         System suitability

·         Sample preparation

·         Stability

Verification protocol must have characteristic test

Specificity

LOD

LOQ

Precision

Accuracy

Specification limits of Protocol is tighter than compendial acceptance criteria, RT, RRT are changing in chromatographic method because of synthetic route of drug substance or difference in manufacturing process or matrix of drug product.

If method have no deviation then compendial assay robustness studies is not required.

Reference.: Analytical Procedures and Methods Validation for Drugs and Biologics Guidance for Industry by U.S. Department of Health and Human Services Food and Drug Administration Center for Drug Evaluation and Research (CDER) Center for Biologics Evaluation and Research (CBER) July 2015 Pharmaceutical Quality/CMC.

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