Chemistry Reference
In-Depth Information
approach, and to establish inspection and enforcement policies and procedures. For
example, the FDA guidance provides recommendations to applicants on submitting
analytical procedures, validation data, and samples to support the documentation
of the identity, strength, quality, purity, and potency of drug substances and drug
products, and is intended to assist applicants in assemblingß information, submitting
samples, and presenting data to support analytical methodologies [10,11]. The recom-
mendations apply to drug substances and drug products covered in NDAs, ANDAs,
biologics license applications (BLAs), product license applications (PLAs), and sup-
plements to these applications. The guidelines are generic; that is, they apply to any
analytical procedure, technique, or technology used in a regulated laboratory (e.g.,
gas chromatography, GC; mass spectrometry, MS; and infrared spectroscopy, IR).
Analytical chemists have practiced method validation for decades without even
knowing it. Always striving for repeatability, linearity, accuracy, etc., they called it
“good science.” In 1987, the FDA issued a guidance document that formally coined
the term “method validation” for the first time, and designated the specifications in
the current edition of the
United States Pharmacopeia
(USP) as those legally rec-
ognized when determining compliance with the Federal Food, Drug, and Cosmetic
Act [10-12]. Since the late 1980s, government and other agencies (e.g., FDA, ICH)
have issued new and updated guidelines on validating methods. More recently, new
information has been published, updating the previous guidelines and providing
more detail and harmonization with ICH guidelines. In August of 2000, the FDA
updated the original 1987 guidance document in draft form to reflect changes in
the agency's approach, the use of new technology, and to be consistent with the ICH
guidelines Q2A: Text on Validation of Analytical Procedures and Q2B: Validation
of Analytical Procedures: Methodology [11]. USP Chapter <1225> on Validation of
Analytical Procedures has also been updated to reflect these changes and the newer
Q2 (R1) “combined” guideline” [13]. Table 1.2 is a list of some of the USP and FDA
guidance pertaining to AMV. The 2000 FDA draft guidance, in combination with
USP Chapter <1225> and ICH Q2 (R1), forms the very foundation of AMV.
The 2000 FDA draft guidance emphasizes the ICH recommendations for non-
compendial analytical procedures and elaborates on topics such as types of analytical
tAble 1.2
general usp/FdA guidelines pertaining to Amv
guideline
subject/title (reference)
USP <1225>
Validation of Compendial Procedures
USP <1226>
Verification of Compendial Procedures
USP <621>
Chromatography
USP <1092>
The Dissolution Procedure: Development and Validation
USP <1058>
Analytical Instrument Qualification
USP <1010>
Analytical Data Interpretation and Treatment
FDA 1987
Guideline for Submitting Samples and Analytical Data for Methods Validation [10]
FDA 2000
Draft Guidance for Industry: Analytical Procedures and Methods Validation [11]
