Chemistry Reference
In-Depth Information
• Any deviations from the protocol, planned or observed, and the impact (if
any) on the validation.
• Any amendments to the protocol, with explanations and approvals.
• Conclusion.
A properly designed validation protocol can serve as a template for the validation
report. For example, in the protocol a test can be described and the acceptance crite-
ria listed. For the validation report, this information is supplemented with support-
ing results, a reference to the location and identity of the raw data, and a pass/fail
statement.
4.6 summAry
Method validation constantly evolves and is just one part of the overall regulated-
environment process. The validation process starts with instrument qualification
(Chapter 2) before an HPLC instrument is placed online, and continues long after
method development (Chapter 3), optimization, and transfer (Chapter 9), living on
with the method during routine use. A well-defined and documented validation pro-
cess provides regulatory agencies with evidence that the system and method are both
suitable for their intended use. It also ensures that guidelines have been framed to
help establish method validation requirements and specifications.
The bottom line is that all parties involved should be confident that an HPLC
method will give results that are sufficiently accurate, precise, and reproducible for
the analysis task at hand. Formal method validation is just a set of tools to use to
accomplish this task. Whether or not a formal validation is required, performance of
good, justifiable science as part of an established quality system will help to ensure
that the resultant method and the data that it generates will survive the scrutiny of
reviewers.
reFerences
1. Guideline for Submitting Samples and Analytical Data for Methods Validation, USFDA-
CDER (February 1987), http://www.fda.gov/cder/guidance/ameth.htm.
2. Chapter 1225, Validation of Compendial Methods,
United States Pharmacopeia No.
34-NF
297, (2011).
3. Analytical Procedures and Methods Validation, USFDA-CDER (August 2000),
http://www.fda.gov/cder/guidance/2396dft.htm.
4. Harmonized tripartite guideline, validation of analytical procedures, text and meth-
odology, Q2 (R1)
International Conference on Harmonization,
November 2005,
http://www.ich.org/LOB/media/MEDIA417.pdf.
5. Guidance for Methods Development and Methods Validation for the Resource
Conservation and Recovery Act (RCRA) Program, U.S. EPA (1995), http://www.epa.
gov/epawaste/hazard/testmethods/pdfs/methdev.pdf.
6. ISO/IEC 17025, General requirements for the competence of testing and calibration
laboratories, 2005, http://www.iso.org/iso/iso_catalogue/catalogue_tc/catalogue_detail.
htm?csnumber=39883.
7. Current Good Manufacturing Practice in Manufacturing, Processing, Packing, or
Holding of Drugs, 21 CFR Part 210, http://www.fda.gov/cder/dmpq/cgmpregs.htm.
