Definition pubs.acs.org/doi/book/10.1021/acsreagents
Validation of Analytical Methods Part 1, Introduction and Definitions eISBN: 9780841230460 Tom Tyner Chair, ACS Committee on Analytical Reagents James Francis Secretary, ACS Committee on Analytical Reagents
Downloaded by CORNELL UNIV on May 11, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.1004
ABSTRACT A method validation process must demonstrate-with evidence to a high degree of assurance-that a specific method will consistently perform according to its intended specified purpose. It is the policy of the ACS Committee on Analytical Reagents to validate any new method described in an individual monograph that is published in or after the Tenth Edition. Analytical methods published in the Ninth Edition or earlier have been tested and proven by both intra- and interlaboratory verifications and will be accepted retrospectively as validated. Major modifications made to existing methods (from the Ninth Edition or earlier) that are incorporated into editions after the Tenth Edition or published in supplements to later editions will be validated according to the new policy.
METHOD VALIDATION The Committee defines the validation terminology in the following ways: • Method specificity is a measure of the method’s ability to accurately measure the analyte in the presence of similar analytes, impurities, or interfering substances. • Method linearity is a measure of the method’s ability to provide a linear response across the intended range of the method. • Method accuracy is the nearness of a measurement or result to its true value. • Method precision is a measure of the method’s ability to reproduce a measurement or result, and it can include elements of instrument precision, repeatability, and reproducibility. • Method verification (ruggedness) is the ability of a method result to be reproduced between analysts, instruments, days, and laboratories. Validation of a new analytical method is carried out in the following manner: Validations are initiated by a method sponsor, who is responsible for ensuring that validations are performed according to this policy and that all validations are properly documented. A validation protocol is drafted before initiating a validation. The protocol discusses the purpose, scope, procedure, and documentation of results. • The purpose describes the reason for the protocol. • The scope defines the boundaries of the protocol and may also define exclusions. If applicable, a reference is provided for the derivation of the method.
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.1004 ACS Reagent Chemicals, Part 1
ACS Reagent Chemicals
Definition
pubs.acs.org/doi/book/10.1021/acsreagents
• The procedure is a detailed guidance for performing the validation and includes components to illustrate a method’s specificity, linearity, accuracy, precision, and ruggedness. For methods where impurity testing is required, the limit of quantitation and limit of detection are also addressed in the protocol, where applicable. (Guidelines for determining detection limits are covered in the Method Detection Limits section, [Part 1: Method Detection Limits; Determining Detection Limits].) Each component has acceptance criteria that are defined in the protocol. • The documentation of results describes the documentation requirements for the protocol, including the requirements for recording raw data and for preparing a validation summary report. The draft of the validation protocol is submitted by the method sponsor to the Method Validation Subcommittee for approval. The method sponsor then coordinates execution of the validation protocol. The initial validation steps may be performed in the sponsor’s laboratory or in a sponsor-designated laboratory.
Downloaded by CORNELL UNIV on May 11, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.1004
After completion of the intralaboratory portion of the validation, the method sponsor identifies one or more laboratories to perform the interlaboratory verification. Upon completion of all laboratory tests, the method sponsor compiles the validation data, ensures that all data have met the acceptance criteria, and writes the summary report. This report summarizes the results of the validation and contains the following information: an introduction that states the method being validated, method sponsor, and interlaboratory participants; a summary of the test results; and observations of any changes or deviations that occurred during the protocol performance. The summary report and all supporting data are submitted to the Method Validation Subcommittee for final review and acceptance of the protocol, documentation, and summary report. After final review and approval by the Method Validation Subcommittee, all reports and documentation are turned over to the Committee Secretary for archiving. A copy of the summary report is made available to requestors.
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.1004 ACS Reagent Chemicals, Part 1
