Laboratory Method Validation
For any method that will be used for routine analysis, a Method Validation and Quality Control
plan should be developed. This plan should ensure that the method, together with the equipment,
delivers consistently accurate results.
Procedure
1. Develop a validation master plan or an operating procedure for method validation.
2. For individual method validation projects, develop a validation project plan
3. Define intended use of the method and performance criteria.
4. Check all equipment and material for performance and quality.
5. Perform validation experiments.
6. Develop an operating procedure for method transfer between laboratories if necessary
The validation plan should include recommendations for the following:
1. Selection, handling and testing of QC standards
2. Type and frequency of equipment checks and calibrations (for example, should the
wavelength accuracy and the baseline noise of an HPLC UV detector be checked after each
sample analysis, or on a daily or weekly basis?)
3. Type and frequency of system testing (for example, at which point during the sequence
should standards be analyzed?)
4. Type and frequency of QC samples (for example, should a QC sample be analyzed after 1,
5, 20 or 50 unknown samples, and should there be single or duplicate QC sample analysis,
or should this be run at one or several concentrations?)
5. Analyses criteria such as sample storage, type, number of replicates.
6. Acceptance criteria for equipment checks, system suitability tests and QC sample analysis
7. Action plan in case criteria 2, 3 and/or 4 are not met.
Parameters for Method Validation:
Parameters for method validation as defined by the International Conference on Harmonisation
(ICH) and by others are summarised as:
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2.
3.
4.
5.
6.
7.
8.
Specificity
Selectivity
Precision
Reproducibility
Accuracy
Linearity
Detection limit
Range
Parameters should be assessed during the method development stage using published
guidelines for the type of method being used.
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Doc. Ref. 090 TASC Laboratory Validation Method V2.0
Issue Date: 12/03/2013
Transferring Validated Routine Methods
In instances where methods are developed and validated in another lab, it is necessary to
demonstrate that the method transfers successfully to the user lab before implementation.
References
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ISO/IEC 17025, General requirements for the competence of testing and calibration
laboratories, 2005
International Conference on Harmonization (ICH) of Technical Requirements for the
Registration of Pharmaceuticals for Human Use, Validation of analytical procedures:
definitions and terminology, Geneva (1996)
International Conference on Harmonization (ICH) of Technical Requirements for the
Registration of Pharmaceuticals for Human Use, Validation of analytical procedures:
Methodology, adopted in 1996, Geneva
J. M. Green, A practical guide to analytical method validation, Anal. Chem. News &
Features, 1 May 1996, pp. 305A–309A.
Wegscheider, Validation of analytical methods, in: Accreditation and quality assurance in
analytical chemistry, edited by H. Guenzler, Springer Verlag, Berlin (1996).
P. A. Winslow and R. F. Meyer, Defining a master plan for the validation of analytical
methods, J. Validation Technology, pp. 361–367 (1997).
J.Breaux, K. Jones, and P. Boulas, Pharmaceutical Technology, Analytical Technology
and Testing, 6-13, 2003
EURACHEM – The Fitness for Purpose of Analytical Methods A Laboratory Guide to
Method Validation and Related Topics, 1998
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Doc. Ref. 090 TASC Laboratory Validation Method V2.0
Issue Date: 12/03/2013