Validation, of analytical methods

To provide validation of analytical methods to ensure accuracy and reliability 

It is the responsibility of the quality control analyst and quality control manager to follow the procedure. The quality assurance manager is responsible for SOP compliance. 

For detailed description, refer USP 24 (1225) Validation of Compendial Methods. 

The precision of an analytical method can be defined as the pattern of variation of single assays on a uniform sample. The precision serves to identify random errors and is described by the repeatability (variability within a laboratory) and reproducibility (variation between different laboratories). 

In providing evidence of selectivity, it must be shown that an analytical method exclusively determines the desired compound. 

Method validation is the process of documenting or proving that an analytical method provides analytical data acceptable for the intended use. 

The basic concept of the validation process encompasses two aspects  

As mentioned in Chapter 1, the analytical process benefits when the analyst can be involved in defining the problem, that is, in making sure the proper questions are posed. When data requirements are poorly conceived or unrealistic, analytical measurements can be unnecessarily expensive if the method selected is more accurate than needed. Or, it may be inadequate if the method is less accurate than required, or of questionable value if the accuracy of the method is unknown. The first step in method development and validation is setting minimum requirements, which essentially are the specifications of the method for the intended purpose. How accurate and precise does it have to be W at is the target concentration  

We described in Chapter 1 the general procedure for establishing how an analysis will proceed. The hierarchy of methodology (Table 4.1) may be considered as follows  

Technique Scientific principle useful for providing compositional information Spectrophotometry 

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Some internationally harmonized guidelines regarding specifications and tests, impurities and validation of analytical methods have particular relevance to the development of chiral drugs and are discussed below. In addition, the impact of work on the common technical document is considered. 

ICH Guideline (1994) Validation of analytical methods (Definition and Terminology). IFPMA, Geneva. 

The purpose of this article is to clarify the assessment of residue analytical methods in the context of Directive 91/414/EEC. After discussing the legal and historical background, requirements for enforcement methods as well as data generation methods are reviewed. Finally, an outlook over further developments in the assessment and validation of analytical methods is provided. 

J.D. MacNeU, J. Patterson, and V. Martz, Validation of analytical methods - proving your method is fit for purpose, in Principles and Practices of Method Vahdation, ed. A. Flajgelj and A. Ambrus, MPG Books, Bodmin, pp. 100-107 (2000). 

Validation of analytical methods for post-registration control and monitoring purposes in the European Union... 

AOAC/FAO/IAEA/IUPAC Expert Consultation, Guidelines for Single Laboratory Validation of Analytical Methods for Trace-level Concentrations of Organic Chemicals, Workshop, 8-11 November 1999, Miskolc, Hungary (1999). Also available on the Word Wide Web http //www.iaea.oi trc/(see pesticides —> method validation). 

In analytical practice, they are best recognized by the determination of xtest as a function of the true value xtrue, and thus, by analysis of certified reference materials (CRMs). If such standards are not available the use of an independent analytical method or a balancing study may provide information on systematic errors (Doerffel et al. [1994] Kaiser [1971]). In simple cases, it may be possible, to estimate the parameters a, / , and y, in Eq. (4.5) by eliminating the unknown true value through appropriate variation of the weight of the test portions or standard additions to the test sample. But in the framework of quality assurance, the use of reference materials is indispensable for validation of analytical methods. 

Wegscheider W (1996) Validation of analytical methods. In H. Gunzler (ed) Accreditation and quality assurance in analytical chemistry. Springer, Berlin Heidelberg New York... 

ICH (1994) ICH Topic Q2A (ICH Harmonised Tripartite Guideline) Validation of analytical methods Definitions and terminology (CPMP/ICH/381/95), ICH, London... 

L. Huber, Validation of Analytical Methods Review and Strategy, http //www.labcompliance.com (6/8/2004). 

W. Wegscheider, Validation of analytical method, in Accreditation and Quality Assurance in Analytical Chemistry (ed. H. Guenzler), Springer, Berlin, 1996, pp. 135-157. 

Approaches to Process Validation Process Validation Program Periodic Review of Validated Systems Cleaning Validation Validation of Analytical methods Change Control, Rejection, and Reuse of Materials Rejection Reprocessing Reworking... 

Kirsch, R. B., Validation of Analytical Methods Used In Pharmaceutical Cleaning Assessment and Validation Analytical Validation in the Pharmaceutical Industry, Supplement to Pharmaceutical Technology pp. 40 6, 1998. 

Hokanson, G. C., A Life Cycle Approach to the Validation of Analytical Methods During Pharmaceutical Product Development, Part II Changes and the Need for Additional Validation, Pfjarm. Tech., 18(16) 92-100, 1994. 

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