Validating chromatographic methods
The validation procedure in this particular article is based on requirements for EU multistate registration.
Wegscheider (13) has published procedures for method validation with a special focus on calibration, recovery experiments, method comparison and investigation of ruggedness. (14) have described how analytical methods are validated in a Japanese QC laboratory.
Green (11) gave a practical guide for analytical method validation, with a description of a set of minimum requirements for a method.
Renger and his colleagues (12) described the validation of a specific analytical procedure for the analysis of theophylline in a tablet using high-performance thin layer chromatography (HPTLC).
The preparation and execution should follow a validation protocol, preferably written in a step-by-step instruction format.
Possible steps for a complete method validation are listed in Table 1.
Operators should be sufficiently familiar with the technique and equipment.The analyst should be very well versed in the technique and operation of the instrument.Before an instrument is used to validate a method, its performance specifications should be verified using generic chemical standards.Representatives of the pharmaceutical and chemical industry have published papers on the validation of analytical methods.Hokanson (9,10) applied the life cycle approach, developed for computerized systems, to the validation and revalidation of methods.
For example, if the method is to be run on a specific instrument in a specific laboratory, there is no need to use instruments from other vendors or to include other laboratories in the validation experiments.