Validation, Chromatographic Methods

Stanaszek, R., Zuba, D. A comparison of developed and validated chromatographic methods (FIPLC, GC MS) for determination of delta-9-tetrahydrocannabinol (5 -TFIC) and delta-9-tetrahydrocannabinolic acid (5 -TFICA-A) in hemp. Probl. Forensic Sci. 71, 313-322 (2007)... 

Confirmatory methods should preferably be based on MS, providing direct information on the molecular structure of the analyte(s), especially for residues of prohibited substances or substances for which no MRLs are set. However, validated chromatographic methods with specific detectors (e.g., photodiode array, fluorescence) or using two or more different chromatographic separation systems may be used, particularly for contaminants for which MRLs are specified. 

Bliesner DM, editor. Validating chromatographic methods a practical guide. New York Wiley 2006. 

Developed standai d validation procedure is demonstrated for validation of a spectrophotometric assay of ambroxol hydrochloride tablets. Without any considerable revisions, this approach may be applied to chromatographic methods. Recommendations for validation criteria were included in the State Phai macopoeia of Ukraine. 

Center for Drug Evaluation Research, Reviewer Guidance Validation of Chromatographic Methods, November 1994. 

Validation results obtained from factor analysis of Table 31.2, containing the retention times of 23 chalcones in 8 chromatographic methods, after log double-centering and global normalization. The results are used in the Malinowski s f-test and in cross-validation by PRESS. 

For the validation of chromatographic methods a good starting point can be found in the EURACHEM/ WELAC document on Accreditation of Chemical Laboratories [30]. ASTM Committee E19 on Chromatography covers all forms of chromatography including gas, liquid, ion and supercritical chromatography. 

Tab. 2.4. Liquid-liquid chromatographic methods for measurement of log D at pH 7.4. Results for a series of validation compounds.

Several of the chapters in the current volume are comprehensive in nature, but others are more specialized. Volume 32 also contains a methodology review article on the validation of chromatographic methods of analysis. New to the series are annual reviews, and volume 32 contains a summary of the publications appearing during 2004 that dealt with polymorphism and solvatomorphism. It is anticipated that future volumes in the Profiles series will contain similar methodology reviews, as well as other types of review articles that summarize the current state in a particular field of pharmaceutics. As always, I welcome communications from anyone in the pharmaceutical community who might want to provide an opinion or a contribution. 

Gagliardi et al. [72] developed a simple high performance liquid chromatographic method for the determination of miconazole and other antimycotics in cosmetic antidandruff formulations. This high performance liquid chromatographic method was carried out on a Discovery RP Amide Ci6 column and spectrophotometric detection was performed at 220 nm. The initial mobile phase was a mixture of acetonitrile and aqueous 0.001 M sodium perchlorate (pH 3) in the ratio of 15 85 (v/ v) then a linear gradient less than 46% acetonitrile in 70 min, and less than 50% in 80 min. The extraction procedure was validated by analyzing samples of shampoo... 

M. Wells and M. Dantus, Validation of chromatographic method, in Ewing s Analytical Instrumentation HandBook (ed. J. Cazes), 3rd edn., Marcel-Dekker, 2005, pp. 1015-1033. 

Reviewer Guidance, Validation Method of Chromatographic Method, Center for Drug Evaluation and Research, CEDER, 1994. 

Hartmann, C., Smeyers-Verbeke, J., Massart, D. L., McDowell, R. D. Validation of bioanalytical chromatographic methods. J. Pharm. Biomed. Anal., 17, 1998, 193-218. 

In addition to online resources, other texts and references have discussed the process of validation for methods used in the pharmaceutical industry in relation to the regulatory guidance documents. These guides include discussions on method development in relation to method validation, the validation of non-chromatographic methods and stability indicating methods. 

Other chromatographic systems snch as DryLab 2000 Pins from LC Resonrces (http //www.lcresources.com) incorporate aspects of method development and validation throngh simnlation software combined with actnal experiments to determine optimal operating conditions. This system is designed to generate efficient method development and method optimization experiments. Resnlts from these experiments can be nsed for the evaluation of robusmess as part of the validation for methods developed using this type of software. 

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