Validation of liquid chromatographic

J. Fogel, J. Sisco, and F. Hess, Validation of liquid chromatographic method for assay of chlorthalidone in tablet formulations, J. Assoc. Off. Anal. Chem., 68 96 (1985). 

Clark, M.J.R. Whitfield, P.H. Conflicting perspectives about detection hmits and about the censoring of environmental data. Water Resour. BuU. 1994, 30, 1063 1079. Jenke, D.R. Poss, M. Story, J. Odufu, A. Zietlow, D. Tsilpetros, T. Development and validation of liquid chromatographic methods for the identification and quantification of organic compounds leached from a laminated polyolefin material. J. Chromatogr. Sci. in press. Jenke, D.R. Chromatographic method vahdation A review of current practices and procedures Part II. Guidelines for primary validation parameters. Instrum. Sci. Technol. 1998, 26, 1-18. 

The focus of this chapter is validation of liquid chromatographic methods. Numerous articles describe details and provide examples for LC method validation [6,7] therefore, a step-by-step guide to method validation is not provided here. This chapter provides an overview of LC method validation as well as a discussion about some of the pitfalls associated with traditional validation and some alternative practices that are currently being discussed in the literature. 

Rao Nageswara, R., Nagaraju, D., Parimala, P. and Adapa, R. S. Development and validation of liquid chromatographic method for monitoring reaction involved in the synthesis of 4-methoxyphenylacetic acid. J. Chromatogr. A 972 277-282, 2002. 

Schubert et al. [72] developed and validated a liquid chromatographic method for the determination of omeprazole in powder for injection and in pellets. The analyses were performed at room temperature on a reversed-phase Ci8 column of 250 mm x 4.6 mm (5 /im). The mobile phase, composed of methanol-water (90 10) was pumped at a constant flow-rate of 1.5 ml/min. Detection was performed on a UV detector at 301 nm. The method was validated in terms of linearity, precision, accuracy, and ruggedness. 

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. 

Whereas SEC is the dominant technique for the characterisation of polymers, various nonexclusion liquid chromatographic (NELC) methods, such as GPEC and LACCC offer equally valid possibilities for deformulation of complex polymer systems. In fact, molecular characterisation of polymers in the precip-itation/adsorption mode (gradient HPLC) enables differences in chemical structure and composition to be... 

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

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... 

Larsimont V, Meins J, Buschges HF, Blume H. 1998. Validated high-performance liquid chromatographic assay for the determination of promazine in human plasma. J Chromatogr B Biomed Sci Appl 719(1-2) 222-226. 

Gupta, M. and Bhargava, H. N., Development and validation of a high-performance liquid chromatographic method for the analysis of bndesonide. Journal of Pharmaceutical and Biomedical Analysis 40(2), 423-428, 2006. 

W. Furman, T. Layloff, and R. Tetzlaff, Validation of computerized liquid chromatographic system, J. AOAC, 77, 1314, 1994. 

PQ should be performed on a daily basis or whenever the instrument is used. The test frequency not only depends on the stability of the equipment but on everything in the system that may contribute to the results. For a liquid chromatograph, this may be the chromatographic column or a detector s lamp. The test criteria and frequency should be determined during the development and validation of the analytical method. 

Furman et al. discussing the validation of computerised liquid chromatographic systems, present the concept of modular and holistic qualification. Modular qualification involves the individual components of a system such as pump, autosampler, column heater and detector of an HPLC. The authors make the point that ... 

A de Kok, M Hiemstra. Optimization, automation, and validation of the solid-phase extraction cleanup and on-line liquid chromatographic determination of V-methylcarbamate pesticides in fruits and vegetables. J Assoc Off Anal Chem 75 1063-1072, 1992. 

Reversed-phase high performance liquid chromatography has come into use for estimating the purity of proteins and peptides as well. However, before employed, a high performance liquid chromatographic (hplc) profile of a given protein must be completely validated (43). 

There are no official guidelines on the sequence of validation experiments, and the optimal sequence can depend on the method itself. For a liquid chromatographic method the sequence from Table 2 has been proven to be useful. 

J.L. Marty, N. Mionetto, S. Lacorte and D. Barcelo, Validation of an enzymic biosensor with various liquid-chromatographic techniques for... 

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