High-performance liquid validation

These authors noted the potential for the assay to underestimate the concentration of TSR due to decreased binding of metabolites relative to parent spinosad. However, the major residue found was parent spinosad, so underestimation of residues is not likely to be problematic. Overall, this method was validated in 34 matrices and showed excellent agreement with results obtained with a high-performance liquid chromatography/ultraviolet detection (HPLC/UV) method. ... 

Full acceptance of HPLC/MS methods by the US EPA OPP as enforcement methods occurred between 1998 and 2001. For example, in 1998, the EPA OPP accepted HPLC/MS (without MS/MS) methods as primary enforcement methods, and high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) only was suitable for confirmatory methods. However, in 2001, HPLC/MS/MS methods also became acceptable for primary enforcement. Table 4 summarizes the types of methods that were validated by the EPA OPP method validation program, for both food tolerance enforcement methods and environmental chemistry methods. 

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... 

High performance liquid chromatography-mass spectrometric methods Nitin et al. [75] developed and validated a sensitive and selective liquid chromatography-tandem mass spectrometric method (LC MS MS) for the simultaneous estimation of bulaquine and its metabolites primaquine in monkey plasma. The mobile phase consisted of acetonitrile ammonium acetate buffer (20 mM, pH 6) (50 50, v/v) at a flow rate of 1 mL/min. The chromatographic separations were achieved on two Spheri cyano columns (5 pm, 30 cm x 4.6 mm), connected in... 

Chu, I. et al. 2000. Validation of higher throughput high-performance liquid chromatography/atmo-spheric pressure chemical ionization tandem mass spectrometry assays to conduct cytochrome P450s... 

King, R.C. et al. 2002. Description and validation of a staggered parallel high performance liquid chromatography system for good laboratory practice level quantitative analysis by liquid chromatography/tandem mass spectrometry. Rapid Commun. Mass Spectrom. 16 43. 

Sripalakit, P., Nermhom, P., and Saraphanchotiwitthaya, A. 2006. Validation and pharmacokinetic application of a method for determination of doxazosin in human plasma by high performance liquid chromatography. Biomed Chromatogr. 20 729. 

In the last twenty years, many of the developed and validated high performance liquid chromatography methods with conventional diode array or fluorescence detectors (DAD, FLD) were improved and substituted by new hyphenation with mass spectrometric instrumentation and/or NMR, especially for the analyses of raw materials derived from Natural sources. The main goal of this coupling is achieved by improvement of selectivity and sensitivity of new instrumental configurations [7], Furthermore, with these configurations it is possible to obtain, in only one analysis, the complete chemical structure elucidation, identification and quantification of targeted compounds. 

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. 

This chapter focuses on approaches to the validation of high-performance liquid chromatography methods based on regulatory guidance documents and accepted industry practices. The information in this chapter gives a brief review of the reasons for performing method validation and the regulations that describe this activity. Individual validation parameters are discussed in relation to the type of method to be validated. Examples of typical validation conditions are presented with references to additional information on individual topics. This chapter was written to help analysts responsible for method validation. 

Wynia, G. S., Windhorst, G., Post, P. C., and Maris, F. A. (1997). Development and validation of a capillary electrophoresis method within a pharmaceutical quality control environment and comparison with high-performance liquid chromatography. /. Chromatogr. A 773(1—2), 339—350. 

KieBling, P., Scrlba, G. K. E., SiiB, E, Werner, G., Knoth, H., and Hartmann, M. (2004). Development and validation of a high-performance liquid chromatography assay and a capillary electrophoresis assay for the analysis of adenosine and the degradation product adenine in infusions.. Pharm. Biomed. Anal. 36(3), 535—539. 

Kunkel, A., Gunter, S., Dette, C., and Watzig, H. (1997). Quantitation of insulin by capillary electrophoresis and high-performance liquid chromatography — method comparison and validation. J. Chromatogr. A 781, 445—455. 

Penalvo, G. C., Julien, E., and Eabre, H. (1996). Cross validation of capillary electrophoresis and high-performance liquid chromatography for cefotaxime and related impurities. Chromatographia 42, 159-164. 

T.R.M. De Beer, W.R.G. Baeyens, A. Venneire, D. Broes, J.R Remon, and C. Vervaet, Raman spectroscopic method for the determination of medroxyprogesterone acetate in a pharmaceutical suspension Validation of quantifying abilities, uncertainty assessment and comparison with the high performance liquid chromatography reference method. Anal. Chim. Acta, 589, 192-199 (2007). 

Shabir, G. A. Validation of high-performance liquid chromatography methods for pharmaceutical analysis. Understanding the differences and similarities between validation requirements of the U S Food and Drug Administration, the US Pharmacopeia and the International Conference on Harmonization. 

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. 

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). 

Table 2 Proposed Sequence of Validation Experiments, Example High Performance Liquid Chromatography... 

Priestner AA. Use of radiolabeled drug substance to investigate mass balance during validation of a high-performance liquid chromatography method for impurities. Anal Proc 1993 30 374-377. 

Hansen, A.M., Olsen, I.L.B., Holst, E. and Poulsen, O.M. (1991) Validation of a high-performance liquid chromatography/ fluorescenes detection method for the simultaneous quantification of fifteen polycyclic aromatic hydrocarbons. Annals of Occupational Hygiene, 35, 603-11. 

W.W. Bullen, R.A. Miller, R.N. Hayes, Development and validation of a high-performance liquid chromatography tandem mass spectrometry assay for atorvastatin, ortho-hydroxy atorvastatin, and para-hydroxy atorvastatin in human, dog, and rat plasma, J. Am. Soc. Mass Spectrom. 10 (1999) 55-66. 

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