Determination of Ketoconazole in Capsules by High-Performance Liquid Chromatography and Microbiological Assay

The development and validation of an HPLC-UV method and a microbiological assay were performed for the analysis of ketoconazole in capsule formulations. The bioassay was developed using a specific agar diffusion technique with the strain of Candida albicans ATCC 18804 as the test organism. The effec...

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Bibliographic Details
Published in:Journal of AOAC International 2009-07, Vol.92 (4), p.1076-1081
Main Authors: LIMA, Paulo Marcelo Andrade, DUQUE PRADO, Nathalia, SILVA, Maria-Luiza Martins, LOPES DINIZ, Rosiane Dias, MARQUES QUEIROZ, Kelly, DA COSTA CESAR, Isabela, PIANETTI, Gérson Antônio, ASSIS SANTOS, Daniel
Format: Article
Language:English
Subjects:
Antifungal Agents - analysis
Antifungal Agents - pharmacology
Biological and medical sciences
Biological Assay
Candida albicans - drug effects
Capsules
Chromatography, High Pressure Liquid
Food industries
Fundamental and applied biological sciences. Psychology
Hydrogen-Ion Concentration
Indicators and Reagents
Ketoconazole - analysis
Ketoconazole - pharmacology
Microbial Sensitivity Tests
Reference Standards
Reproducibility of Results
Spectrophotometry, Ultraviolet
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Summary:The development and validation of an HPLC-UV method and a microbiological assay were performed for the analysis of ketoconazole in capsule formulations. The bioassay was developed using a specific agar diffusion technique with the strain of Candida albicans ATCC 18804 as the test organism. The effect of the mobile phase pH in the range of 2.5-7.5 on the retention and tailing factors of the ketoconazole peak was analyzed in the chromatography method and a pH value of 4.5 was considered to be adequate. A prospective validation of both methods showed adequate linearity (r2 > 0.99 for the two methods), precision, (RSD = 2.42% for intraday and 2.69% for interday precision for bioassay; RSD = 0.74% for intraday and 0.66% for interday precision for HPLC-UV), and accuracy (mean recoveries were 103 +/- 1.0% for bioassay and 99 +/- 1.0% for HPLC-UV). Student's t-test revealed no significant difference between the results obtained by the two methods (P < 0.05). The contents found for three capsule samples showed a strong correlation, as attested by Pearson's coefficient value (r = 0.9998), which also evidenced the concordance between the studied methodologies.
ISSN:1060-3271
1944-7922
DOI:10.1093/jaoac/92.4.1076