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Karthikeyan K, Saravanan R, Rajeswari R, et al. Validation of single isocratic HPLC method for the assay of valdecoxib and determination of metaisomer impurity. J Chromatogr Sci. 2009;47(4):309-14doi: 10.1093/chromsci/47.4.309.
Karthikeyan, K., Saravanan, R., Rajeswari, R., & Chandrasekara Pillai, K. (2009). Validation of single isocratic HPLC method for the assay of valdecoxib and determination of metaisomer impurity. Journal of chromatographic science, 47(4), 309-14. https://doi.org/10.1093/chromsci/47.4.309
Karthikeyan, K, et al. "Validation of single isocratic HPLC method for the assay of valdecoxib and determination of metaisomer impurity." Journal of chromatographic science vol. 47,4 (2009): 309-14. doi: https://doi.org/10.1093/chromsci/47.4.309
Karthikeyan K, Saravanan R, Rajeswari R, Chandrasekara Pillai K. Validation of single isocratic HPLC method for the assay of valdecoxib and determination of metaisomer impurity. J Chromatogr Sci. 2009 Apr;47(4):309-14. doi: 10.1093/chromsci/47.4.309. PMID: 19406018.
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J Chromatogr Sci. 2009 Apr;47(4):309-14. doi: 10.1093/chromsci/47.4.309.

Validation of single isocratic HPLC method for the assay of valdecoxib and determination of metaisomer impurity.

Journal of chromatographic science

K Karthikeyan, R Saravanan, R Rajeswari, K Chandrasekara Pillai

Affiliations

  1. Analytical Development, Shasun Research Center, Chennai, India. [email protected]

PMID: 19406018 DOI: 10.1093/chromsci/47.4.309

Abstract

A sensitive and accurate isocratic high-performance liquid chromagraphic method is developed for the determination of both metaisomer impurity and assay of valdecoxib drug substance. This method uses a Phenomenex Luna C18 (2) column, a mobile phase of 60:30:10 (v/v) 20 mM NaH2PO4, methanol, and tetrahydrofuran, respectively, with UV detection. This method is validated and its stability-indicating capability is established by performing stress studies under acidic, basic, oxidation, light, humidity, and thermal conditions. Valdecoxib is well separated from its metaisomer impurity with a resolution of more than 2.0. The limit of detection of 0.007% is obtained for the metaisomer impurity, and the relative response factor is also determined. Repeatability is good, with a relative standard deviation of not more than 0.2% and 0.8% for the assay and impurity methods, respectively. A system suitability test is developed with acceptance criteria and the requirements are met throughout the method validation. The method is validated as robust to variations in chromatographic conditions.

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