ENANTIOMERIC SEPARATION OF ETODOLAC IN A BULK DRUG SUBSTANCE BY REVERSE-PHASE CHIRAL LIQUID CHROMATOGRAPHY METHOD
Keywords:Etodolac, Reverse phase, Chiral HPLC, Validation, Solution and mobile phase stability
Objective: To develop novel, simple and rapid enantiomeric separation of Etodolac by reverse-phase high-performance liquid chromatographic method as per ICH guidelines.
Methods: The R-isomer and S-isomer were baseline resolved on a CHIRAL-AGP, (100 x 4.0 mm i. d, 5 mm) column using a mobile phase system containing 0.1 M sodium dihydrogen phosphate dihydrate pH 4.0 buffer: Isopropanol (85:15 v/v.) at detector wavelength 225 nm and column temperature 25 Â°C. The chromatographic resolutions between R-isomer and S-isomer were found three. The developed method was extensively validated according to ICH guidelines.
Results: Good linearity was observed for R-isomer over the concentration range of 300â€“3000 ng/ml, with the linear regression (Correlation coefficient R = 0.999) and proved to be robust. The limit of detection and limit of quantification of R-isomer was found to be 300 and 900 ng/ml, respectively for 10 ml injection volume. The percentage recovery of R-isomer was ranged from 98.0 to 102.0 in bulk drug samples of Etodolac. Etodolac sample solution and mobile phase were found to be stable for at least 48 hours. The proposed method was found to be suitable and accurate for the quantitative determination of R-isomer in bulk drugs.
Conclusion: A novel, simple and rapid enantiomeric separation of Etodolac by reverse-phase high-performance liquid chromatographic method was developed and validated as per ICH guidelines. The developed method can be used for the quantitative determination R-isomer in bulk drug materials in pharmaceutical industry.
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