Abstract

DEVELOPMENT AND VALIDATION OF A SUPERCRITICAL FLUID LIQUID CHROMATOGRAPHIC METHOD FOR DETERMINATION OF ENANTIOMERIC PURITY OF ATORVASTATIN IN BULK DRUGS AND PHARMACEUTICALS

Dr. K. Bhavyasri* and Dammu Rambabu

Abstract

A simple, rapid and robust SFC method for enantiospecific separation and determination of Atorvastatin in drugs and pharmaceuticals was developed using UV and polarimetric detectors connected in series. Baseline separation with resolution > 3.0 was achieved within 10 min on Chiralpak AD-H (250 mm x 4.6 mm) 5 micron column using a mobile phase containing of Supercritical carbon dioxide and methanol (90:10) at a flow rate of 2.5ml/min, at 25oC. Effects of methanol and temperature on enantioselectivity and resolution of the enantiomers were evaluated. For quantitative determinations using UV detector at 240nm. Polarimetric detector was used for identification of enantiomers. The limits of detection (LOD) and quantification (LOQ) were 0.5 and 1.3 μg/ml respectively for both the enantiomers. The linearity of the method was in the range of 50-600 μg/ml with r2 > 0.9999. The inter- and intra-day assay precision was less than 0.63% (%R.S.D.) and recoveries were in the range 99.38-100.41%. The method was validated and found to be suitable for determination enantiomeric purity of citalopram in bulk drugs and pharmaceutical formulations.

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