Development and validation of a chiral LC-MS method for the enantiomeric resolution of (+) and (-)-Mebeverine Hydrochloride in bulk drug by using polysaccharide-based chiral stationary phase

Abstract

The aim of this study was to develop a simple, specific, sensitive and precise LC-MS method for the determination of mebeverine enantiomers in pharmaceutical formulations and it was validated as per ICH guidelines. The chromatographic separation was achieved on Phenomenex® Lux Cellulose 1 (250 mm x 4.6 mm i.d, 5μm particle size) column using mobile phase system containing acetonitrile: 10 mM ammonium acetate (85:15) at the flow rate of 0.8 mL/min. In the spectral investigation by LC-MS, the standard solution of Mebeverine showed major peak at m/z of 430.70, which was assigned to the [M+H] ion of Mebeverine. The described method was linear over the range of 15–75 ng /mL for (±) Mebeverine enantiomers with a correlation coefficient (r2 = 0.999). Detection limits and quantification limits of (+) Mebeverine and (-) Mebeverine were found to be 5 ng/mL and 15 ng/mL respectively. The recovery study of mebeverine from tablet formulation was found to be 99.16%. Mebeverine standard solution and mobile phase were found to be stable for at least 48h. The Mebeverine enantiomers were well resolved with mean retention times of about 1.16 min and 1.20 min respectively. The developed method was extensively validated and proved to be robust, accurate, precise, and suitable for analysis of Mebeverine enantiomers in tablet dosage form.