Author(s)

Cholleti Vijay Kumar^1,2*, Pavan Kumar Vasa³, Y. Ravindra Kumar¹, Pasula Aparna², Padi Pratyusha¹

¹Dr. Reddy’s Laboratories Ltd. Active Pharmaceutical Ingredients, IPDO, Hyderabad, India.
²Department of Chemistry, J.N.T. University, Hyderabad, India.
³Department of Pediatrics, SUNY Stony Brook Medical Center, Stony Brook, New York, USA.

The aim of this study was to develop a simple and derivatization free method for the Quantification of S-Epichlorohydrin in R-Epichlorohydrin by using a gas chromatography coupled with flame ionization detector (FID). Enantiopure epichlorohydrin was a valuable epoxide key starting material for preparing optically active Rivaroxaban. The enantiomeric separations of S-Epichlorohydrin and R-Epichlorohydrin were achieved on Gamaa-Dex-225 (30 meters × 0.25 mm I.D, 0.25 μm) column with a total run time of 30 min. Nitrogen was used as a carrier gas with constant pressure 25.0 psi. The critical experimental parameters such as, column selection, flow rate, injection volume and diluent were studied and optimized. Excellent correlation coeffient between peak responses and concentrations was >0.9998. The recoveries of S-Epichlorohydrin spiked in R-Epichlorohydrin were in the range from 98.2% to 102.8%. Limit of quantitation for S-Epichlorohydrin was sufficiently lower than limits specified by ICH. The method has validated as per International Conference on Harmonization (ICH) guidelines. A precise, accurate, linear and robust Gas Chromatography method was developed for the quantification of S-Epichlorohydrin in R-Epichlorohydrin for Rivaroxaban.

S-Epichlorohydrin, R-Epichlorohydrin, Method Development, ICH Guidelines, Method Validation, Gas Chromatography

Kumar, C. , Vasa, P. , Kumar, Y. , Aparna, P. and Pratyusha, P. (2016) Enantiomeric Separation of S-Epichlorohydrin and R-Epichlorohydrin by Capillary Gas Chromatography with FID Detector. American Journal of Analytical Chemistry, 7, 772-784. doi: 10.4236/ajac.2016.711069.