Enantiomeric Separation of S-Epichlorohydrin and R-Epichlorohydrin by Capillary Gas Chromatography with FID Detector  

作　　者：Cholleti Vijay Kumar Pavan Kumar Vasa Y. Ravindra Kumar Pasula Aparna Padi Pratyusha Cholleti Vijay Kumar;Pavan Kumar Vasa;Y. Ravindra Kumar;Pasula Aparna;Padi Pratyusha(Dr. Reddy’s Laboratories Ltd. Active Pharmaceutical Ingredients, IPDO, Hyderabad, India;Department of Chemistry, J.N.T. University, Hyderabad, India;Department of Pediatrics, SUNY Stony Brook Medical Center, Stony Brook, New York, USA)

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

出　　处：《American Journal of Analytical Chemistry》2016年第11期772-784,共13页美国分析化学（英文）

摘　　要：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.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.

关 键 词：S-Epichlorohydrin R-Epichlorohydrin Method Development ICH Guidelines Method Validation Gas Chromatography 

分 类 号：O62[理学—有机化学]