Enantiomeric Separation of S-Epichlorohydrin and R-Epichlorohydrin by Capillary Gas Chromatography with FID Detector
| Autor: | Padi Pratyusha, Cholleti Vijay Kumar, Y. Ravindra Kumar, Pavan Kumar Vasa, Pasula Aparna |
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| Rok vydání: | 2016 |
| Předmět: |
Detection limit
Chromatography 010405 organic chemistry Chemistry 010401 analytical chemistry Analytical chemistry 01 natural sciences Diluent 0104 chemical sciences Volumetric flow rate law.invention Psychiatry and Mental health chemistry.chemical_compound Enantiopure drug law Flame ionization detector Epichlorohydrin Gas chromatography Derivatization |
| Zdroj: | American Journal of Analytical Chemistry. :772-784 |
| ISSN: | 2156-8278 2156-8251 |
| DOI: | 10.4236/ajac.2016.711069 |
| Popis: | 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. |
| Databáze: | OpenAIRE |
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