Abstract
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.
Highlights
An understanding of the nature of the racemic Epichlorohydrin is the foremost prerequisite for successful method development in GC
Column Selection The primary goal of column selection was to separate S-Epichlorohydrin and R-Epichlorohydrin from each other, which were used during the synthesis of Rivaroxaban
The results show that the peak widths of S-Epichlorohydrin and REpichlorohydrin were independent of injection volume within the tested range
Summary
Separation of the enantiomers of chiral drugs has become an important issue in analyt-. Epichlorohydrin is an organochlorine compound and it is a chiral molecule and exists as R-Epichlorohydrin and S-Epichlorohydrin mentioned in Figure 1(a) and Figure 1(b). Epichlorohydrin is a versatile precursor in the synthesis of many organic compounds. Epichlorohydrin is a colorless, volatile and highly reactive liquid. It is soluble in most organic solvents and slightly soluble in petroleum hydrocarbons and in water [3]. Epichlorohydrin has been classified as a probable carcinogen (group A) to human by the International Agency for Research on Cancer (IARC) [5]
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