Study On The Enantiomeric Separation Of Several Chiral Drugs On An Immobilised Polysaccharide-based Chiral Stationary Phase

The quality control of chiral drugs catches people’s attention increasingly,so it becomes a focus in this field. High Performance Liquid Chromatography is one of the most popular analytic techniques and the method with chiral stationary phase is more classical,convenient and fast.The method with bonded chiral stationary phase has a steady performance and now it is used widely.NBP is approved as an anti-cerebral ischemic agent by the State Food and Drug Administration(SFDA) of China.6-Br-NBP, a derivative compound of NBP,has been proved to be more active than NBP. Four chiral compounds (GX-22、GX-25、GX-26and GX-30) are synthesized including a-methylene-y-butyrolactones and studies on the biological activities of four chiral compounds are proved to be satisfying.Three aspects have been carried out in this study:1.Enantioseparation of NBP and6-Br-NBP on Chiralpak IC columnHPLC methods have been developed for the chiral separation of NBP and6-Br-NBP on a Chiralpak IC column under normal phase mode. The influences of organic solvent, column temperature and flow rate were investigated and the enatiomeric separation was optimized systematically. The results showed that NBP and6-Br-NBP can be separated completely. For NBP, ethanol was better than isopropanol as a component of mobile phase. For6-Br-NBP, isopropanol was much better than rthanol.2.Enantioseparation of four chiral compounds (GX-22、GX-25、GX-26and GX-30) including a-methylene-y-butyrolactone on Chiralpak IC columnHPLC methods have been developed for the chiral separation of four chiral compounds including a-methylene-y-butyrolactone on a Chiralpak IC column under normal phase mode. The influences of organic solvent, column temperature and flow rate were investigated and the enatiomeric separation was optimized systematically. The results showed that GX-25and GX-26can be separated completely using isopropanol as the component of mobile phase. Both GX-22and GX-30were separated completely using ethanol and isopropanol as the components of mobile phase. 3.Determination of enantiomers of6-Br-NBP in SD rats plasma on Chiralpak IC column by HPLCThe biological samples were pretreated and separation conditions were optimized. Concentration of enantiomers of6-Br-NBP in SD rats plasma was measured under normal mode by HPLC with fluorescence detector. Method was evaluated from specificity, precision, accuracy, linearity, recovery,etc.