西布曲明对映体的毛细管电泳分离及结合常数的测定

Chiral separation and binding constants measurement of Sibutramine enantiomers by capillary electrophoresis

目的采用毛细管电泳法分离西布曲明对映体并测定其结合常数。方法考察手性添加剂浓度、缓冲溶液pH及浓度、温度、分离电压等因素对分离度的影响,并采用双倒数法计算西布曲明对映体与2,6-二甲基-β-环糊精(DM-β-CD)的结合常数。结果在12.5mmol·L-1DM-β-CD、100mmol·L-1Tris-H3PO4(pH2.5)缓冲液、16℃柱温,30kV操作电压的毛细管电泳条件下,西布曲明对映体在9min内获得了良好分离,分离度达2.0;结合常数分别为154.4、173.3L·mol-1。结论所用高效毛细管电泳方法快速、准确、可靠,适用于西布曲明对映体的分离;结合常数的计算可为研究西布曲明对映体的拆分机理提供依据。

OBJECTIVE A method for separation of sibutramine enantiomers by capillary electrophoresis was set up. And the binding constants was measured. METHODS The effect of the concentration of chiral selector, pH and concentration of buffer, capillary temperature and separation voltage were investigated respectively. The binding constants of sibutramine enantiomers and DM-β-CD were calculated by the double - reciprocal method. RESULTS The optimized HPCE conditions of sibutramine enantiomers were 12.5 mmol·L^-1 of DM -J3 -CD, 100 mmol·L^-1 of buffer （pH2.5）with capillary temperature of 16 ℃ and separation voltage of 30 kV. Sibutramine enautiomers were completely separated within 9.0 min. The resolution was 2.0. The binding constants were 154.4 L·mol^-1 and 173.3 L·mol^-1. CONCLUSION The established HPCE method is rapid and accurate and reliable,which is suitable for separation of sibutramine enantiomers. The binding constants calculated provide the basis for researching the separation mechanism of sibutramine enantiomers.