HPLC手性固定相法拆分丁苯酞及其衍生物对映体

目的建立丁基苯酞（3-n-butylphthalide，NBP）及其衍生物6-Br-NBP的手性HPLC拆分方法。方法以纤维素-三（3，5-二氯苯基氨基甲酸酯）为固定相的手性ChiralpakIC柱，系统研究NBP及其衍生物6-Br-NBP在HPLC系统中的拆分，分别考察流动相改性剂、柱温、流动相流速等对拆分效果的影响。结果当流动相为正己烷-无水乙醇（98：2）、流速为0．8mL·min^-1、柱温为35℃时，NBP的分离因子a和分离度瓜分别为1．07和2．20。当流动相为正己烷：异丙醇（70：30）、流速为0．8mL·min^-1、柱温为20℃时，6-Br-NBP的分离因子α和分离度尺。分别为1．10和2．67。结论该方法适用于NBP及其类似衍生物对映体的拆分。

Enantioseparation of 3-n-Butylphthalide and 6-Br-3-n-butylphthalide on Chiralpak IC Column by HPLC

OBJECTIVE To establish method for enantioseparation of 3-n-butylphthalide（NBP） and 6-Br-NBP on Chiralpak IC column by HPLC. METHODS HPLC had been developed for the chiral separation of NBP and 6-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. RESULTS NBP and 6-BroNBP could be separated completely. In the circumstance of hexane-ethanol（98 ：2）, flow rate 0.8 mL.min-1, temperature 35 ℃, to NBP, the separation factor α was 1.07 and the resolution Rs reached 2.20. As hexane-isopropanol（70 ： 30）, flow rate 0.8 mL·min^-1, injection volume 10 μL, temperature 20 ℃, to 6-Br-NBP, the separation factor α was 1.10 and the resolution Rs reached 2.67. CONCLUSION This method is suitable for the chiral separation of NBP and 6-Br-NBP.