HPLC手性固定相法拆分丁苯酞及其衍生物对映体

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

关键词:  丁基苯酞  高效液相色谱法  Chiralpak IC

Key words:  3-n-butylphthalide  HPLC  Chiralpak IC

摘要:

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Chiralpak IC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0.8 mL·min^-1、柱温为35 ℃时，NBP的分离因子α和分离度R_s分别为1.07和2.20。当流动相为正己烷∶异丙醇(70∶30)、流速为0.8 mL·min^-1、柱温为20 ℃时，6-Br-NBP的分离因子α和分离度Rs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。

Abstract:

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-Br-NBP 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 R_s 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.