HPLC手性固定相法拆分丁苯酞及其衍生物对映体.PDFVIP

HPLC 手性固定相法拆分丁苯酞及其衍生物对映体  1 2 3* 郭红云 ，张超锋 ，李敏 (1.新乡医学院第三附属医院药剂科，河南 新乡 453003 ；2.郑州大学药学院，郑州 450001 ；3.郑州大学第二 附属医院药剂科，郑州 450001) 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Rs 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。 关键词：丁基苯酞；高效液相色谱法；Chiralpak IC 中图分类号：R917.101 文献标志码：B 文章编号：1007-7693(2014)03-0335-04 Enantioseparation of 3-n-Butylphthalide and 6-Br-3-n-butylphthalide on Chiralpak IC Column by HPLC 1 2 3* GUO Hongyun , ZHANG Chaofeng , LI Min (1.Department of Pharmacy, the Third Hospital of Xinxiang Medical University, Xinxiang 453003, China; 2.Zhengzhou University School of Pharmaceutical Sciences, Zhengzhou 450001, China; 3.The Second Affiliated Hospital of Zhengzhou University School, Zhengzhou 450001, China) 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 Rs reached 2.20. As hexane-isopropanol(70 ∶30), flo