高效液相色谱法手性拆分丹参素对映体的研究  

Chiral separation of Danshensu enantiomers by HPLC

作　　者：谢菲[1] 周辛波[1] 郭继倩 郑志兵[1] 

机构地区：[1]军事医学科学院毒物药物研究所,北京100850

出　　处：《药物分析杂志》2014年第4期664-668,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的：以L-苯丙氨酸和硫酸铜为手性流动相添加剂建立丹参素与其对映体的手性拆分方法。方法：采用C8（4．6mm×250mm，5μm）色谱柱，对影响对映体拆分的主要因素：手性添加剂浓度、流动相pH、流动相中甲醇比例和柱温等进行了考察。选择流动相组成为甲醇-手性溶液（含8mmol·L^-1L-苯丙氨酸和3mmol·L^-1硫酸铜，氢氧化钠调pH至3．5）（18：82），柱温20℃。检测波长279nm，流速1．0mL·min^-1。结果：丹参素与其对映体得到基线分离，丹参素先于其对映体出峰。测定其对映体相对于丹参素的校正因子为0．948，平均加标回收率为98．6％～100．8％，RSD小于1％。结论：该方法简便，成本低，对工业生产中丹参素的光学纯度控制有实际意义。Objective：To develop a high performance liquid chromatographic （HPLC）method for the chiral separation of Danshensu enantiomers with L -phenylalanine and copper sulphate as the chiral mobile phase additives. Methods：The separation was performed on a C8 reversed -phase column （4.6mm×250mm,5μm） , and the influences of methanol content,concentrations of chiral mobile phase additives,pH of the buffer and the column tem- perature were investigated. The mobile phase consisted of methanol - chiral solution （ containing 8 mmol · L^- 1 L - phenylalanine and 3 mmol · L^-1 copper sulphate, adjusted to pH 3.5 by NaOH solution） （ 18：82 ） ;the flow rate was 1.0 mL · min^-1 ;the column temperature was controlled at 20 ℃ and the wavelength detector was set at 279 nm. Result： A baseline separation of Danshensu enantiomers was achieved, and Danshensu was eluted prior to L - isomer with a resolution value of 1.79. The correction factor between L - isomer and Danshensu was 0. 948, and the average recoveries were in the range of 98.6% - 100.8% with RSD less than 1.0%. Conclusion：The established method is simple and economic,with practical significance in checking and controlling the optical purity of Danshensu in in- dustrial production.

关 键 词：高效液相色谱 手性流动相添加剂 丹参素 手性拆分 对映异构体 

分 类 号：R917[医药卫生—药物分析学]