区段灌注技术-场放大进样-毛细管电泳手性拆分山莨菪碱  

Chiral Separation & Quantification of Anisodamine by CE Coupling with Partial Filling Technique & Field-amplified Sample Injection

作　　者：周娇[1] 袁庆[1] 张雪琴[1] 周基英[1] 黄家燕[1] 崔书亚[1] 

机构地区：[1]绵阳师范学院化学与化学工程学院,四川绵阳621000

出　　处：《绵阳师范学院学报》2012年第11期49-53,共5页Journal of Mianyang Teachers＇ College

基　　金：绵阳师范学院自然科学研究基金资助项目(2011A15)

摘　　要：首次采用结合区段灌注技术及场放大进样的毛细管电泳技术对山莨菪碱四种异构体进行了拆分。详细探讨了溶液pH值、拆分试剂含量、分离缓冲充入时间、分离电压等对测定的影响,优化了实验条件。在75mmol L-1Tris-H3PO4(pH 3.5)为分离缓冲溶液,1.7%羧甲基-β-环糊精(CM-β-CD,1.0psi,90 s)为拆分试剂,分离电压17.5 kV条件下,23分钟内完成山莨菪碱四种异构体分离。并通过场放大进样进一步提高了测定的灵敏度。该方法成功应用于测定颠茄制剂中山莨菪碱,结果满意。A new, simple and sensitive method for simultaneous separation of two pairs of anisodamine enantiomers has been firstly developed and validated using CZE in combination with partial filling technique and field - amplified sample injection. Carboxymethylated - β - cyclodextrins （ CM - β - CD） was used as chiral selector in this system. Effects of pH, CM - β - CD content, filling time of separation buffer, and separation voltage on the enantiomer separation behavior were evaluated. In an optimal condition, the four enantiomers were resolved in 23 rain by partially filling an electrophoretie capillary with 1.7% C1V[ - β - CD （ 1.0psi, 90 s） and carrying out an electrophoresis with 75 mmol · L-1 Tris- H3PO4（ pH 3.5 ） at 17.5 kV. The sensitivity was further improved by field- amplified sample injection （0.2psi, 1.5s water plug）. Real sample was also tested and promising results for the determination of anisodamine enantiomers were obtained.

关 键 词：山莨菪碱 手性拆分 区段灌注技术 场放大进样 毛细管电泳 

分 类 号：R971[医药卫生—药品]