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高效液相色谱用Pirkle型手性柱直接拆分阿折地平

叶晓霞, 许旭*   

  1. 1. 上海市食品药品检验所, 上海 201203
    2. 上海应用技术学院 化学与环境工程学院, 上海 201418
    3. 中国科学院 上海有机化学研究所, 上海 200032
  • 收稿日期:2012-05-21 修回日期:2012-07-28 出版日期:2012-09-15 发布日期:2012-09-15
  • 通讯作者: 许旭*

Direct chiral separation of azelnidipine by HPLC with Pirkle-type column

Xiaoxia Ye, Xu Xu*   

  1. 1. Shanghai Institute for Food and Drug Control, Shanghai, 201203, China
    2. Shanghai Institute of Technology, School of Chemical and Enviromental Engineering, Shanghai 201418, China
    3. Laboratory of Analytical Chemistry, Shanghai Institute of Organic Chemistry, CAS, Shanghai, 200032, China
  • Received:2012-05-21 Revised:2012-07-28 Online:2012-09-15 Published:2012-09-15
  • Contact: Xu Xu*

摘要:

本文使用 Pirkle型 Sumichiral OA-2500手性柱, 研究了正相和反相色谱直接分离阿折地平对映体的流动相条件。使用正相体系, 阿折地平在正己烷-乙醇 (90:10, v/v) 流动相条件下获得了很好的分离 (分离度 Rs 达到 4.0), 而使用推荐的流动相正己烷-乙醇 (60:40, v/v), 则可以在更短的13分钟内获得分离 (分离度Rs为2.7)。使用反相的甲醇和含有0.05 mol/L 醋酸铵的甲醇做流动相, 仅能获得部分分离。用同样的实验条件研究了氨氯地平和尼莫地平的拆分, 并在正相条件下获得了部分分离。

关键词: 手性拆分, 阿折地平, 氨氯地平, 尼莫地平

Abstract:

Direct chiral separation of azelnidipine enantiomers with Pirkle-type Sumichiral OA-2500 column was studied by normal phase and reserve phase conditions. By normal phase, azelnidipine enantiomers were well separated with Rs as 4.0 using hexane-ethanol (90:10, v/v) as mobile phase, and Rs as 2.7 in shorter time (no more than 13 min) using hexane-ethanol (60:40, v/v) as the recommended mobile phase. They were only partially separated by reverse phase using methanol or methanol containing 0.05 mol/L ammonium acetate. Using same chiral column, the chiral separation of other dihydropyridine calcium antagonist analogues almodipine and nimodipine were also studied and showed partial chiral separation in normal phase.

Key words: Chiral separation, Azelnidipine, Almodipine, Nimodipine

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*Corresponding author. Tel.: 86-21-60877215, 60873235