色谱

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羧甲基-β-环糊精手性流动相添加剂法拆分帕罗西汀及其中间体对映体

卢铁刚,杨茂俊

  

  1. Sichuan Industrial Institute of Antibiotic, Chengdu 610051, China
  • 收稿日期:2007-05-24 修回日期:2007-09-07 出版日期:2007-11-30 发布日期:1984-12-25
  • 通讯作者: 卢铁刚

Separation of Paroxetine and Its Intermediate Enantiomers by High Performance Liquid Chromatography Using Carboxy-methyl-β-Cyclodextrin as Chiral Mobile Phase Additive

LU Tiegang, YANG Maojun   

  1. Sichuan Industrial Institute of Antibiotic, Chengdu 610051, China
  • Received:2007-05-24 Revised:2007-09-07 Online:2007-11-30 Published:1984-12-25
  • Contact: LU Tiegang

摘要:

建立了帕罗西汀及其中间体的高效液相色谱手性拆分分析方法。选用C18柱(4.6 mm×250 mm,5 μm),流动相为0.1%磷酸-甲醇(体积比为65∶35,含0.38 g/L羧甲基-β-环糊精,以三乙胺调pH 7.2),柱温25 ℃,检测波长210 nm。结果表明,帕罗西汀及其中间体HFP的对映异构体在30 min内同时得到了基线分离,该法与手性固定相法相比具有分离效果更好的优势。

关键词: 对映体分离, 高效液相色谱, 帕罗西汀 , 手性流动相添加剂, 羧甲基-β-环糊精

Abstract:

A high performance liquid chromatographic method to separate the respective enantiomers of paroxetine and its intermediate was developed using chiral mobile phase additive. Separation was performed on a Diamond C18 column (4.6 mm×250 mm, 5 μm). The mobile phase was 0.1% phosphate acid-methanol (65∶35, v/v) containing 0.38 g/L carboxymethyl-β-cyclodextrin and the pH was adjusted to 7.2 by triethylamine.The detection wavelength was set at 210 nm and the temperature was 25 ℃. With this method, paroxetine’s trans/cis isomers and their enantiomers as well as intermediate HFP’s trans/cis isomers and their enantiomers were separated simultaneously. The method is simple, rapid with high resolutions.

Key words: carboxymethyl-β-cyclodextrin (CM-β-CD), chiral mobile phase additive, enantiomeric resolution, paroxetine , high performance liquid chromatography (HPLC)