色谱

• 研究论文 • 上一篇    下一篇

高速逆流色谱与硅胶柱色谱结合分离制备高纯度芦荟素异构体

黄丹凤,曹学丽,赵华,董银卯

  

  1. Beijing Key Laboratory of Plant Resources Research and Development, School of Chemical and Environmental Engineering, Beijing Technology and Business University, Beijing 100037, China
  • 收稿日期:2005-01-17 修回日期:2005-11-21 出版日期:2006-01-30 发布日期:1987-09-25
  • 通讯作者: 曹学丽

Preparative Separation of Aloin Diastereoisomers by High-Speed Countercurrent Chromatography Combined with Silica Gel Column Chromatography

HUANG Danfeng, CAO Xueli, ZHAO Hua, DONG Yinmao   

  1. Beijing Key Laboratory of Plant Resources Research and Development, School of Chemical and Environmental Engineering, Beijing Technology and Business University, Beijing 100037, China
  • Received:2005-01-17 Revised:2005-11-21 Online:2006-01-30 Published:1987-09-25

摘要:

芦荟素是芦荟叶中主要的蒽醌类成分,通常以芦荟素A和B两种非对映异构体形式并存,目前已成为许多芦荟产品质量控制指标之一。采用高速逆流色谱和硅胶柱色谱结合的方法,从老芦荟干粉中分离制备了高纯度的芦荟素A(纯度为98%)和芦荟素B(纯度为96%)样品,并采用快原子轰击质谱(FAB-MS)和核磁共振氢谱(1H NMR)以及GOESY(gradient-enhanced nuclear Overhauser effect spectroscopy)等方法对所得的两个芦荟素异构体的立体构象进行了确认。该法具有制备量大和分离效率高的特点。

关键词: 分离制备, 高速逆流色谱, 高效液相色谱, 硅胶柱色谱, 芦荟素异构体

Abstract:

Aloin, naturally a mixture of two diastereoisomers, aloin A and aloin B, is the major anthraquinone in aloe, and now served as one of the important control constituents in most of the commercial aloe products. High-speed countercurrent chromatography (HSCCC) combined with silica gel column chromatography was developed for the preparative separation of the two individual aloins. Aloin A (98%) and aloin B (96% ) were obtained. Fast atom bombardment mass spectrometry (FAB-MS), 1H nuclear magnetic resonance (1H NMR) and GOESY (gradient-enhanced nuclear Overhauser effect spectroscopy) were employed for the elucidation of their structure conformation. The developed method is of high preparative capacity and high efficiency in resolution.

Key words: aloin diastereoisomers , high performance liquid chromatography (HPLC), preparative separation, silica gel column chromatography, high-speed countercurrent chromatography (HSCCC)