色谱

色谱 ›› 2012, Vol. 30 ›› Issue (03): 327-331.DOI: 10.3724/SP.J.1123.2011.11021

• 技术与应用 • 上一篇    

高良姜中二苯基庚烷类化合物的高速逆流色谱分离制备

叶琼仙1, 谭雄1, 朱龙平1,2, 赵志敏1, 杨得坡1,2, 尹胜1,2, 王冬梅1,2*   

  1. 1. 中山大学药学院, 广东 广州 510006; 2. 广东省现代中药工程技术研究开发中心, 广东 广州 510006
  • 收稿日期:2011-11-11 修回日期:2011-12-19 出版日期:2012-03-28 发布日期:2012-05-02
  • 通讯作者: 王冬梅,博士,副教授,主要从事天然药物化学研究. Tel: (020)39943042,
  • 基金资助:

    国家科技部中澳国际合作项目(2009DFA31230)和中山大学医科学生业余科研基金项目(［2010］31号).

Isolation and purification of diarylheptanoids from Alpinia officinarum Hance by high-speed counter-current chromatography

YE Qiongxian1, TAN Xiong1, ZHU Longping1,2, ZHAO Zhimin1, YANG Depo1,2, YIN Sheng1,2, WANG Dongmei1,2*   

  1. 1. School of Pharmaceutical Sciences, Sun Yat-Sen University, Guangzhou 510006, China; 2. Guangdong Technology Research Center for Advanced Chinese Medicine, Guangzhou 510006, China
  • Received:2011-11-11 Revised:2011-12-19 Online:2012-03-28 Published:2012-05-02

PDF

336

被引次数

3

摘要：

应用高速逆流色谱法(HSCCC)分离纯化了高良姜中3种二苯基庚烷类化合物。以正己烷-乙酸乙酯-甲醇-水(2:3:1.75:1, v/v/v/v)为两相溶剂系统,下相为固定相,上相为流动相,在主机转速为858 r/min、流速1.5 mL/min的条件下,从122.20 mg高良姜石油醚萃取物中经一步HSCCC分离可制备得到5R-羟基-7-(4-羟基-3-甲氧基苯基)-1-苯基-3-庚酮(7.37 mg)、7-(4-羟基-3-甲氧基苯基)-1-苯基-4E-烯-3-庚酮(9.11 mg)和1,7-二苯基-4E-烯-3-庚酮(15.44 mg),经高效液相色谱分析,纯度均大于93%,各化合物的结构由质谱和核磁共振氢谱、碳谱鉴定确证。该方法简便、快速、高效,可用于高良姜中二苯基庚烷类化合物的快速分离制备。

关键词: 二苯基庚烷类化合物, 高良姜, 高速逆流色谱, 制备, 中药材

Abstract:

Three diarylheptanoids were isolated and purified from Alpinia officinarum Hance by high-speed counter-current chromatography (HSCCC). A two-phase solvent system composed of hexane-ethyl acetate-methanol-water (2:3:1.75:1, v/v/v/v) was used. The lower phase was used as the stationary phase. From 122.20 mg petroleum ether extract of A. officinarum, 5R-hydroxy-7-(4-hydroxy-3-methoxyphenyl)-1-phenyl-3-heptanone (7.37 mg), 7-(4-hydroxy-3-methoxyphenyl)-1-phenyl-4E-en-3-heptanone (9.11 mg) and 1,7-diphenyl-4E-en-3-heptanone (15.44 mg) with purities over 93% were obtained within 140 min in one-step separation by HSCCC under the conditions of a flow rate of 1.5 mL/min and 858 r/min. The obtained compounds were analyzed by high performance liquid chromatography to provide their purities, and their structures were confirmed by using mass spectrometry, 1H-nuclear magnetic resonance (1H-NMR) and 13C-NMR. The established HSCCC method is relatively simple, fast and suitable for the isolation and purification of diarylheptanoids from A. officinarum.

Key words: Alpinia officinarum Hance, diarylheptanoids, preparation, traditional Chinese herbal medicine, high-speed counter-current chromatography (HSCCC)