色谱

色谱 ›› 2014, Vol. 32 ›› Issue (12): 1404-1408.DOI: 10.3724/SP.J.1123.2014.07025

• 技术与应用 • 上一篇    

高速逆流色谱法分离制备中药诃子中的没食子酸

李忠琴, 李秋云, 江兴龙, 张坤, 关瑞章   

  1. 集美大学水产学院, 鳗鲡现代产业技术教育部工程研究中心, 福建 厦门 361021
  • 收稿日期:2014-07-16 修回日期:2014-09-29 出版日期:2014-12-08 发布日期:2014-11-28
  • 通讯作者: 关瑞章,E-mail:rzhguan@jmu.edu.cn.
  • 基金资助:

    国家海洋局海洋经济创新发展区域示范专项(2012FJ03);厦门市重点项目(3502Z20110014,3502Z20123027);鳗鲡现代产业技术教育部工程研究中心开放基金项目(RE201305);国家级大学生创新创业训练计划项目(Z81231).

Isolation and preparation of gallic acid from Terminalia chebula Retz. with high-speed counter-current chromatography

LI Zhongqin, LI Qiuyun, JIANG Xinglong, ZHANG Kun, GUAN Ruizhang   

  1. Fisheries College, Jimei University, Engineering Research Centre of the Modern Industry Technology for Ministry of Education, Xiamen 361021, China
  • Received:2014-07-16 Revised:2014-09-29 Online:2014-12-08 Published:2014-11-28

PDF

290

被引次数

18

摘要：

利用高速逆流色谱法从100 mg诃子醇提物中一次性分离制备得到8.6 mg没食子酸。通过分析型高速逆流色谱对5种溶剂系统进行筛选,确定以正己烷-乙酸乙酯-甲醇-水(体积比为1:5:1:5)为两相溶剂体系并放大到制备型上,以上相为固定相,下相为流动相,在主机转速850 r/min、流动相流速2 mL/min、检测波长254 nm的条件下进行分离制备,获得4个分离峰(组分Ⅰ、Ⅱ、Ⅲ、Ⅳ)。经高效液相色谱检测,按照面积归一法计算,其中组分Ⅲ的纯度达96.40%。经电喷雾电离质谱分析,并结合与没食子酸标准品的高效液相色谱测定结果的对比,确定组分Ⅲ为没食子酸。该方法简便、快速、重复性好,适合于诃子中没食子酸的分离制备。

关键词: 高速逆流色谱, 诃子, 没食子酸

Abstract:

A separation method based on high-speed counter-current chromatography (HSCCC) has been established for the isolation and preparation of gallic acid from the ethanol extract of Terminalia chebula Retz. After comparing five kinds of solvent protocols of HSCCC, the two-phase system of n-hexane-ethyl acetate-methanol-water (1:5:1:5, v/v/v/v) was finally chosen as the operating solvent of HSCCC for the separation of gallic acid, in which the lower phase was used as the mobile phase and the upper phase as stationary phase. The detection in the experiments was performed with an ultraviolet detector at 254 nm. Under the conditions of rotation speed of 850 r/min, lower phase flow rate of 2 mL/min, four peaks (Ⅰ/Ⅱ/Ⅲ/Ⅳ) were displayed on HSCCC chromatogram. Among them, only peak Ⅲ contained a large amount of gallic acid (about 96.40%), which was confirmed by electrospray ionization mass spectrometry (ESI-MS) and high performance liquid chromatographic (HPLC) analysis. As much as 8.6 mg of gallic acid was obtained from 100 mg of the ethanol extract of Terminalia chebula Retz., indicating the method is simple, robust and efficient for the preparation of gallic acid.

Key words: Terminalia chebula Retz, gallic acid, high-speed counter-current chromatography (HSCCC)

中图分类号: