色谱

色谱

• 研究简报 • 上一篇    下一篇

杜仲中京尼平甙酸的硅胶柱色谱分离纯化及反相高效液相色谱/液相色谱-电喷雾质谱/核磁共振鉴定

曹慧1,陈晓青1,肖建波1,唐兆麒1,欧阳冬生2

  

  1. 1. Department of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China;2. Institute of Clinical Pharmacology, Central South University, Changsha 410078, China
  • 收稿日期:2004-08-30 修回日期:1900-01-01 出版日期:2005-09-30 发布日期:1988-03-25
  • 通讯作者: 陈晓青

Isolation, Purification and Identification of Geniposidic Acid in Eucommia ulmoides Oliv. by Silica Column Chromatography, Reversed-Phase High Performance Liquid Chromatography, Liquid Chromatography-Electrospray Ionization Mass Spectrometry and Nuclear Magnetic Resonance

CAO Hui1, CHEN Xiaoqing1, XIAO Jianbo1, TANG Zhaoqi1, OUYANG Dongsheng2   

  1. 1. Department of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China;2. Institute of Clinical Pharmacology, Central South University, Changsha 410078, China
  • Received:2004-08-30 Revised:1900-01-01 Online:2005-09-30 Published:1988-03-25

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摘要：

建立了杜仲中京尼平甙酸的硅胶柱色谱分离纯化及反相高效液相色谱/液相色谱-电喷雾质谱/核磁共振(RP-HPLC/LC-ESI-MS/NMR)鉴定方法。杜仲皮经粉碎后,用70%乙醇提取,提取液经减压蒸馏至干,再用甲醇溶解，然后吸附于硅胶上,并以不同体积比的氯仿-甲醇混合液按洗脱剂的极性由小到大进行洗脱,以RP-HPLC法检测洗脱液中物质的种类和含量。结果表明:洗脱剂为氯仿-甲醇（体积比为8∶1）的洗脱液经分析为单一组分,其保留时间为5.142 min；以对照品京尼平甙酸添加法测定,其峰高增加；相关紫外光谱和红外光谱检测结果与京尼平甙酸对照品基本一致；结合LC-ESI-MS、 1H-NMR和13C-NMR等测定，确定该洗脱组分为京尼平甙酸。

关键词: 杜仲, 反相高效液相色谱法, 核磁共振, 京尼平甙酸, 液相色谱-电喷雾质谱, 中药 , 柱色谱法

Abstract:

The methods using silica column chromatography, reversed-phase high performance liquid chromatography, liquid chromatography-electrospray ionization mass spectrometry and nuclear magnetic resonance (RP-HPLC/LC-ESI-MS/NMR) for the isolation, purification and identification of geniposidic acid (GPA) in Eucommia ulmoides Oliv. were established. The crude extract of E. ulmoides was obtained after E. ulmoides was extracted with 70% ethanol and the extract was concentrated under reduced pressures. The obtained crude extract dissolved in methanol was injected to a silica gel column and eluted with chloroform-methanol. The eluted fractions were analyzed by RP-HPLC. The eluant from chloroform-methanol (8∶1, v/v) was indicated to be a single component by HPLC with a retention time of 5.142 min. The HPLC analysis of the mixture of this fraction with a GPA standard resulted in a single peak. The ultraviolet and infrared spectra of the eluted solution were essentially the same to those of GPA. On the other hand, LC-ESI-MS, 1H- and 13C-NMR experiments also indicated that the fraction was identical to GPA.

Key words: Eucommia ulmoides Oliv.； traditional Chinese medicine , geniposidic acid, liquid chromatography-electrospray ionization mass spectrometry, nuclear magnetic resonance, reversed-phase high performance liquid chromatography, column chromatography