色谱

色谱

• 研究论文 • 上一篇    下一篇

高效液相色谱-质谱法分析菊芋叶中的绿原酸类化合物

袁晓艳1,高明哲1,王锴2,肖红斌1,谭成玉1,杜昱光1

  

  1. 1.Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China;
    2.Northwest Tobacco Test Center, Lianzhou 730030, China
  • 收稿日期:2007-08-13 修回日期:2007-10-24 出版日期:2008-05-30 发布日期:1984-03-25
  • 通讯作者: 肖红斌

Analysis of chlorogenic acids in Helianthus tuberosus Linn leaves using high performance liquid
chromatography-mass spectrometry

YUAN Xiaoyan1, GAO Mingzhe1, WANG Kai2, XIAO Hongbin1, TAN Chengyu1, DU Yuguang1

  

  1. 1.Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China;
    2.Northwest Tobacco Test Center, Lianzhou 730030, China
  • Received:2007-08-13 Revised:2007-10-24 Online:2008-05-30 Published:1984-03-25
  • Contact: Hongbin Xiao

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摘要：

建立了菊芋叶中绿原酸类化合物的高效液相色谱-紫外检测-质谱(HPLC-UV-MS)定性分析方法。液相色谱条件:Inertsil ODS-3色谱柱(250 mm×4.6 mm,5 μm);甲醇和水(含1%乙酸)梯度洗脱,流量1.0 mL/min;柱温35 ℃;检测波长327 nm。质谱条件:Thermo公司TSQ三级四极杆质谱仪;电喷雾电离(ESI)接口;负离子检出模式。采用该方法得到了菊芋叶提取物的紫外检测的色谱图、负离子监测的总离子流图以及相应色谱峰的紫外光谱图和一级、二级质谱图,对其进行解析,鉴别出菊芋叶中的7个绿原酸类成分。该方法简便、快速、灵敏度高,可以很好地对菊芋叶中的绿原酸类化合物进行定性分析。

关键词: 高效液相色谱-质谱法, 菊芋叶 , 绿原酸

Abstract:

To identify chlorogenic acids in Helianthus tuberosus Linn leaves, a method of high performance liquid chromatography-ultraviolet-mass spectrometry (HPLC-UV-MS) was developed. HPLC analysis was performed on an Inertsil ODS-3 column (250mm×4.6 mm, 5 μm). The mobile phase consisted of 1% acetic acid (A) and methanol (B). A gradient program was adopted as follows: 0-10 min, 20%B to 35%B; 10-25 min, 35%B to 50%B; 25-35 min, 50%B to 80%B. The flow rate was set at 1.0 mL/min and the column temperature was 35 ℃. HPLC chromatogram was extracted at 327 nm. The mass spectrometer used was a TSQ triple quadrupole MS equipped with an electrospray ionization （ESI） interface. Initially, the mass spectrometer was programmed to perform full scan ranging from m/z 250-1200. For MS/MS, negative ion monitoring mode was used and the collision energy was set at 10-45 eV. By analyzing UV characteristics and MS fragmentation patterns, 7 chlorogenic acids were assigned to be three categories, i.e., three caffeoylquinic acids, one feruloylquinic acid and three dicaffeoylquinic acids. As the results of the method development efforts, an effective and fast method for the qualitative identification of the chlorogenic acids in Helianthus tuberosus Linn leaves was established.

Key words: chlorogenic acid, Helianthus tuberosus Linn leaves , high performance liquid chromatography-mass spectrometry (HPLC-MS)