高效液相色谱-质谱法分析菊芋叶中的绿原酸类化合物  

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

作　　者：袁晓艳[1] 高明哲[1] 王锴 肖红斌[1] 谭成玉[1] 杜昱光[1] 

机构地区：[1]中国科学院大连化学物理研究所,辽宁大连116023 [2]西北烟草质量监督检查站,甘肃兰州730030

出　　处：《色谱》2008年第3期335-338,共4页Chinese Journal of Chromatography

基　　金：中国科学院知识创新工程领域前沿项目资助

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(250mm×4.6mm,5μm);甲醇和水(含1%乙酸)梯度洗脱,流量1.0mL/min;柱温35℃;检测波长327nm。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。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 250-1 200. 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.

关 键 词：高效液相色谱-质谱法 绿原酸 菊芋叶 

分 类 号：O658[理学—分析化学]