色谱

色谱

• 研究论文 • 上一篇    下一篇

二维液相色谱-质谱联用分离中药复方葛根芩连汤中的有效成分

郭菲1,3,王彦1,王刃锋1,阎超1,2,3

  

  1. 1.School of Pharmacy, Shanghai Jiao Tong University, Shanghai 200240, China;
    2.Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China;
    3.Unimicro （Shanghai） Technologies Co., Ltd., Shanghai 201203, China
  • 收稿日期:2007-06-29 修回日期:2007-09-17 出版日期:2008-01-30 发布日期:1984-09-25
  • 通讯作者: 阎超

Application of two-dimensional liquid chromatography coupled with mass spectrometry for the separation of active compounds in Gegen Qinlian decoction

GUO Fei1,3, WANG Yan1, WANG Renfeng1, YAN Chao1,2,3   

  1. 1.School of Pharmacy, Shanghai Jiao Tong University, Shanghai 200240, China;
    2.Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China;
    3.Unimicro （Shanghai） Technologies Co., Ltd., Shanghai 201203, China
  • Received:2007-06-29 Revised:2007-09-17 Online:2008-01-30 Published:1984-09-25

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摘要：

建立了二维液相色谱-质谱联用方法分离中药复方葛根芩连汤的成分。以CN柱作第一维色谱柱,水和甲醇梯度洗脱分离;以ODS柱作第二维色谱柱,20 mmol/L乙酸铵缓冲液和乙腈梯度洗脱分离;质谱检测采用电喷雾电离/大气压化学电离（ESI/APCI）复合离子源,正负离子扫描。实验结果表明搭建的二维液相色谱的峰容量显著高于一维色谱,分离效率得到了明显的提高。以第一维色谱的第3个流分为例,对其二维分离进行仔细分析,发现质谱比紫外光谱检测到的组分多,质谱中采用负离子模式比正离子模式检测到的组分多。表明搭建的二维液相色谱-质谱分离平台分离效果好,提高了液相色谱的峰容量和分离效率。该方法操作简便,可作为中药等复杂体系分离分析的有效手段。

关键词: 电喷雾电离/大气压化学电离复合离子源, 二维液相色谱-质谱联用, 葛根芩连汤 , 活性成分

Abstract:

An system of two-dimensional liquid chromatography (2D-LC) coupled with mass spectrometry was developed for the separation of components in Gegen Qinlian decoction, a complex traditional Chinese medicine. A CN column was used in the first dimensional chromatography, with gradient elution using water and methanol as the mobile phase A and mobile phase B, respectively; an ODS column was used in the second dimensional chromatography, with gradient elution using 20 mmol/L ammonium acetate buffer and acetonitrile as the mobile phase A and mobile phase B, respectively. The effluent was detected by mass spectrometry with electrospray ionization （ESI）/atmospheric pressure ionization （APCI） combined ion source and positive and negative scan modes. The components in Gegen Qinlian decoction was separated with the 2D-LC system with peak capacity up to 8000. Compared with UV detection, MS detected more components, especially in the negative mode. The 2D-LC/MS system provides higher peak capacity, better resolution and the capacity of peak identification. It is suitable for the analysis of complex samples such as the traditional Chinese medicine.

Key words: active compounds, electrospray ionization/atmosphere pressure ionization （ESI/APCI） combined ion source, Gegen Qinlian decoction
, two-dimensional liquid chromatography-mass spectrometry