色谱

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高效液相色谱-串联质谱法分析姜黄中微量的姜黄素类化合物

李伟1, 肖红斌1, 王龙星1, 梁鑫淼1,2*   

  1. 1.Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China; 2.School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China
  • 收稿日期:2009-03-11 修回日期:2009-04-17 出版日期:2009-05-30 发布日期:1982-09-25
  • 通讯作者: 梁鑫淼

Analysis of minor curcuminoids in Curcuma longa L. by high performance liquid chromatography-tandem mass spectrometry

LI Wei1, XIAO Hongbin1, WANG Longxing1, LIANG Xinmiao1,2*   

  1. 1.Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China; 2.School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China
  • Received:2009-03-11 Revised:2009-04-17 Online:2009-05-30 Published:1982-09-25
  • Contact: LIANG Xinmiao

摘要: 建立了同时检测中药姜黄中3种微量的姜黄素类化合物的高效液相色谱-电喷雾串联质谱分析方法。姜黄根茎经乙醇超声提取后,无需其他处理可直接进样分析。以Microsorb C18色谱柱(250 mm×4.6 mm,5 μm)分离,乙腈和0.1%甲酸水梯度洗脱,在多反应监测模式(MRM)下对目标成分进行定性分析。利用质谱碎裂规律,分别对每个目标成分同时监测8个母离子/特征子离子对的反应过程,首次从姜黄中发现了3个微量的姜黄素类化合物成分。一次性完成了目标成分的同时定性,方法的检出限为0.2 μg/L。结果表明,该方法具有简便、快速、准确、灵敏度高的优点,适用于中药复杂体系中姜黄素类化合物的分析检测。

关键词: 多反应监测模式, 高效液相色谱-串联质谱法, 姜黄 , 姜黄素类化合物, 微量成分

Abstract: A high performance liquid chromatography-tandem mass spectrometric method has been developed for the simultaneous analysis of three minor curcuminoids in the crude extract of Curcuma longa L. After ultrasonic extraction with ethanol, the sample was separated on a Microsorb C18 column (250 mm×4.6 mm, 5 μm) with the gradient elution of acetonitrile and 0.1% (v/v) formic acid aqueous solution as mobile phase, then detected by electrospray ionization tandem mass spectrometry in multi-reaction monitoring (MRM) mode. On the basis of analysis of the fragmentation patterns, the identification of the minor ones was achieved in a single experiment using MRM with 8 precursor-product ion transitions for each component. Using this technique, the three minor curcuminoids were observed in C. longa L. for first time and the limit of detection was 0.2 μg/L. The experimental results show that this method is simple, rapid, accurate, sensitive and suitable for the analysis of curcuminoids in the complex samples of traditional Chinese medicine.

Key words: Curcuma longa L. , curcuminoids, minor constituents, multi-reaction monitoring (MRM) mode, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)