化学学报 ›› 2007, Vol. 65 ›› Issue (23): 2743-2749. 上一篇    下一篇

研究论文

高效毛细管电泳-电喷雾飞行时间质谱联用分析黄连中的生物碱

陈军辉1,2, 赵恒强1, 李文龙1, 王小如*,1,3, 黎先春1, 杨黄浩1   

  1. (1国家海洋局第一海洋研究所 青岛现代分析技术及中药标准化重点实验室 青岛 266061)
    (2中国海洋大学化学化工学院 青岛 266003)
    (3厦门大学化学化工学院化学系 现代分析科学教育部重点实验室 厦门 361005)
  • 投稿日期:2007-05-09 修回日期:2007-07-02 发布日期:2007-12-14
  • 通讯作者: 王小如

Analysis of Alkaloids in Coptis chinensis Franch by High Performance Capillary Electrophoresis-Electrospray Ionization Time of Flight Mass Spectrometry

CHEN Jun-Hui1,2; ZHAO Heng-Qiang1; LI Wen-Long1; WANG Xiao-Ru*,1,3; LEE Frank Sen-Chun1; YANG Huang-Hao1   

  1. (1 Qingdao Key Laboratory of Analytical Technology Development and Standardization of Chinese Traditional Medicines, First Institute of Oceanography of State Oceanic Administration, Qingdao 266061)
    (2 College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266003)
    (3 Department of Chemistry and the Key Laboratory of Analytical Science of the Ministry of Education, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005)
  • Received:2007-05-09 Revised:2007-07-02 Published:2007-12-14
  • Contact: WANG Xiao-Ru

建立了高效毛细管电泳-电喷雾飞行时间质谱联用(HPCE-ESI-TOF/MS)快速定性分析黄连中生物碱类化合物的分析方法. 使用未涂层石英毛细管, 以50 mmol/L乙酸铵-0.5%甲醇溶液(用氨水调至pH=7.2)作为运行缓冲液, 分离电压为25 kV; 鞘液组成为50%甲醇-49.5%水-0.5%乙酸, 鞘液流速为4 μL/min; 质谱选用正离子模式, 碰撞电压(Fragmentor)为100 V. 结果表明, 通过各色谱峰紫外光谱和质谱测得精确分子量结果, 结合文献, 对黄连中7种生物碱进行了鉴定. 表明本方法简便、快速, 是黄连中生物碱类化合物快速分离、鉴别的有效方法.

关键词: 高效毛细管电泳-电喷雾飞行时间质谱, 黄连, 生物碱类化合物

A new method for the analysis of alkaloids in Coptis chinensis Franch was established by high performance capillary electrophoresis-electrospray ionization time of flight mass spectrometry (HPCE-ESI-TOF/MS). The real samples were separated by an uncoated capillary. 50 mmol/L ammonium acetate containing 0.5% methanol (pH=7.2) was used as the running buffer, and separation voltage was 25 kV. A coaxial sheath flow interface was used as the CE-MS interface, and a 50% methanol-49.5% water- 0.5% acetic acid mixture was used as the sheath liquid with a flow rate of 4 μL/min. The lens voltages in a positive ion mode with a collision induced dissociation (CID) voltage of 100 V were used for ESI-TOF/MS analysis. Seven alkaloids in Coptis chinensis Franch methanol extracts were separated and identified by CE-DAD and CE-ESI-TOF/MS. The coupling of HPCE separation with accurate mass measurement capability of ESI-TOF/MS provides an attractive tool for the identification of alkaloid compounds in Coptis chinensis Franch.

Key words: high performance capillary electrophoresis-electrospray ionization time of flight mass spectrometry, Coptis chinensis Franch; alkaloid