色谱

色谱

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液质联用分析葛根提取物及中药片剂中异黄酮类化合物

田宏哲,王华,关亚风

  

  1. Dalian　Institute of Chemical Physics, The Chinese Academy of Sciences, Dalian 116023, China
  • 收稿日期:2005-05-08 修回日期:1900-01-01 出版日期:2005-09-30 发布日期:1988-03-25
  • 通讯作者: 关亚风

Separation and Identification of Isoflavonoids in Pueraria　 lobata Extracts and Its Preparations by Reversed-Phase Capillary Liquid Chromatography Coupled with Electrospray Ionization Quadrupole Time of Flight Mass Spectrometry

TIAN Hongzhe, WANG Hua, GUAN Yafeng   

  1. Dalian　Institute of Chemical Physics, The Chinese Academy of Sciences, Dalian 116023, China
  • Received:2005-05-08 Revised:1900-01-01 Online:2005-09-30 Published:1988-03-25

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摘要：

采用反相C18毛细管液相色谱柱,以乙腈(含0.1%(体积分数,下同)三氟乙酸)和水(含0.1%三氟乙酸)为流动相梯度洗脱,在26 min内分离了葛根异黄酮提取物以及愈风宁心片中的主要成分。采用毛细管液相色谱/四极杆飞行时间串联质谱仪对葛根提取物以及片剂中的几种主要异黄酮类化合物做了结构分析,发现葛根素是主成分(提取物中其平均质量分数是13.32%;片剂中每片含量19.28~24.34 mg)。对微量未知化合物,用它们的子离子谱图与已知化合物的谱图比较,推测其成分为3′-甲氧基葛根素和3′-甲氧基大豆苷。

关键词: 反相毛细管液相色谱, 葛根素, 葛根异黄酮, 液相色谱-电喷雾离子质谱, 中药

Abstract:

Isoflavonoids in Pueraria lobata extract and its preparations were separated and identified by reversed-phase capillary liquid chromatography (RP-CapLC) coupled with photodiode array (PDA) detector and negative electrospray ionization quadrupole time of flight (Q-TOF) mass spectrometry. The separation was performed on a 150 mm×0.32 mm i.d., 5 μm C18 capillary column, using mobile phase of 0.1% aqueous trifluoroacetic acid solution and acetonitrile containing 0.1% trifluoroacetic acid under gradient elution. The product ion spectra of the deprotonated ions allowed for the identification of puerarin, daidzin and daidzein in the sample. Puerarin was found to be the most abundant component in the extract (about 13%, mass fraction) and its preparations (19.28-24.34 mg per tablet). The structures of trace amount of unknown isoflavonoids were deduced based on the spectra of known compounds. They were proposed to be 3′-methoxypuerarin and 3′-methoxydaidzin.

Key words: isoflavonoids of pueraria lobata, liquid chromatography-electrospray ionization mass spectrometry, puerarin, traditional Chinese medicine , reversed-phase capillary liquid chromatography