化学学报 ›› 2009, Vol. 67 ›› Issue (22): 2613-2618. 上一篇    下一篇

研究论文

朝鲜淫羊藿的色谱指纹图谱及液相色谱/电喷雾串联质谱分析

窦建鹏a,b,宋凤瑞a,刘志强a,刘淑莹*,a   

  1. (a中国科学院长春应用化学研究所 长春 130022) (b吉林大学生物与农业工程学院 长春 130022)
  • 投稿日期:2009-01-01 修回日期:2009-03-24 发布日期:2009-07-08
  • 通讯作者: 刘志强 E-mail:liuzq@ciac.jl.cn

Studies on Fingerprint of Epimedium koreanum in Changbai Mountains by High-performance Liquid Chromatography

Dou, Jianpeng a,b,Song, Fengruia,Liu, Zhiqianga,Liu, Shuying*,a   

  1. (a Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022) (b College of Biological and Agricultural Engineering, Jilin University, Changchun 130022)
  • Received:2009-01-01 Revised:2009-03-24 Published:2009-07-08

建立了长白山区朝鲜淫羊藿药材的高效液相色谱指纹图谱的分析方法. 确定了18批朝鲜淫羊藿药材的13个共有峰, 该指纹图谱的精密度、稳定性和重现性的相对标准偏差均低于3.0%. 结合液相色谱/电喷雾串联质谱对特征峰进行了结构确认, 并根据电喷雾串联质谱数据推测了13个特征化合物的结构. 结果表明采用高效液相色谱与质谱联用技术对朝鲜淫羊藿色谱指纹图谱中的特征峰进行结构确认, 使其色谱指纹图谱的特征性更强, 更适合于药材质量的鉴别与评价.

关键词: 朝鲜淫羊藿, 黄酮, 高效液相色谱, 电喷雾串联质谱, 指纹图谱

A high-performance liquid chromatography (HPLC) fingerprint method was developed for analysis of Epimedium koreanum Nakai in Changbai mountains. The chromatographic conditions are as follows: Zorbax Extend C18 (5 µm, 4.6 mm×250 mm, Agilent) column; mobile phase: 0.5% acetic acid-water and methanol, gradient elute; flow rate: 0.6 mL/min; column temperature: 25 ℃; wavelength: 270 nm; run time: 80 min. 13 common peaks were selected from 18 crude extracts of Epimedium koreanum, and their structures were identificated by electrospray ionization tandem mass spectrometry (ESI-MS/MS), and according to the data of MS, the structures of the 13 compounds were speculated. Relative standard deviation values (RSD) of precision, stability and repeatability are less than 3.0%. The results indicate the HPLC fingerprint of Epimedium koreanum Nakai. will show more characters through identification of component structures using an HPLC-MS/MS method.

Key words: Epimedium koreanum, flavonoid, high-performance liquid chromatography, electrospray ionization mass spectrometry, fingerprint spectrum