色谱

色谱 ›› 2016, Vol. 34 ›› Issue (2): 184-188.DOI: 10.3724/SP.J.1123.2015.08027

• 研究论文 • 上一篇    下一篇

超高效液相色谱-三重四极杆质谱法测定银杏叶提取物及其制剂中银杏酸

孙健, 李丽敏, 胡青, 毛秀红, 季申   

  1. 上海市食品药品检验所, 上海 201203
  • 收稿日期:2015-08-24 出版日期:2016-02-08 发布日期:2012-09-11
  • 通讯作者: 季申
  • 基金资助:

    2015-上海市食品药品监督管理局技术类专项课题.

Determination of ginkgolic acids in the ginkgo biloba extract and its preparations by ultra high performance liquid chromatography-triple quadrupole mass spectrometry

SUN Jian, LI Limin, HU Qing, MAO Xiuhong, JI Shen   

  1. Shanghai Institute for Food and Drug Control, Shanghai 201203, China
  • Received:2015-08-24 Online:2016-02-08 Published:2012-09-11
  • Supported by:

    The 2015 Special Project of Technology Sponsored by Shanghai Food and Drug Administration.

PDF

173

摘要：

建立了超高效液相色谱-串联三重四极杆质谱测定银杏叶提取物及其制剂中银杏酸的方法。采用Agilent Poroshell 120 EC-C18色谱柱(50 mm×3.0 mm, 2.7 μ m),以甲醇-1%冰醋酸溶液(90 : 10, v/v)为流动相,在电喷雾离子化负离子模式下,以多反应监测方式(MRM)检测。银杏酸C13 : 0、C15 : 1、C17 : 1在2~200 μ g/L范围内呈良好的线性关系,相关系数均大于0.999;在5、20和100 μ g/L加标水平下的平均加样回收率为86.3%~114.3%,相对标准偏差(RSD)为0.5%~13.6%;检出限为0.003~0.08 μ g/g,定量限为0.01~0.19 μ g/g。本方法已应用于实际样品的测定。

关键词: 超高效液相色谱-三重四极杆质谱, 银杏酸, 银杏叶胶囊, 银杏叶片, 银杏叶提取物

Abstract:

An analytical method was developed for the determination of ginkgolic acids in ginkgo biloba extract and its preparations by ultra high performance liquid chromatography-triple quadrupole mass spectrometry. A chromatographic column, Agilent Poroshell 120 EC-C18(50 mm×3.0 mm, 2.7 μ m), was used with methanol-1% acetic acid (90 : 10, v/v) as the mobile phase. The ginkgo acids were detected by electrospray ionization mass spectrometry in negative mode with multiple reaction monitoring (MRM) mode. Ginkgo acids C13 : 0, C15 : 1 and C17 : 1 possessed good linear correlations in the mass concentration range from 2 to 200 μ g/L, with the correlation coefficients more than 0.999. The mean recoveries at the spiked levels of 5, 20 and 100 μ g/L were in the range of 86.3%-114.3%, and the RSDs were 0.5%-13.6%. The limits of detection and quantification were 0.003-0.08 μ g/g and 0.01-0.19 μ g/g, respectively. The method was successfully applied to the analysis of actual samples.

Key words: ginkgo biloba extract, ginkgo leaf capsule, ginkgo leaf tablet, ginkgolic acid, ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS)

中图分类号: