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色谱

• 研究论文 •    下一篇

高效液相色谱-二极管阵列检测/质谱法分析生脉饮煎剂中的人参皂甙类成分

王占良,王弘,陈世忠

  

  1. Research Laboratory of Traditional Chinese Medicine, School of Pharmaceutical Sciences,
    Peking University, Beijing 100083, China

  • 收稿日期:2006-03-02 修回日期:2006-05-23 出版日期:2006-07-30 发布日期:1986-12-25
  • 通讯作者: 陈世忠

Analysis of Ginsenosides in Sheng-Mai-Yin Decoction by High Performance Liquid Chromatography-Diode
Array Detection-Electrospray Mass Spectrometry

WANG Zhanliang, WANG Hong, CHEN Shizhong

  

  1. Research Laboratory of Traditional Chinese Medicine, School of Pharmaceutical Sciences,
    Peking University, Beijing 100083, China

  • Received:2006-03-02 Revised:2006-05-23 Online:2006-07-30 Published:1986-12-25
  • Contact: CHEN Shizhong

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摘要：

采用高效液相色谱-二极管阵列检测/质谱（HPLC-DAD/MS）联用技术,以10 mmol/L醋酸铵和乙腈混合溶液梯度洗脱
系统为流动相,应用C18色谱柱对生脉饮煎剂中人参皂甙类成分进行分离鉴定。分析结果表明:生脉饮煎剂中主要含有17个
人参皂甙类成分,即20(R)-人参皂甙Rh1、Rh2、Rg3、Rg2,20(S)-人参皂甙Rh1、Rh2、Rg3、Rg2,人参皂甙Rf、Rg6、Rg5
、F4、Rk1、Rk3、Rh4,20(S)-和20(R)-原人参三醇。人参皂甙成分在煎煮过程中发生了很大变化,主要变成了一些中低
极性产物,这是因为煎煮过程中发生了水解、差向异构、脱水等反应。该方法简便、精确、灵敏度高,可以用来分析生脉
饮煎剂中人参皂甙的变化。

关键词: 高效液相色谱法, 人参皂甙, 生脉饮煎剂 , 质谱法

Abstract:

A method of high performance liquid chromatography coupled with diode array detection and
electrospray ionization mass spectrometry (HPLC-DAD/MS) in negative ion mode was developed for the
analysis of ginsenosides in Sheng-Mai-Yin decoction (Panax gingeng C. A. Mey, Ophiopogon japonicus
(Thunb.) Ker-Gawl, Shisandra chinensis (Turcz.) Baill.). The analyses were preformed on a
reversed-phase C18 column (4.6 mm i.d.×150 mm, 5 μm) using a binary eluent (10 mmol/L ammonium
acetate (A) and acetonitrile (B), 1 mL/min) under gradient conditions (60%A-40%A at 0-30 min,
40%A-30%A at 30-40 min). Seventeen ginsenosides (20 (R)-Rh1, Rh2, Rg3, Rg2; 20(S)-Rh1, Rh2, Rg3,
Rg2; Rf, Rg6, Rg5, F4, Rk1, Rk3, Rh4; 20 (S)- and 20 (R)-protopanaxatriol) were well separated and
detected at 203 nm by a DAD detector. The effluent from the DAD detector was introduced into the
electrospray ionization (ESI) source in a post-column splitting flow rate at 0.3 mL/min. In the mass
spectrum two major ions ［M-H］- and ［M+AcO］- were observed for ginsenoside standards (20 (R)-Rh1,
Rg3, Rh2; 20 (S)-Rh1, Rg3, Rh2; 20 (S)- and 20 (R)-protopanaxatriol) and ginsenosides in
Sheng-Mai-Yin decoction. Some other ions ［M-Glc-H］-, ［M-2Glc-H］-, ［M-Rha-H］-and ［M-Rha-Glc-H］
- were also found in the mass spectrum of ginsenosides of Sheng-Mai-Yin decoction. In the decoction
process ginsenosides changed into constituents of moderate and low polarity by hydrolysis,
isomerization and dehydration at the site of C-20 and hydrolysis reaction also occurred at the site
of C-3 or C-6. The work above presents a quick and accurate assay method which can could be used for
the qualitative analysis of ginsenosides in Sheng-Mai-Yin decoction and the quality control of
Sheng-Mai-Yin preparation.

Key words:
Sheng-Mai-Yin decoction , ginsenosides, mass spectrometry (MS), high performance liquid chromatography (HPLC)