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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
引用本文:王占良,王弘,陈世忠.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[J].色谱,2006,24(4):325-330.
作者姓名:王占良  王弘  陈世忠
作者单位:Research Laboratory of Traditional Chinese Medicine, School of Pharmaceutical Sciences, ;Peking University, Beijing 100083, China
基金项目:致谢:感谢岛津公司北京分析测试中心在HPLC/DAD/MS分析仪器方面提供的帮助.
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  质谱法  人参皂甙  生脉饮煎剂
文章编号:1000-8713(2006)04-0325-06
收稿时间:2006-02-27
修稿时间:2006年2月27日

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.Analysis of Ginsenosides in Sheng-Mai-Yin Decoction by High Performance Liquid Chromatography-Diode Array Detection-Electrospray Mass Spectrometry[J].Chinese Journal of Chromatography,2006,24(4):325-330.
Authors:WANG Zhanliang  WANG Hong  CHEN Shizhong
Institution:Research Laboratory of Traditional Chinese Medicine, School of Pharmaceutical Sciences, ;Peking University, Beijing 100083, China
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. x 150 mm, 5 microm) 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.
Keywords:high performance liquid chromatography (HPLC)  mass spectrometry(MS)  ginsenosides  Sheng-Mai-Yin decoction
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