色谱

色谱 ›› 2014, Vol. 32 ›› Issue (12): 1306-1312.DOI: 10.3724/SP.J.1123.2014.08023

• 研究论文 • 上一篇    下一篇

基于部分酸水解-亲水作用色谱-质谱的黄芪多糖结构表征

梁图1, 傅青1, 辛华夏1, 李芳冰1, 金郁1, 梁鑫淼1,2   

  1. 1. 华东理工大学药学院, 上海 200237;
    2. 中国科学院大连化学物理研究所, 辽宁 大连 116023
  • 收稿日期:2014-08-25 修回日期:2014-10-10 出版日期:2014-12-08 发布日期:2014-11-28
  • 通讯作者: 梁鑫淼,E-mail:liangxm@ecust.edu.cn.
  • 基金资助:

    高等学校博士学科点专项科研基金项目(20130074120017);中国博士后科学基金面上项目(2013M541481).

Structural characterization of Astragalus polysaccharides using partial acid hydrolysis-hydrophilic interaction liquid chromatography-mass spectrometry

LIANG Tu1, FU Qing1, XIN Huaxia1, LI Fangbing1, JIN Yu1, LIANG Xinmiao1,2   

  1. 1. School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China;
    2. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China
  • Received:2014-08-25 Revised:2014-10-10 Online:2014-12-08 Published:2014-11-28

PDF

477

被引次数

6

摘要：

来自中药的水溶性多糖具有广谱治疗和低毒性特点,是天然药物及保健品研发中的重要组成部分。针对中药多糖结构复杂、难以表征的问题,本文以中药黄芪中的多糖为研究对象,采用"自下而上"法完成对黄芪多糖的表征。首先使用部分酸水解方法水解黄芪多糖,分别考察了水解时间、酸浓度和温度的影响。在适宜条件(4 h、1.5 mol/L三氟乙酸、80 ℃)下,黄芪多糖被水解为特征性的寡糖片段。接下来,采用亲水作用色谱与质谱联用对黄芪多糖部分酸水解产物进行分离和结构表征。结果表明,提取得到的黄芪多糖主要为1→4连接线性葡聚糖,水解得到聚合度4~11的葡寡糖。本研究对其他中药多糖的表征具有一定的示范作用。

关键词: 表征, 部分酸水解, 多糖, 黄芪, 亲水作用色谱, 质谱

Abstract:

Water-soluble polysaccharides from traditional Chinese medicine (TCM) have properties of broad-spectrum treatment and low toxicity, making them as important components in natural medicines and health products. In order to solve the problem of polysaccharides characterization caused by their complex structures, a "bottom-up" approach was developed to complete the characterization of polysaccharides from Astragalus. Firstly, Astragalus pieces were extracted with hot water and then were precipitated by ethanol to obtain Astragalus polysaccharides. Secondly, a partial acid hydrolysis method was carried out and the effects of time, acid concentration and temperature on hydrolysis were investigated. The degree of hydrolysis increased along with the increase of hydrolysis time and acid concentration. The temperature played a great role in the hydrolysis process. No hydrolysis of the polysaccharides occurred at low temperature, while the polysaccharides were almost hydrolyzed to monosaccharide at high temperature. Under the optimum hydrolysis conditions (4 h, 1.5 mol/L trifluoroacetic acid, and 80 ℃), Astragalus polysaccharides were hydrolyzed to characteristic oligosaccharide fragments. At last, a hydrophilic liquid chromatography-mass spectrometry method was used for the separation and structural characterization of the polysaccharide hydrolysates. The results showed that the resulting polysaccharides were mainly 1→4 linear glucan, and gluco-oligosaccharides with the degrees of polymerization (DP) of 4-11 were obtained after partial acid hydrolysis. The significance of this study is that it is the guidance for the characterization of other TCM polysaccharides.

Key words: Astragalus, characterization, hydrophilic interaction liquid chromatography (HILIC), mass spectrometry (MS), partial acid hydrolysis, polysaccharides

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