基于亲水作用色谱-串联质谱方法的玉竹多糖质量评价  

Quality evaluation of Polygonatum odoratum polysaccharides based on hydrophilic interaction chromatography-tandem mass spectrometry method

作　　者：傅青[1] 王惠 金郁[1] FU Qing1, WANG Hui2, JIN Yu1(1. School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China;2. Department of Food, Shanghai Trade School, Shanghai 200333, China)

机构地区：[1]华东理工大学药学院,上海200237 [2]上海市贸易学校食品教研室,上海200333

出　　处：《中国科技论文》2018年第6期660-666,共7页China Sciencepaper

基　　金：高等学校博士学科点专项科研基金资助项目(20130074120017)

摘　　要：中药多糖具有广泛的药理活性,在中药质量评价过程中不可或缺,但因其分子量巨大、结构复杂,质量评价非常困难。因此,建立有效可行的多糖质量评价方法具有重要意义。以中药玉竹为对象,建立基于亲水作用色谱-串联质谱分离表征的玉竹多糖质量评价方法。通过甲醇脱色、水提醇沉法制备玉竹多糖,提取率为10.3%。优化部分酸水解方法,得到最佳水解条件为三氟乙酸浓度为1.5mol/L、温度为80℃、水解时间为4h,可将玉竹多糖水解为特征性的寡糖片段。利用亲水作用色谱-串联质谱对降解后的寡糖片段进行表征。结果表明,得到的玉竹中性多糖主链为1→4连接的果聚糖,或含少量葡萄糖。研究结果将为玉竹多糖质量评价标准的完善提供基础数据。As ingredient with extensive activities,polysaccharides are indispensable in quality control of traditional Chinese medicines（TCMs）.However,because of its large molecular weight and complex structure,the quality evaluation is very difficult.Therefore,it is of great value to build effective and feasible method for the quality control of polysaccharide.Using Polygonatum odoratumas an object,the quality evaluation method of polysaccharides was built based on hydrophilic interaction chromatography-tandem mass spectrometry.P.odoratumpolysaccharides were prepared by methanol decolorization,water extract and alcohol precipitation,and the extract rate was 10.3%.Partial acid hydrolysis condition was optimized as following：concentration of trifluoroacetic acid 1.5 mol/L,temperature 80 ℃ and 4 h.Hydrophilic interaction liquid chromatography（HILIC）-MS/MS method was used for characterization of the oligosaccharides after hydrolysis.The results showed that the neutral polysaccharides obtained was 1→4 connected polyfructosans containing some glucose.The results will provide the basic data for the improvement of the quality evaluation standard of P.odoratumpolysaccharides.

关 键 词：液质联用 亲水作用色谱 结构表征 质量评价 质谱 玉竹多糖 

分 类 号：O658[理学—分析化学]