文献类型：期刊文献

中文题名：麦冬多糖单糖组成的分析方法研究：

英文题名：Study on the analysis method of monosaccharide composition in Ophiopogon japonicus polysaccharides

作者：胡坪[1,2];乔晚芳[1,2];沈骏文[2];张弛[1,2];章弘扬[1,2];张敏[3];王月荣[1,2]

机构：[1]上海市功能性材料化学重点实验室,华东理工大学,上海200237;[2]华东理工大学化学与分子工程学院,上海200237;[3]华东理工大学药学院,上海200237

年份：2013

卷号：33

期号：1

起止页码：50

中文期刊名：药物分析杂志

外文期刊名：Chinese Journal of Pharmaceutical Analysis

收录：CSTPCD;;北大核心:【北大核心2011】；CSCD:【CSCD2013_2014】；

基金：国家自然科学基金(21006023);国家十一五重大项目创新药物开发项目(2009ZX09103-364)资助

语种：中文

中文关键词：麦冬多糖;高效液相色谱-蒸发光散射检测器;全水解;方法学验证;单糖组成;果糖测定

外文关键词：Ophiopogon japonicus polysaccharides;high performance liquid chromatography -evaporative light scat-tering detector; full hydrolysis ; method validation ; monosaccharide composition analysis ; fructose determination

摘要：目的:建立一种麦冬多糖中单糖组成的高效液相色谱(HPLC)-蒸发光散射(ELSD)测定方法。方法:以三氟乙酸(TFA)水解麦冬多糖,采用Waters XBridgeTMAmide色谱柱,乙腈-水-三乙胺(75∶25∶0.2)为流动相,ELSD检测器监测麦冬多糖的酸水解产物,优化麦冬多糖的全水解条件,并对麦冬多糖的单糖组成进行分析。结果:麦冬多糖由果糖和葡萄糖组成,其全水解条件为以0.02 mol·L-1TFA为水解试剂,在110℃下水解2 h。HPLC-ELSD方法验证结果表明,该单糖组成测定方法的精密度和重复性良好,果糖和葡萄糖的加样回收率分别为95.9%～104.4%和91.3%～104.1%(RSD<5.9%)。麦冬多糖中果糖和葡萄糖的摩尔比约为15∶1。结论:本研究为麦冬多糖中单糖组成的准确测定提供了方法。
Objective：To develop a method for determination of monosaccharide composition in Ophiopogon japoni- cus polysaccharides（OJP） by high performance liquid chromatography coupled with evaporative light scattering de- tector （ HPLC - ELSD）. Methods： OJP was hydrolyzed by trifluoroacetic acid （TFA） solution, and the acid hydrolysis products were separated by a Waters XBridgeTM Amide column, using acetonitrile - water - triethylamine （75： 25： 0. 2 ） as a mobile phase. ELSD detector was utilized to monitor the acid hydrolysis products of OJP. The full optimized hy- drolysis conditions were investigated and monosaccharide compositions in OJP were finally determined by HPLC - ELSD. Results： The OJP was composed of fructose and glucose, and the full hydrolysis was conducted at 110 ℃ for 2 h with 0.02 mol . L-1 TFA as hydrolysis reagent. The validation results of the HPLC - ELSD method showed that both precision and repeatability of the hydrolysis and determination method for monosaccharide composition were good. The recoveries of fructose and glucose were 95.9% - 104.4% and 91.3% - 104.1% （with RSD less than 5.9% ）, respectively. The molar ratio of fructose and glucose in OJP was about 15： 1. Conclusion：This study pro- vides an accurate method for monosaccharide composition determination in OJP.