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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2013年第1期50-56,共7页
Chinese Journal of Pharmaceutical Analysis
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
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
Ophiopogon japonicus polysaccharides
high performance liquid chromatography -evaporative light scat-tering detector
full hydrolysis
method validation
monosaccharide composition analysis
fructose determination
