高效液相色谱-蒸发光散射法测定皂荚壳多糖的单糖组分及其含量  

Determination of Composition and Content of Monosaccharide in Polysaccharides of Gleditsia Sinensis Shell by HPLC with ELSD

作　　者：罗立梅[1] 陈朝银[2] 李时琪[1] 张春梅[1] 赵声兰[1] 

机构地区：[1]云南中医学院中药学院,昆明650500 [2]昆明理工大学生命科学学院,昆明650500

出　　处：《理化检验（化学分册）》2013年第3期270-273,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家自然科学基金项目(30760304);云南省自然科学基金项目(2006C0046M)资助

摘　　要：提出了高效液相色谱法测定皂荚壳多糖的单糖组分及其含量的方法。皂荚壳样品经乙醇-水(95+5)溶液提取,滤液经分级沉淀除去蛋白质,过中空纤维膜净化。以ZORBAX Carbohy-drate色谱柱(4.6mm×250mm,5μm)分离,以不同体积比的乙腈和水为流动相进行梯度洗脱,用蒸发光散射检测器检测。鼠李糖、核糖、木糖、阿拉伯糖、果糖、甘露糖、葡萄糖、山梨醇和半乳糖等9种单糖的质量浓度分别在一定的范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.010～0.048g.L-1之间。采用标准加入法做回收试验,平均回收率在99.3%～101%之间,测定值的相对标准偏差(n=8)均小于0.2%。HPLC was applied to the determinations of composition and content of monosaccharide in polysaccharides of Gleditsia sinensis shell.The sample was extracted with ethanol-water（95＋5） solution and the filtrate was fraction-ally precipitated to remove protein,and the polysaccharides obtained were purified by passing through hollow-fiber film.Nine monosaccharides were separated on ZORBAX Carbohydrate column（4.6 mm× 250 mm,5 μm） by gradient elution with mixtures of acetonitrile and water in different ratio,and their contents were determined by evaporation light scattering detector（ELSD）.Linear relationships between values of peak area and mass concentration of the 9 monosaccharides were kept in the definite ranges,with detection limits（3S/N） in the range of 0.010-0.048 g·L-1.The values of average recovery found by standard addition method were in the range of 99.3%-101%,with values of RSD′s（n=8） less than 0.2%.

关 键 词：高效液相色谱法 蒸发光散射检测 皂荚壳多糖 单糖 

分 类 号：O657.7[理学—分析化学]