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作 者:张萍[1] 陈燕[1] 刘建波[1] 尚永辉[1] 刘静[1] ZHANG Ping;CHEN Yan;LIU Jian-bo;SHANG Yong-hui;LIU Jing(College of Chemistry and Chemical Engineering,Xianyang Normal University,Xianyang 712000)
机构地区:[1]咸阳师范学院化学与化工学院
出 处:《分析科学学报》2019年第5期572-576,共5页Journal of Analytical Science
基 金:国家自然科学基金(No.21305117);陕西省自然科学基础研究计划(No.2017JQ2043,2018JM2044);陕西省教育厅专项研究基金(No.17JK0829)
摘 要:建立了3-氨基-9-乙基咔唑(AEC)柱前衍生-高效液相色谱(HPLC)法分析香菇多糖的单糖组成。香菇多糖水解成单糖后用AEC衍生化,采用Ultimate LP-C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.05 mol·L-1NH4Ac溶液(pH=7.0)为流动相,梯度洗脱,分离6种单糖-AEC衍生物,在254 nm下检测。结果表明,AEC对中性单糖的衍生效果比酸性单糖好,衍生物稳定性高;方法的线性范围宽,重复性好;测得香菇多糖的单糖组成有:甘露糖(Man)、鼠李糖(Rha)、葡萄糖(Glc)、半乳糖(Gal)、阿拉伯糖(Ara)和木糖(Xyl),其摩尔比为:4.69(Man)∶1.23(Ara)∶1.00(Gal)∶0.48(Glc)∶0.17(Rha)∶0.14(Xyl),和文献报道吻合。该方法准确灵敏,可用于香菇多糖单糖组成分析。A method for the analysis of monosaccharide composition of letinous edodes polysaccharide by 3-amino-9-ethylcarbazole(AEC) precolumn derivatization was established.After the polysaccharide from letinous edodes was hydrolyzed to the monosaccharides by 2 mol·L-1 trifluoracetic acid,it was derivatized with AEC.Using acetonitrile and 0.05 mol·L-1 NH4Ac(pH=7.0) as mobile phase, six monosaccharide-AEC derivatives were separated on Ultimate LP-C18(250 mm×4.6 mm,5 μm) column by gradient elution and detected at 254 nm.The results showed that the better derivatization effect on neutral monosaccharide with high stability for the AEC derivatives than acid monosaccharide was obtained.The wide linear range and the good repeatability for the established method were verified.6 kinds of monosaccharides such as mannose(Man),rhamnose(Rha),glucose(Glc),galactose(Gal) and arabinose(Ara),were discovered in the polysaccharide from letinous edodes by this method and their molar ratios were 4.69(Man):1.23(Ara):1.00(Gal):0.48(Glc):0.17(Rha):0.14(Xyl),which was in agreement with the reported results in literature.The method is accurate,sensitive and simple,and can be used as a routine method for the analysis of monosaccharide of the polysaccharides from letinous edodes.
关 键 词:香菇多糖 3-氨基-9-乙基咔唑 高效液相色谱
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