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糖肟三甲基硅醚化衍生法分析中药多糖单糖组成研究

Analysis of Monosaccharide Composition of Polysaccharide in Chinese Herbs by Sugar Oxime Trimethylsilylation Derivatization
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摘要 目的:建立糖肟三甲基硅醚化衍生法分析中药多糖单糖组成。方法:样品经糖肟三甲基硅醚化衍生,采用气相色谱法测定麻黄根多糖的单糖组成。色谱柱:DB-5毛细管柱(60 m×0.25 mm×0.25μm),载气:He,进样量:1μL,分流比20∶1,柱流速1.2 mL/min,程序升温,柱温150℃,以3℃/min至230℃,以20℃/min至300℃。质谱条件:EI(70 eV),离子源温度230℃,接口温度250℃,扫描范围:m/z 50~550,扫描率:2.5 scan/s。结果:9种单糖标准品均得到很好的分离。麻黄根纯化多糖Ⅱ中主要含阿拉伯糖、半乳糖和鼠李糖,其摩尔比为16.96∶5.03∶1.01,还有痕量的葡萄糖、岩藻糖和甘露糖。结论:该方法可以准确测定中药多糖中单糖的种类和比例,并成功用于检测麻黄根纯化多糖中的单糖组分。 Objective:To determine monosaccarides composition of polysaccaride in Chinese herbs with oxime trimethy silylation.Methods:The samples were derived from oxime trimethy silylation,and monosaccharide composition in Ephedra root was determinated by gas chromatography.DB-5capillary column(60m×0.25mm×0.25μm)was applied,nitrogen was served as carrier gas,sample volume was1uL,split ratio was20∶1,column flow rate was1.2ml/min,column temperature was150℃;the temperature rose to230℃at the speed of3℃/min;then to300℃at20℃/min;250℃inlet temperature,20∶1split ratio,flow rate was1.2mL/min.MS condition:EI(70eV),ion source temperature was230℃,interface temperature was250℃;scanning range was50~550m/z,with scanning rate of2.5scan/s.Results:9kinds of monosaccharides got a good separation.Polysaccharide of Ephedra root mainly contained arabinose,galactose and rhamnose,the mole proportion of them was16.96∶5.03∶1.01,there was also a small amount of glucose,fucose and mannose.Conclusion:This method can obtain a single peak,which can be used for determination of monosaccharides composition in polysaccharide of Chinese herbs,and it has been successfully tested in Ephedra root.
作者 夏永刚 孙慧敏 王天龙 梁军 杨炳友 匡海学 XIA Yong-gang;SUN Hui-min;WANG Tian-long;LIANG Jun;YANG Bing-you;KUANG Hai-xue(Key Laboratory of Chinese Materia Medica, Ministry of Education, Heilongjiang Key Laboratory of Traditional Chinese Medicine and Natural Medicine Pharmacodynamic Material Bases, Heilongjiang University of Chinese Medicine, Harbin 150040, China)
出处 《中医药学报》 CAS 2017年第6期17-20,共4页 Acta Chinese Medicine and Pharmacology
基金 全国百篇优秀博士学位论文作者专项资金项目(201367) 中国博士后第61批科学基金面上项目(2017M611409) 哈尔滨市科技创新人才研究专项资金项目(2017RAXXJ059)
关键词 糖肟三甲基硅醚化衍生法 麻黄根多糖 GC-MS 单糖组成 Oxime trimethy silylation Polysaccharide of Ephedra root GC-MS Monosaccharide composition
作者简介 夏永刚(1980-),男,博士,教授,主要研究方向:中药及复方药效物质基础研究。;通讯作者:匡海学(1955-),男,博士,教授,博士研究生导师,主要研究方向:中药及复方药效物质基础研究,中药性味理论研究。
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