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机构地区:[1]河南省天然产物与免疫工程重点实验室,河南大学化学生物学研究所,河南开封475004 [2]河南大学化学化工学院环境与分析科学研究所,河南开封475004 [3]河南省武陟县永盛药材加工厂,河南焦作454981
出 处:《中国实验方剂学杂志》2013年第13期61-65,共5页Chinese Journal of Experimental Traditional Medical Formulae
基 金:“十二五”国家科技支撑项目(2011BAI06B04);中国博士后科学基金面上项目(20110490992);河南省科技厅科技发展计划项目(092102310282)
摘 要:目的:采用1-苯基-3-甲基-5-吡啶酮(PMP)柱前衍生化高效液相色谱法(HPLC)建立了多种单糖的分离模式,应用于怀山药、怀地黄单味药材及其"对药"中多糖的单糖含量测定,并对怀山药、怀地黄单味药材和配伍药对中的单糖组成及其含量进行了比较。方法:以Hypersil ODS2色谱柱(4.6 mm×250 mm,5μm)为色谱柱,以0.05 mol.L-1磷酸盐缓冲液(pH 6.7)-乙腈(83∶17)为流动相,检测波长254 nm,流速1 mL.min-1,柱温30℃。结果:怀山药和怀地黄单味药及其"对药"3种多糖水解后均含有甘露糖、鼠李糖、半乳糖醛酸、葡萄糖、半乳糖和阿拉伯糖,但未检测到岩藻糖。与山药多糖和地黄多糖相比,怀山药和怀地黄"对药"中多糖的单糖组分甘露糖、鼠李糖、半乳糖醛酸和葡萄糖、半乳糖和阿拉伯糖的含量在山药多糖和地黄多糖之间。结论:该方法操作简便快速、结果准确可靠,可用于分析药品及食品中多糖中的单糖组成和含量。Objective: The high performance liquid chromatography(HPLC) method of precolumn derivatization with 1-phenyl-3-methyl-5-pyranozolone(PMP) was developed to efficiently separate several monosaccharides.And the monosaccharide composition and content of polysaccharides in the medicine pair of Dioscorea opposita and Rehmannia glutinosa and their single herb medicine were determined and compared.Method: A Hypersil ODS2 column with the mobile phase of 0.05 mol.L-1 phosphate buffer(pH 6.7) acetonitrile(83∶ 17) at the detection wavelength of 254 nm was used.The flow rate was 1 mL.min-1,the column temperature was kept at 30 ℃.Result: All three polysaccharides contained mannose,rhamnose,glucuronide acid,glucose,galactose and arabinose.However,fucose was not detected.At the same time,it was found that the content of mannose,rhamnose,glucuronide acid,glucose,galactose and arabinose in their medicine pair was between in the single Dioscorea opposita polysaccharides and Rehmannia glutinosa polysaccharides.Conclusion: The developed method is simple,rapid and accurate.Therefore,it is an efficient method to analyze the monosaccharide composition in different kinds of polysaccharides in drug and food.
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