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目的研究制备型高效液相分离纯化巫山淫羊藿中淫羊藿属苷A和朝藿定C的条件。方法巫山淫羊藿粗提物经大孔吸附树脂和硅胶柱色谱得朝藿定C与淫羊藿属苷A的混合物,进行HPLC制备色谱分离,以乙腈-水(24∶76)为流动相,收集相应流分浓缩至干,甲醇溶解,滤过,滤液蒸干即得。结果该法所得产品极易结晶,用面积归一化法定量,质量分数大于98.0%,经紫外、红外、核磁共振确定结构,与文献数据基本一致。结论本法简便快捷,可获得高纯度的淫羊藿属苷A和朝藿定C,解决在常规柱色谱法制备朝藿定C对照品中存在的不易结晶和纯度不够的问题,产品可用作分析用对照品。
OBJECTIVE To study the preparation and purification of Epimedium glycoside A and epimedin C in Wushan epimedium by preparative high performance liquid chromatography. Methods The crude extract of Epimedium wuenshanense was purified by macroporous adsorption resin and column chromatography on silica gel column. The mixture of Epimedin C and Epimedrin A was separated by HPLC. The mobile phase was acetonitrile - water (24:76) , Collect the corresponding fractions concentrated to dry, dissolved in methanol, filtered, the filtrate evaporated to dryness. Results The product obtained by this method was easy to crystallize and was quantified by the area normalization method. The mass fraction was more than 98.0%. The structure was confirmed by UV, IR and NMR and was consistent with the literature data. Conclusion This method is simple and rapid, and high purity Epimedium glycoside A and epimedin C can be obtained. This method solves the problems of not easy to crystallize and insufficient purity in the epimedin C preparation prepared by conventional column chromatography. The product is available For analysis of reference substance.