大孔树脂-高速逆流色谱法分离纯化地黄中毛蕊花糖苷（英文）

Separation and purification of acteoside from Rehmannia glutinosa by combining macroporous resin with high-speed countercurrent chromatography

该文建立了大孔树脂-高速逆流色谱分离中药材地黄中有效成分毛蕊花糖苷的方法。考察了4种大孔树脂对地黄粗提物中毛蕊花糖苷的静态吸附与解吸情况,其中D101大孔树脂对目标成分的吸附率与解吸率最理想,实验结果表明体积分数为10%的乙醇洗脱得到的毛蕊花糖苷含量最高,目标成分含量从4.9%提高到32.6%。最后,部分纯化的样品(165 mg)采用高速逆流色谱进一步纯化,两相溶剂系统由乙酸乙酯-正丁醇-水(1∶4∶5,v/v/v)组成,分离得到45 mg纯度为96%的毛蕊花糖苷。

Acteoside,a chemical component of the traditional Chinese medicinal herb Rehmannia glutinosa,was separated from the plant by a combination of macroporous resin column chromatography and high-speed countercurrent chromatography. The static adsorption and desorption of acteoside in the crude extract were investigated using four kinds of macroporous resin,among which the D101 macroporous resin presented the best adsorption and desorption rates toward the compound. The crude extract was then gradient-eluted with increasing volume percentages of ethanol,where it was found that the highest content of acteoside was obtained when using 10%(v/v)ethanol eluent,in which the purity of acteoside was increased from 4. 9% to 32. 6%.Then,the partially purified crude extract(165 mg)was further purified by high-speed countercurrent chromatography using a two-phase solvent system consisting of ethyl acetate-n-butanol-water(1 ∶4 ∶5,v/v/v),yielding45 mg of acteoside with 96% purity.