高速逆流色谱法分离何首乌粗提物中蒽醌类化合物及组分结构鉴定

目的:利用高速逆流色谱法(HSCCC法)对何首乌粗提物中蒽醌类成分进行分离纯化并进行结构鉴定研究。方法:通过测定分配系数,选择分离的溶剂体系;以三氯甲烷-甲醇-水(4:3:2)为溶剂系统,流动相的流速为2.0 mL·min^-1,主机转速为900 r·min^-1,检测波长254 nm,对何首乌粗提物中蒽醌类化合物进行分离;利用HPLC法测定化合物的纯度;利用ESI-MS、¹H-NMR和¹³C-NMR及参照文献报道确定化合物的结构。结果:从何首乌粗提物中分离鉴定得到了大黄素、大黄素-8-O-β-D-吡喃葡萄糖苷、大黄素甲醚-8-O-β-D-吡喃葡萄糖苷和羟基大黄素,其纯度分别为96.55%、96.33%、21.69%、71.57%。结论:应用HSCCC法,以三氯甲烷-甲醇-水(4:3:2)为溶剂系统,可以有效地从何首乌粗提物中分离出蒽醌类化合物。

Objective:To separate and purify anthraquinones from extract of the tuber roots of Polygonum multiflorum by high-speed countercurrent chromatography(HSCCC)and identify the structure of separated compounds.Methods:The solvent system for separation was selected by determining the distribution coefficient,and the solvent system was composed of chloroform-methanol-water(4:3:2),the flow rate was 2.0 mL·min^-1,the rotational speed was 900 r·min^-1,and the detection wavelength was set at 254 nm.Anthraquinones from the tuber roots of P.multiflorum were separated,their purity was assessed by HPLC;the structures of these compounds were identified by ESI-MS,¹H-NMR,¹³C-NMR and compared with the literature reports.Results:Four anthraquinones(emodin,physcion-8-O-β-D-glucopyranoside,emodin-8-O-β-D-glucopyranoside,citreorosein)were separated from crude extract of the tuber roots of P.multiflorum.The purity of obtained anthraquinones was 96.55%,96.33%,21.69%,71.57% respectively.Conclusion:HSCCC with solvent system of chloroform-methanol-water(4:3:2)was proved to be a very fast and efficient tool for separation of anthraquinones from P.multiflorum.