论文部分内容阅读
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 m L·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 purify and identify the anthraquinones from the crude extracts of Radix Polygoni Multiflori by high-speed countercurrent chromatography (HSCCC). Methods: The solvent system was selected by determining the partition coefficient. The mobile phase consisted of trichloromethane - methanol - water (4: 3: 2) at a flow rate of 2.0 m L · min- · Min-1, the detection wavelength was 254 nm, the anthraquinones were separated from crude extracts of Polygonum multiflorum Thunb., The purity of the compounds was determined by HPLC. The compounds were identified by ESI-MS, 1H-NMR and 13C- structure. Results: The emodin, emodin-8-O-β-D-glucopyranoside, emodin-8-O-β-D-glucopyranoside and hydroxy Emodin, its purity were 96.55%, 96.33%, 21.69%, 71.57%. CONCLUSION: Anthraquinones can be effectively separated from the crude extract of Radix Polygoni multiflori by HSCCC with chloroform-methanol-water (4: 3: 2) as solvent system.