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  

Separation and purification of anthraquinones from the tuber roots of Polygonum multiflorum by high-speed countercurrent chromatography

作　　者：俞静静[1] 李瀚元 楼招欢[1] 吕圭源[1] 

机构地区：[1]浙江中医药大学,杭州310053

出　　处：《药物分析杂志》2015年第11期1888-1892,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：国家十二五科技重大专项"重大新药创制"(2011ZX09102-011-07);浙江省中医药科技计划(2012ZA030);浙江省重点实验室(No.2012E10002);浙江中医药大学校级创新团队(2011-3)

摘　　要：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 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, 1 H- NMR, 13 C - NMR and compared with the literature reports. Results： Four anthraquinones （ emodin, physcion-8 - 0 - β - D- glucopyranoside, emodin- 8 - O - β - D - glueopyranoside, eitreorosein ） 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： proved to be a very fast and efficient tool HSCCC with solvent system of chloroform- methanol- water （ 4 ： 3 ： 2 ） was for separation of anthraquinones from P. multiflorum.

关 键 词：高速逆流色谱 何首乌 蒽醌 质谱 氢谱 碳谱 大黄素 大黄素-吡喃葡萄糖苷 大黄素甲醚-吡喃葡萄糖苷 羟基大黄素 

分 类 号：R917[医药卫生—药物分析学]