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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nifdc.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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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

分类号:
出版年·卷·期(页码):2015,35 (11):0-0
DOI: 10.16155/j.0254-1793.2017.01.01
-----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 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。

-----英文摘要:---------------------------------------------------------------------------------------

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.

-----参考文献:---------------------------------------------------------------------------------------

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