高速逆流色谱同时分离头花蓼中的没食子酸和短叶苏木酚酸  

Simultaneous isolation and purification of gallic acid and brevifolincarboxylicacid from Polygonum capitatum by high-speed counter-current chromatography

作　　者：陈欣霞[1] 张丽艳[2] 万金志[1] 梁斌 谢宇 

机构地区：[1]中山大学药学院药物分析实验室,广东广州510006 [2]贵阳中医学院,贵州贵阳550002 [3]贵州威门药业股分有限公司,贵州贵阳550018

出　　处：《中国中药杂志》2010年第15期1957-1960,共4页China Journal of Chinese Materia Medica

基　　金：贵州省科技厅2008年度重大专项计划项目(20080620)黔科合重大专项字

摘　　要：目的:应用高速逆流色谱法从头花蓼中同时分离没食子酸和短叶苏木酚酸。方法:对头花蓼水提粉末的正丁醇粗提物进行高速逆流色谱分离纯化,以乙酸乙酯-正丁醇-0.44%醋酸水(3∶1∶5)为溶剂系统,上相为固定相,主机转速860r.min-1,流速2.0mL·min-1,检测波长272nm,进样量1.07g。结果:在该条件下经一步分离可得到纯度为99.7%,97.5%的2种产物,经高效液相色谱、红外、质谱及核磁共振等方法进行结构分析,确定分别为没食子酸和短叶苏木酚酸,其中短叶苏木酚酸为首次在该属植物中分离得到。结论:该法简便、快速,具有较好的实际应用价值,适合于头花蓼中有效成分的研究和单体的提取制备。Objective：To isolate and purify gallic acid and brevifolincarboxylic acid simultaneously by high-speed counter-current chromatography（HSCCC）from a crude extract of Polygonum capitatum.Method：The biphasic solvent system composed of ethyl acetate-n-butanol-0.44% acetic acid（3∶1∶5）was used at a flow rate of 2.0 mL·min^-1,while the aqueous phase was selected as the mobile phase and the apparatus was rotated at 860 r·min^-1.The effluent was detected at 272 nm.Result：51.5 mg of gallic acid and 5.9 mg of brevifolincarboxylic acid were separated from 1.07 g of the crude extract with the purities of 99.7% and 97.5%,respectively,while brevifolincarboxylic acid was obtained firstly from the genus Polygonum.The structures of the compounds were identified by ultraviolet spectrometry（UV）,infra-red spectrometry（IR）,liquid chromatography/mass spectrometry（LC/MS）,time-of-flight mass spectrometry（TOF-MS）,1H-nuclear magnetic resonance（NMR）and 13C-NMR.Conclusion：This method is feasible and rapid for isolation and purification of gallice acid and brevifolincarboxylil acid.

关 键 词：高速逆流色谱 头花蓼 没食子酸 短叶苏木酚酸 

分 类 号：R284.1[医药卫生—中药学]