高速逆流色谱法同时分离制备头花蓼中没食子酸和原儿茶酸  

Preparing Gallic Acid and Protocatechuic Acid in One Step from Polygonum capitatum Buch-Ham ex D.Don by High-speed Counter-current Chromatography

作　　者：方炜[1] 万金志[1] 张丽艳[2] 梁斌 陈欣霞[1] 

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

出　　处：《天然产物研究与开发》2011年第2期299-303,共5页Natural Product Research and Development

基　　金：贵州省科技厅2008年度重大专项计划项目--<贵州苗药头花蓼深度研究开发与产业化>黔科合重大专项字(20080620)

摘　　要：对蓼科蓼属头状蓼组植物头花蓼进行化学成分的研究。本研究建立了HPLC测定中药头花蓼水提喷雾干燥粉末中化学成分含量的方法,然后应用高速逆流色谱法对头花蓼水提喷雾干燥粉末的乙酸乙酯粗提物的化学成分进行了半制备性分离研究,通过对分离方法和溶剂系统的筛选,寻找到最佳的溶剂系统(正己烷∶乙酸乙酯∶甲醇∶水=1∶5∶1∶5),上相为固定相,转速840 r/min,流速2.0 mL/min,进样量756 mg,检测波长272 nm。结果显示,在该条件下经一步分离可同时得到质量为148.5 mg和9.2 mg的两种产物,纯度为99.8%和97.4%,经紫外、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原儿茶酸。A HPLC method was established for the determination of chemical components from Polygonum capitatum Buch-Han ex D.Don.And high-speed counter-current chromatography was successfully applied to isolate and purify phenolic constituents from the crude extract of Polygonum capitatum.The solvent system used was hexane-ethyl acetate-methanol-water（1∶5∶1∶5,v/v/v/v）,the rotate speed was 840 r/min,the flow rate was 2 mL/min,and the effluent was detected at 272 nm.148.5 mg of gallic acid and 9.2 mg of protocatechuic acid were separated from 756.0 mg extract with the purities of 99.8% and 97.4%,respectively.The structures of the compounds were identified by UV,IR,LC/MS,1H and 13C NMR.

关 键 词：头花蓼 高效液相 高速逆流色谱 没食子酸 原儿茶酸 

分 类 号：R284.2[医药卫生—中药学] Q946.91[医药卫生—中医学]