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

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.