高速逆流色谱法分离制备中药诃子中的没食子酸  

Isolation and preparation of gallic acid from Terminalia chebula Retz. with high speed counter-current chromatography

作　　者：李忠琴[1] 李秋云[1] 江兴龙[1] 张坤[1] 关瑞章[1] 

机构地区：[1]集美大学水产学院鳗鲡现代产业技术教育部工程研究中心,福建厦门361021

出　　处：《色谱》2014年第12期1404-1408,共5页Chinese Journal of Chromatography

基　　金：国家海洋局海洋经济创新发展区域示范专项(2012FJ03);厦门市重点项目(3502Z20110014,3502Z20123027);鳗鲡现代产业技术教育部工程研究中心开放基金项目(RE201305);国家级大学生创新创业训练计划项目(Z81231)

摘　　要：利用高速逆流色谱法从100 mg诃子醇提物中一次性分离制备得到8.6 mg没食子酸。通过分析型高速逆流色谱对5种溶剂系统进行筛选,确定以正己烷-乙酸乙酯-甲醇-水(体积比为1∶5∶1∶5)为两相溶剂体系并放大到制备型上,以上相为固定相,下相为流动相,在主机转速850 r/min、流动相流速2 mL/min、检测波长254 nm的条件下进行分离制备,获得4个分离峰(组分Ⅰ、Ⅱ、Ⅲ、Ⅳ)。经高效液相色谱检测,按照面积归一法计算,其中组分Ⅲ的纯度达96.40%。经电喷雾电离质谱分析,并结合与没食子酸标准品的高效液相色谱测定结果的对比,确定组分Ⅲ为没食子酸。该方法简便、快速、重复性好,适合于诃子中没食子酸的分离制备。A separation method based on high speed counter current chromatography（HSCCC）has been established for the isolation and preparation of gallic acid from the ethanol extract of Terminalia chebula Retz. After comparing five kinds of solvent protocols of HSCCC,the two phase system of n hexane ethyl acetate methanol water（1∶ 5∶ 1∶ 5,v / v / v / v）was final ly chosen as the operating solvent of HSCCC for the separation of gallic acid,in which the low er phase was used as the mobile phase and the upper phase as stationary phase. The detection in the experiments was performed with an ultraviolet detector at 254 nm. Under the conditions of rotation speed of 850 r / min,lower phase flow rate of 2 mL / min,four peaks（Ⅰ / Ⅱ / Ⅲ / Ⅳ）were displayed on HSCCC chromatogram. Among them,only peak Ⅲ contained a large amount of gallic acid（about 96. 40%）,which was confirmed by electrospray ionization mass spectrom etry（ESI MS）and high performance liquid chromatographic（HPLC）analysis. As much as 8. 6mg of gallic acid was obtained from 100 mg of the ethanol extract of Terminalia chebula Retz.,indicating the method is simple,robust and efficient for the preparation of gallic acid.

关 键 词：高速逆流色谱 没食子酸 诃子 

分 类 号：O658[理学—分析化学]