高速逆流色谱制备玫瑰红景天中的三种酚性化合物

Isolation of Phenolic Compounds from Rhodiola rosea by High-speed Counter-current Chromatography

采用高速逆流色谱方法(HSCCC,High-speed Counter-current Chromatography)同时分离三种玫瑰红景天酚性化合物。玫瑰红景天提取物经聚酰胺吸附多酚后经硅胶柱分级得预分离样品,采用正己烷∶乙酸乙酯∶甲醇∶水(4∶5∶4∶5,v/v/v/v)组成的两相溶剂系统对预分离样品进行分离纯化,一次进样150 mg,一次色谱分离得到化合物1:68.5 mg、化合物2:8.5 mg、化合物3:45.5 mg,纯度都超过98%。通过ESI-MS、1H NMR对其结构进行鉴定化合物1为没食子酸(Gallic acid),化合物2为没食子酸甲酯(Methyl gallate),化合物3为山奈酚(Kaempferol)。结果表明利用HSCCC可以成功分离三种酚性化合物,分离效果好,产品纯度高。

A high-speed counter-current chromatography （HSCCC） method was used to separate three phenolic com- pounds from Rhodiola roses. The sample was pre-separated by polyamide column and followed by silica column ehr0ma- tography. Further separation was applied on the pre-separated sample by HSCCC using a solvent system consisting of hexane-ethyl aeetate-methanol-water at a ratio of 4： 5： 4： 5. By one run,68.5 nag of compound 1,8.5 mg of compound 2, and 45.5 mg of compound 3 were obtained from 150 mg of the pre-separated sample. The purities of the three isolated eompounds were all higher than 98%. By ESI-MS andlH NMR analyses, these compounds were identified as gallic acid （1）, methyl gaUate （2） and kaempferol （3）. The results showed that the HSCCC is an effective technique for the sepa- ration of three phenolie eompounds with high purity.