高速逆流色谱分离制备大黄化学成分  

Separation and preparation of the chemical components of Rheum officinale Baill. by pH-zone-refining counter-current chromatography and HSCCC

作　　者：吴秋霞[1,2] 孙常磊[2] 王晓[2] 周洁[2] 郑振佳 杨丙田 孙卫红[1] 

机构地区：[1]江苏大学食品与生物工程学院,江苏镇江212013 [2]山东省分析测试中心,山东济南250014 [3]济南三峰生物工程有限责任公司,山东济南250014

出　　处：《山东科学》2015年第1期1-6,共6页Shandong Science

基　　金：国家药典委员会科研项目;江苏省博士后基金(1102132C);江苏高校优势学科建设工程资助项目

摘　　要：采用pH-区带精制逆流色谱(pH-ZRCCC)与常规高速逆流色谱(HSCCC)结合技术分离制备大黄粗提物中的化学成分。首先采用pH-ZRCCC分离大黄粗提物,溶剂体系为石油醚-乙酸乙酯-甲醇-水(3:7:4:6,V/V),上相加TFA(10 mmol/L)作为固定相,下相加Na OH(15 mmol/L)作为流动相。从1.3 g粗提物中得到140 mg桂皮酸(纯度为96.1%)、130 mg大黄酸(纯度为92.5%)和560 mg尾吹物。称取260 mg该尾吹物采用常规HSCCC的方法进一步分离,溶剂体系为石油醚-乙酸乙酯-甲醇-水(7:3:7:4,V/V),得到约98 mg大黄素(纯度为96.5%)和60 mg芦荟大黄素(纯度为94.6%)。用HPLC检测纯度,用ESI-MS和1HNMR鉴定结构。研究结果表明pH-ZRCCC与HSCCC结合是分离大黄中化合物的一种有效方法。We employed pH-zone-refining counter-current chromatography （pH-ZRCCC）and conventional high-speed counter-current chromatography （HSCCC） to separate and prepare the chemical components in the crude extracts of Rheum officinale Baill. We initially used pH-ZRCCC to separate the crude extracts of Rheum officinale Baill. with petroleum ether-ethyl acetate-methanol-water（3：7：4：6, V/V） as a binary phase solvent system. Trifluoroacetic acid of 10 mmol/L was added to the upper organicstationary phase as a retainer and NaOH of 15 mmol/L was added to the aqueous mobile phase as an eluter. We acquired cinnamic acid （ purity of 96.1% ） of 140 mg, rhein（ purity of 9：2.5% ） of 130 mg and residue of 560 mg from crude extracts of 1.3 g. We further applied conventional HSCCC to the separation of the residue of 260 mg with petroleum ether-ethyl acetate-methanol-water （7：3：7：4, V/V） as a binary phase solvent system, and obtainedaboutemodin （ purity of 96.5% ）of 98 mg and aloeemodin （ purity of 96.5% ） of 60 mg. We employed HPLC to detect the purity and ESI-MS and HNMR to identify those structures. Results show that the combination of pH-ZRCCC and HSCCC is an effective method for the separation of chemical compounds from Rheum officinale Baill.

关 键 词：pH-区带精制逆流色谱 高速逆流色谱 大黄 大黄酸 大黄素 芦荟大黄素 

分 类 号：R284.2[医药卫生—中药学]