大黄提取物中5种蒽醌化合物的分离纯化

为研究大孔树脂对大黄5种蒽醌的分离效果,本文采用静态吸附实验,比较6种大孔树脂(HPD-100、XDA-6、AB-8、LX-38、ADS-7和ADS-17)对5种游离蒽醌(芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚)的吸附及解吸附性能,筛选出对大黄5种蒽醌吸附率和吸附率最高的大孔树脂。然后以筛选的大孔树脂作为载体,对其动态吸附特性进行了初步研究。结果显示,HPD-100大孔树脂对大黄5种蒽醌吸附率和吸附率最高;在层析柱径高比1:8,上样溶液5种蒽醌总浓度为3.64 mg/mL,上样体积2.0 BV,流速1.0 BV/h,85%的乙醇洗脱,洗脱体积为3.0 BV的优化条件下,HPD-100对5种蒽醌的动态吸附率为86.3%,洗脱率为85.9%,5种蒽醌总含量增加了2.88倍,由原来的7.13％增加到20.5％,总回收率98.7%,提取物中残留的离子液体[bmim]Br也同时被除去,表明本实验选择的优化条件具有可行性。

Separation and Purification of Five Anthraquinones from Crude Extracts of Rhubarb

The effect of separation of five anthraquinones in rhubarb by macroporous resin was investigated through static adsorption experiment in this paper. The sorption and desorption properties of five anthraquinones(aloe-emodin,rhein,emodin,chrysophanol,physcion)on macroporous resins including HPD-100,XDA-6,AB-8,LX-38,ADS-7 and ADS-17 had been compared. Then,Dynamic adsorption and desorption were performed on the chosen macroporous resin packed in glass columns to optimize the separation process.Results showed that,HPD-100 resin offered much higher adsorption and desorption ratios for five anthraquinones than other resins;under the optimised conditions:the ratio of column height to diameter bed 1∶8,loading concentration 3.64 mg/mL,loading volume 2.0 BV,flow rate 1.0 BV/h,85% ethanol as eluent,and elution volume 3 BV,the dynamic adsorption and desoption rate of five anthraquinones on HPD-100 were 86.3% and 85.9%,respectively. The content of five anthraquinones in the final product increased 2.88-times from 7.13% to 20.5%,with a recovery of 98.7%,ionic liquids[bmim]Br could be removed from crude extract,which showed that the optimized conditions were feasible.