水解原位萃取分离刺五加异秦皮啶

目的对刺五加80%体积分数乙醇提取物采用水解原位萃取的方法将结合态异秦皮啶转化成游离态异秦皮啶。方法确定的工艺条件为每克80%体积分数乙醇浸膏按固液比1∶100加入0.6 mol.L^-1盐酸,加入同体积的1,2-二氯乙烷,搅拌下85℃回流水解2.5 h。结果在此条件下,刺五加根皮、茎皮和根茎混合异秦皮啶分别由原来的0.042 4、0.011 2和0.005 3 mg.mL^-1增加到1.264 1、0.441 2和0.260 0 mg.mL^-1,分别增加28.81、38.39和48.06倍;根木质部和茎木质部由水解前检测不到异秦皮啶增加到0.023 3和0.009 7 mg.mL^-1。结论将水解原位萃取法分离异秦皮啶工艺与目前常用的传统酸水解-有机溶剂萃取工艺进行了对比,水解温度由原来的100℃降低到85℃,处理时间由原来的14.5 h降低到2.5 h,溶剂使用量仅为原来的3/4。

Isolated Isofraxidin from Acanthopanax Senticosu Extract by Extraction in Combination Hydrolysis in Situ

OBJECTIVE The method of simultaneous hydrolysis and extraction in situ was applied to process 80% of the volume fraction of ethanol extract of Acanthopanax senticosus,in order to convert the bound isofraxidin into free isofraxidin.METHODS The optimum conditions were confirmed as follows： the hydrochloric acid concentration of 0.6 mol.L^-1,the ratio of solid to liquid was 1∶100 by adding hydrochloric acid,the same volume of 1,2-dichloroethane for extraction,reflux temperature 85 ℃,hydrolysis time 2.5 h.RESULTS Under these conditions,the isofraxidin content in the root bark,stem bark and root-stem mixture product had increased from 0.042 4,0.011 2 and 0.005 3 mg.mL^-1 to 1.264 1,0.441 2 and 0.260 0 mg.mL^-1,which were 28.81-fold,38.39-fold and 48.06-fold of those in the untreated extracts,respectively;the isofraxidin content in the root xylem and stem xylem were 0.023 3 and 0.009 7 mg.mL^-1,which can’t detect the concentration without treatment.CONLUTSION Using the process of simultaneous extraction and hydrolysis for separation of isofraxidin,hydrolysis temperature decreased from 100 ℃ to 85 ℃,hydrolysis time shortened from 14.5 h to 2.5 h and the solvent amount was only the three-quarter of traditional method,comparing with the traditional acid hydrolysis and then extract with organic solvents method.