杜仲叶提取绿原酸的中间试验研究

STUDY ON TECHNIQUE UPON ISOLATION AND PURIFICATION OF CHLOROGENIC ACID FROM LEAVES OF EUCOMMIA

本研究在以前研究的基础上进行中间试验,利用以下工艺流程从杜仲叶中制得绿原酸纯品:40%乙醇提取(80℃,2h,1∶16料液比,提取2次)→制备浸膏(真空浓缩,80℃鼓风干燥)→加水转溶(4次)→铅盐沉淀(每100g杜仲叶用140g乙酸铅)→解析绿原酸(20%H2SO4)→乙酸乙酯萃取(约20次)→浓缩析出粗品→重结晶得纯品,平均得率0.53%,纯度98.35%。研究中还发现杜仲叶中不含异绿原酸。

Based on the previous study,chlorogenic acid was isolated and purified from leaves of Eucommia ulmoides Oliver in an pilotscale experiment by the following process:refluxing by 40% ethanol(80 ℃,2 h,ratio of material to solvent:1∶16,extract twice)→extracts preparation(vaccum evaperation,drying at 80 ℃)→extraction by water(4 times)→precipitation by Pb(OAc)2\→resolution of chlorogenic acid by 20% sulfuric acid→extraction by ethyl acetate(20 times)→condensation→recrystallization.The yield of chlorogenic acid is 0.53%,at purity 98.35%.Results of the experiment showed that this technological process was feasible and practical.It was found that no isomers of chlorogenic acid occurs in the leaves of E.ulmoides after comparing with honeysuckle flowers and raw coffee beans,in which the occurrence of isochlorogenic acids was reported.This is traceable to the views of secondary metabolism and chemical reaction.