从吴茱萸中提取和简易分离柠檬苦素

A simple method for extraction and separation of limonin from Evodiae fructus

提出了一种快速从吴茱萸中分离柠檬苦素的工艺。采用超声辅助提取法提取吴茱萸中的柠檬苦素,并且结合脱脂、酸洗、碱溶酸沉、结晶等分离提纯技术,实现了从吴茱萸中简易分离柠檬苦素的目的;另外利用核磁共振谱和高效液相色谱对所得柠檬苦素的结构和纯度进行了验证和测定。实验结果表明:柠檬苦素的回收率可达84.55%,产品纯度超过98%,与其他提取分离方法相比,具有操作简单易行,分离方法环保经济,产品纯度高的特点。

Firstly,Evodiae fructus was extracted by ethanol with ultrasound-assistance,and the extract was obtained by recovery of ethanol; Secondly,the extract was degreased with petroleum ether and washed with acid solution; Thirdly,that the extract was dissolved in alkaline solution,and p H of the solution was adjusted to 4.0 with HCl solution,then a precipitation was obtained; Fourthly,the precipitation was dissolved in chloroform,and the solution was filtered,and after recovery of chloroform,a residue was obtained; Finally,the residue was washed with ethanol and then crystallized in acetone to obtain limonin.The purity and structure of the as-prepared limonin were confirmed by HPLC and HNMR.The results showed that the recovery of limonin in Evodia rutaecarpa was above 84.55%,and the purity of limonin was above 98 %.Compared with other methods,our separation method was much simpler and has lower cost and higher yield.