高速逆流色谱法分离制备吴茱萸中的柠檬苦素、吴茱萸碱和吴茱萸次碱

Isolation and Purification of Limonin,Evodiamine and Rutaecarpine from Evodia Rutaecarpa(Juss.) Benth by High-Speed Counter-Current Chromatography

目的:制备柠檬苦素、吴茱萸碱和吴茱萸次碱化学对照品。方法:采用高速逆流色谱法分离纯化吴茱萸二氯甲烷萃取物,溶剂系统为正己烷-乙酸乙酯-甲醇-水(5∶5∶5∶5),上相做固定相,下相做流动相,流速2.0mL.min-1,仪器转速855rpm,进样量400mg,所得样品由高效液相色谱法检测纯度。结果:一次分离可制备6.2mg柠檬苦素、10.4mg吴茱萸碱、10.5mg吴茱萸次碱,其纯度分别为96.2%、98.1%和95.4%。结论:该方法操作简单,可作为柠檬苦素、吴茱萸碱和吴茱萸次碱化学对照品的制备分离方法。

This study aimed to develop a preparative high-speed counter-current chromatography （HSCCC） for the isolation of alkalogenic constituents from Evodia rutaecarpa （ Juss. ） Benth. A two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water （5： 5： 5： 5 ） was used at a flow rate of 2.0mL·min^ - 1, while the apparatus rotated at 855 rpm. And the effluent was detected at 254 nm. The obtained fractions were analyzed by high-performance liquid chromatography （ HPLC）. All 6.2 mg of limonin with the purity of 96.2%, 10.4mg of evodiamine with the purity of 98.1% , and 10.5 mg of rutaecarpine with the purity of 95.4% , were obtained from 400mg of crude extract in a one-step elution within 5h. The results indicated that HSCCC is a powerful technique for the purification of natural products.