延胡索中生物碱成分的研究

Chemical Constituents from Corydalis yanhusuo

目的:建立高速逆流色谱结合半制备高效液相色谱法分离纯化延胡索中生物碱的方法。方法:延胡索生物碱经高速逆流色谱法分离,以石油醚-乙酸乙酯-甲醇-水(2∶3∶3∶2)为溶剂系统,上样量300 mg,得到1个混合物和2个生物碱单体。混合物再以半制备高效液相色谱分离,得到2个生物碱单体,所得产物采用ESI-MS,NMR进行结构鉴定。结果:分离得到4个高纯度的生物碱单体:海罂粟碱(125 mg,1)、四氢巴马亭(40.5 mg,2)、d-紫堇碱(23.5 mg,3)、四氢小檗碱(10 mg,4),其纯度分别为96.5%,97.54%,98.3%,97.3%。结论:HSCCC结合半制备高效液相色谱是一种有效的分离制备延胡索生物碱的方法。

Objective： To develop a method for separation and purification of alkaloids from the crude extract of Corydalis yanhusuo by combination of semi-preparative HPLC and high-speed counter-current chromatography（HSCCC）. Method： First, high speed counter-current chromatography was successfully performed with a two-phase solvent system, petroleum ether-ethyl acetate-Methanol-water（2： 3： 3： 2）.From 300 mg of crude extract, a mixture and two compounds were obtained.And then, the mixture was separated by semi-preparative HPLC. The structures of the target compounds were identified by ESI-MS and NMR. Result： 4 compounds with glaucine （125 mg, 1）, tetrahydropalmatine （40.5 mg, 2）, tetrahydroberberine （23.5 mg, 3） and d-corydaline （10 mg, 4） were obtained with purities of 96.5%, 97.54%, 98.3% and 97.3%, respectively. Conclusion： Combination of HSCCC and semi-preparative HPLC is an efficient method for separation of alkaloids from the crude of C.yanhusuo.