高速逆流色谱法分离制备波棱瓜子中波棱芴酮  

Separation of Herpetfluorenone from the Seeds of Herpetospermum Caudigerum Waill.by High-Speed Counter-Current Chromatography

作　　者：巩法强[1,2] 杨丽[1] 周洪雷[1] 王岱杰[2] 方磊[2] 王晓[2] 

机构地区：[1]山东中医药大学,山东济南250355 [2]山东省分析测试中心,山东济南250014

出　　处：《辽宁中医杂志》2012年第5期897-899,共3页Liaoning Journal of Traditional Chinese Medicine

基　　金：山东省中青年科学家科研奖励基金(BS2009SW047);山东省科技发展计划项目(20100816632)

摘　　要：目的:建立了常规柱色谱结合高速逆流色谱法(HSCCC)分离纯化波棱瓜子中波棱芴酮的方法。方法:首先采用聚酰胺和硅胶柱色谱富集波棱芴酮,再用HSCCC进行分离制备,HSCCC最佳溶剂体系为石油醚-乙酸乙酯-甲醇-水(4∶9∶6∶8,V/V),上相为固定相,下相为流动相,从200mg富集物中一次分离得到80mg纯度为98.3%的波棱芴酮,所得产物经ESI-MS和NMR鉴定结构。结论:本方法所得产物纯度高,重现性好,适合于波棱芴酮的制备型分离。Objective ： A method was established for the separation and purification of herpettluorenone from the seeds of Her-petospermum caudigerum Waill. using conventional column chromatography and high-speed counter-current chromatography. Methods ： The herpetfluorenone was first enriched with polyamide and silica gel. HSCCC was used for the further separation with a two- phase solvent system composed of petroleum-ethyl acetate-methanol-water（4： 9： 6：8 ,V/V）. The upper organic phase was used as stationary phase, while the lower aqueous phase as mobile. The separation yielded a total of 80mg of herpetfluorenone from 200mg of enriched extract in one step separation with the purity of 98.3% , respectively, as determined by HPLC. The chemical structure of herpetfluorenone was identified by EI-MS and NMR. Conclusion ： This method fits the preparative separation of herpet-fluorenone for the high-purity and reproductive.

关 键 词：高速逆流色谱 波棱瓜子 波棱芴酮 

分 类 号：R284[医药卫生—中药学]