钩吻生物碱的提取分离及结构鉴定

中草药钩吻中具有抗癌活性生物碱单体成分的提取分离,并测定其结构。方法：药材粉碎后用3%NaOH碱化后,晾干,用氯仿浸泡,回收氯仿提取液得浸膏。加酸溶解后,用氯仿萃取,碱化水层,再用氯仿萃取,得到钩吻总生物碱。然后经硅胶柱层析、反相ODS柱层析以及制备型HPLC层析分离纯化,并经理化性质和光谱学数据的测定鉴定单体化合物的结构。结果：共分离得到12个单体化合物,经测定紫外光谱、1H-NMR数据并与文献报道相比较,初步确定两个化合物的结构分别为gelsemine和koumine。结论：通过硅胶柱层析、ODS柱层析和HPLC相结合的方法可以达到分离钩吻总生物碱的目的。

Extraction,Isolation and Identification of Alkaloids of Gelsegium Elegans Benth

Objective： To extract, isolate and identify the alkaloids of Gelsemium elegans Benth. Methods： The plant was alkalified with 3% NaOH, dried at room temperature, then was extracted with CHCl3. The chloroform extracts were dissolved in the acid water, partitioned with CHCl3, then the water layer was alkalified with saturate NaOH, extracted with CHCl3 again to obtain the alkaloids of Gelsemium elegans. The alkaloids were further subjected on the silica-gel column, ODS column, and pre-HPLC chromatography. The physical-chemical data and 1H-NMR of the components were determined. Results： 26 fractions were obtained by the silica-gel column chromatography, and 12 compounds were obtained by pre-HPLC. Two needle-shaped crystal chemical constituents were confirmed to be gelsemine and koumine. Conclusion： The alkaloids of Gelsemium elegans can be isolated and purified by use of the methods of silica gel, ODS and HPLC chromatography.