摘要
以夹竹桃科植物止泻木子的干燥种子为原材料,采用乙醇提取法对其生物碱类物质进行粗提取,通过硅胶柱层析和重结晶技术对生物碱粗提物进行分离和纯化。利用核磁共振波谱和质谱法对其一种生物碱单体进行化学结构和分子量鉴定。实验结果表明,用70%乙醇在60℃条件下静止浸取3次,每次提取6h,得到止泻木子总生物碱提取物,其得率达到0.244%。经过硅胶柱分离和重结晶纯化,可获得3种生物碱单体。对HPLC检测纯度达到94.89%的2号生物碱单体进行核磁共振波谱和质谱检测,得知该生物碱单体是一个分子量为356.59的锥丝碱(conessine)。该结果有利于了解以止泻木子为主要成分的蒙药药剂作用机理。
In this paper, one of the agent of alkaloid was extracted from the dry seeds of Holarrhena antidysenterica Wall.ex A.DC by ethanol, purified by silica gel chromatography and recrystallization.The structures of it was established on the basis of NMR techniques and mass spectrometry.The results showed that the optimum conditions of extraction were as follows:the Holarrhena antidysenterica Wall.ex A.DC was extracted under 60℃ for 6 h by 70% ethanol,and the getting rate of total alkaloid reached to 0.244%.By silica gel chromatography and recrystallization,the purity of one sample of compound 2 reached to 94.89%.The compound 2 was obtained as white crystal and its molecular formula C24 H40 N2 was established by mass spectrometry (m/z 356.59 [M+ H]+ ).From the NMR data,the structure of compound 2 was deduced as conessine and its 1 3 C NMR data were consistent with those of literature.
出处
《化工学报》
EI
CAS
CSCD
北大核心
2016年第S2期191-196,共6页
CIESC Journal
基金
内蒙古自治区科技重大专项项目(222089)~~
关键词
止泻木子
核磁共振
硅胶柱分离
锥丝碱
萃取
药物
Holarrhena antidysenterica Wall.ex A.DC
NMR
silica gel columnchromatography
conessine
extraction
pharmaceuticals
