摘要
在对苦豆子的酸水浸提液进行了超滤和脱色预分离的基础上，采用不同的有机溶剂萃取和硅胶柱层析对其中主要的生物碱进行分离纯化及条件优化。结果表明合适的生物碱萃取富集条件是用氯仿为溶剂，pH=10．5。该氯仿萃取液用硅胶柱层析分离，洗脱剂为氯仿．甲醇．氨水（5：0．4：0．01，V/V/V），洗脱速度1柱床体积·h^-1，得到峰1～峰3。峰1和峰2中的化合物经丙酮结晶和重结晶分别得到纯度99％以上的氧化槐果碱和氧化苦参碱；峰3对应的组分再经硅胶柱层析，洗脱剂为丙酮．甲醇（10：1，V／V），洗脱速度1柱床体积·h^-1，得到峰4～峰6，峰4中的化合物经石油醚结晶和重结晶，可以得到纯度95．8％的槐定碱。采用了HPLC-MS，IR，熔点测定和薄层色谱等方法进行上述生物碱单体的定性定量及分子结构确定。本研究为深度开发苦豆子生物碱资源和为制备医药工业所需的高纯度生物碱原料提供了依据。
After ultrafiltration and decoloration of the acidic water extract of Sophora alopecuroides L. seeds, the monomer alkaloids in it were further extracted by using different solvents and the suitable isolation conditions were searched. Chloroform with pH of 10,5 was found to be the most suitable solvent, and the chloroform extract was then loaded on a silica gel column using chloroform-methanol-ammonia water （5 ： 0.4 ： 0.01, V/V/V） as mobile phase with flow rate of 1 bed volume per hour. During which three peaks were obtained, compounds corresponding to peak 1 and peak 2 were crystallized and recrystallized in acetone and correspondingly crystal A （oxymatrine） and crystal B （oxysophocarpine） were gained with purities over 99%, respectively. Compounds corresponding to peak 3 were re-loaded on a silica gel column once more using acetone-methanol （10 ： 1, V/V） as mobile phase with flow rate of 1 bed volume per hour, and during which another three peaks, peak 4 to peak 6, were observed, Compounds corresponding to peak 5 and peak 6 can not form crystal, and compounds corresponding to peak 4 were crystallized and recrystallized in petroleum and crystal C （sophoridine） was obtained with purity over 95.8%. The molecular structure determinations and the qualitative and quantitative analyses of the obtained monomer alkaloids were conducted by HPLC-MS, IR, melting point measurement and thin layer chromatography techniques.
出处
《高校化学工程学报》
EI
CAS
CSCD
北大核心
2007年第2期194-199,共6页
Journal of Chemical Engineering of Chinese Universities
关键词
苦豆子
生物碱单体
萃取
硅胶柱层析
结晶
Sophora alopecuroides L
monomeric alkaloids
extraction
silica gel column chromatography
crystallization
