尿素柱层析结合重结晶制备高纯度茄尼醇  

Preparation of High-purity Solanesol by Urea Column Chromatography Combining with Recrystallization

作　　者：韩蕊蕊[1] 吕纯洁[2] 邓天昇 刘旭光[1] 侯相林[3] 

机构地区：[1]太原理工大学化学化工学院,太原市迎泽西大街79号030024 [2]洛阳理工学院机械工程系,河南省洛阳市王城大道90号471000 [3]中国科学院山西煤炭化学研究所,太原市桃园南路27号030001 [4]中国科学院研究生院

出　　处：《烟草科技》2012年第5期40-43,共4页Tobacco Science & Technology

基　　金：长江学者与创新团队发展计划项目"纳米材料界面物理与化学问题"(IRT0972);国家自然科学基金项目"洋葱状富勒烯表面分子印迹材料制备与性能表征"(20971094);山西省科技攻关项目"从亚麻籽提取高纯度木酚素的中试研究"(20100312026)

摘　　要：为制备高纯度的茄尼醇,进行了尿素柱层析结合重结晶分离茄尼醇试验,考察了尿素柱层析固定相尿素与硅胶的比例、洗脱溶剂、上样量对茄尼醇纯度和收率的影响。结果表明:尿素柱层析固定相尿素与硅胶质量比1∶1,洗脱剂石油醚与乙酸乙酯体积比60∶1,上样量0.4 g,茄尼醇的纯度和收率分别为74.8%和89.8%。再经过甲醇、乙腈各结晶一次,茄尼醇的纯度达96.7%,总收率0.1248%。该方法可以用于浸膏中茄尼醇的精制。To obtain high-purity solanesol, an experiment on the refinement of solanesol by urea column chromatography combining with recrystallization was conducted. The influences of ratio of urea to silica gel in stationary phase, elution solvent and the sample loading in urea column chromatography on the purity and yield of solanesol were investigated. The results showed that when the mass ratio of urea to silica gel in stationary phase was 1：1 （w/w）, the proportion of petroleum ether to ethyl acetate in elution solvent was 60：1 （v/v）, the sample loading was 0.4 g, the purity and yield of solanesol reached 74.8% and 89.8%, respectively. The resultant solanesol was recrystalized in methanol and acetonitrile sequentially, and a white crystalline solanesol was obtained with purity of 96.7% and yield of 0.1248%.

关 键 词：茄尼醇 精制 尿素柱层析 重结晶 

分 类 号：TS49[农业科学—烟草工业]