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0.4g,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%.