摘要
为建立一条不用柱层析法提纯烟叶浸膏中茄尼醇的路线,考察了NaOH和乙醇的用量、皂化时间、除蜡溶剂、结晶溶剂和结晶时间对茄尼醇提纯效果的影响,确定了于无水乙醇中用4%(质量分数)NaOH在65℃下皂化4h、浓盐酸调pH值至中性、过滤除蜡、-18℃下甲醇结晶2次(6h/次)、乙腈重结晶2次的工艺路线,并采用该工艺由50g含7.4%茄尼醇的烟叶浸膏中提纯得到5.1g白色固体,其熔点41.5℃,茄尼醇含量90.5%。该工艺可用于烟叶浸膏中茄尼醇的提纯。
In order to develop a purification procedure for solanesol from tobacco extract without column chromatography, the effects of the dosage of NaOH and alcohol in saponification, saponification time, dewaxing solvent, crystallization solvent and crystallization time on the extraction and purification of solanesol were investigated. The determined optimumprocedure was： tobacco extract in anhydrous alcohol was saponified at 65 ℃ for 4 hours at the presence of 4% NaOH （mass/mass）, then neutralized with concentrated hydrochloric acid, filtrated for dewaxing, crystallized in methanol at -18 ℃ for 6 hours twice and recrystallized in aceto- nitrile twice. 5.1 g of white solid （solanesol concentration 90.5%, mp 41.5 ℃ ） was obtained from 50 g tobacco extract containing 7.4% of solanesol by the procedure. This procedure could be used to isolate solanesol from tobacco extract.
出处
《烟草科技》
EI
CAS
北大核心
2008年第4期42-45,59,共5页
Tobacco Science & Technology
关键词
茄尼醇
烟叶浸膏
提纯
结晶
Solanesol
Tobacco extract
Extraction and purification
Crystallization
