摘要
利用高速逆流色谱分离制备无花果叶中的补骨脂素和佛手内酯,经过高效液相色谱、质谱、核磁共振检测,确定其纯度及结构。新鲜的无花果叶经干燥、破碎后用石油醚(60～90℃)室温浸提48h,浸提液经浓缩后得到浸膏。采用正己烷:乙酸乙酯:甲醇:水(1:1:1:1)的两相体系将所得的浸膏进行高速逆流色谱的分离纯化,得到样品A和样品B。利用高效液相色谱检测样品A和B的纯度分别为99.1%和98.2%。将得到的样品A和B进行MS,1H-NMR,13C-NMR检测确定其化学结构,并最终确认A为补骨脂素,B为佛手内酯。制备型高速逆流色谱可以成功的将无花果叶中的补骨脂素和佛手内酯进行分离制备。
The preparative high-speed counter-current chromatography （HSCCC） was applied to separating and purifying the psoralen and bergapten from the Ficus carica L leaves. At first, the crude extract was obtained by extracting with light petroleum from the dried leaves of Ficus carica L. Then, n-Hexane-ethyl acetate-methanolwater（ 1 ：1 ：1 ：1 ,v/v） was used as the HSCCC two-phase solvent system for the separation and purification. The components purified and collected were analyzed by high-performance liquid chromatography （HPLC）. The structures of psoralen and bergapten were identified by NMR and MS. This method yielded 4.4mg of psoralen at 99.1% purity and 2.1mg of bergapten at 98.2% purity from 200mg of the crude extract in a single run. Preparative high-speed counter-current chromatography could separate and purify these two components successfully from Ficus carica L leaves.
出处
《食品工业科技》
CAS
CSCD
北大核心
2008年第10期62-64,67,共4页
Science and Technology of Food Industry
基金
国家“十一五”科技支撑课题资助(2006BAD12B05-02)
关键词
高速逆流色谱
无花果叶
补骨脂素
佛手内酯
分离
preparative high-speed counter-current chromatography（HSCCC）
Ficus carica L leaves
psoralen
bergapten
separation
