溶剂
样品制备
高效液相色谱法
洗脱
分析物
离子液体
固相萃取
检出限
溶剂萃取
液相色谱-质谱法
液态液体
甲醇
中心组合设计
作者
Jiajia Wang,Dongyu Gu,Miao Wang,Xinfeng Guo,Haoquan Li,Yue Dong,Hong Guo,Yi Wang,Mengqi Fan,Yi Yang
标识
DOI:10.1016/j.jchromb.2017.04.013
摘要
A rational liquid–liquid extraction approach was established to pre–treat samples for high–speed counter–current chromatography (HSCCC). n-Hexane–ethyl acetate–methanol–water (4:5:4:5, v/v) and (1:5:1:5, v/v) were selected as solvent systems for liquid–liquid extraction by systematically screening K of target compounds to remove low- and high-polarity impurities in the sample, respectively. After liquid–liquid extraction was performed, 1.4 g of crude sample II was obtained from 18.5 g of crude sample I which was extracted from the flowers of Robinia pseudoacacia L., and then separated with HSCCC by using a solvent system composed of n–hexane–ethyl acetate–methanol–water (1:2:1:2, v/v). As a result, 31 mg of robinin and 37 mg of kaempferol 7–O–α–l–rhamnopyranoside were isolated from 200 mg of crude sample II in a single run of HSCCC. A scale–up separation was also performed, and 160 mg of robinin with 95% purity and 188 mg of kaempferol 7–O–α–l–rhamnopyranoside with 97% purity were produced from 1.2 g of crude sample II.
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