Wang Jiajia, Gu Dongyu, Wang Miao, Guo Xinfeng, Li Haoquan, Dong Yue, Guo Hong, Wang Yi, Fan Mengqi, Yang Yi
School of Light Industry and Chemical Engineering, Dalian Polytechnic University, Dalian 116034, China.
School of Marine Science and Environment Engineering, Dalian Ocean University, Dalian 116023, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 May 15;1053:16-19. doi: 10.1016/j.jchromb.2017.04.013. Epub 2017 Apr 4.
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, 1.4g of crude sample II was obtained from 18.5g 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, 31mg of robinin and 37mg of kaempferol 7-O-α-l-rhamnopyranoside were isolated from 200mg of crude sample II in a single run of HSCCC. A scale-up separation was also performed, and 160mg of robinin with 95% purity and 188mg of kaempferol 7-O-α-l-rhamnopyranoside with 97% purity were produced from 1.2g of crude sample II.
建立了一种合理的液液萃取方法，用于高速逆流色谱（HSCCC）分析的样品预处理。通过系统筛选目标化合物的分配系数，分别选择正己烷-乙酸乙酯-甲醇-水（4:5:4:5，v/v）和（1:5:1:5，v/v）作为液液萃取的溶剂体系，以去除样品中的低极性和高极性杂质。液液萃取后，从18.5g刺槐花花中提取的粗样品I中获得了1.4g粗样品II，然后使用由正己烷-乙酸乙酯-甲醇-水（1:2:1:2，v/v）组成的溶剂体系通过HSCCC进行分离。结果，在单次HSCCC运行中，从200mg粗样品II中分离出31mg刺槐苷和37mg山奈酚7-O-α-L-鼠李糖苷。还进行了放大分离，从1.2g粗样品II中制备出了纯度为95%的160mg刺槐苷和纯度为97%的188mg山奈酚7-O-α-L-鼠李糖苷。
