成功的应用高效逆流色谱技术一次分离两类顺反异构体

Four flavonoids, isoastilbin, astilbin, isoengelitin, and engelitin were isolated and purified simultaneously from Smilacis Glabrae Roxb. for the first time by high performance counter-current chromatography using a system consisting of n-hexane–n-butanol–water (1:2:3, v/v/v). A total of 392.6 mg of astilbin, 71.4 mg of isoastilbin, 47.4 mg of engelitin, and 10.3 mg of isoengelitin were purified from 1.89 g of the ethyl acetate extract of Smilacis Glabrae Roxb. in six runs, each at over 94.51% purity as determined by HPLC. The structures of the four compounds were identified by their retention time, the LC-ESI-MSn in the negative ion mode, and confirmed by 1H-NMR experiments. The characteristic LC-ESI-MS fragmentation patterns of the four compounds were discussed.

Four flavonoids, isoastilbin, astilbin, isoengelitin, and engelitin were isolated and purified simultaneously from Smilacis Glabrae Roxb. for the first time by high performance counter-current chromatography using a system consisting of n-hexane–n-butanol–water (1:2:3, v/v/v). A total of 392.6 mg of astilbin, 71.4 mg of isoastilbin, 47.4 mg of engelitin, and 10.3 mg of isoengelitin were purified from 1.89 g of the ethyl acetate extract of Smilacis Glabrae Roxb. in six runs, each at over 94.51% purity as determined by HPLC. The structures of the four compounds were identified by their retention time, the LC-ESI-MSn in the negative ion mode, and confirmed by 1H-NMR experiments. The characteristic LC-ESI-MS fragmentation patterns of the four compounds were discussed.

成功地应用ASE快速溶剂萃取与高效逆流色谱结合技术在线提取、分离罗布麻叶中5种化学成分。从10.02g罗布麻叶药材饮片中，以乙酸乙酯：甲醇：水体积比为5:2:5溶剂系统的上层溶剂作为ASE的提取溶剂和高效逆流色谱地固定相，分离得到28.4mg贯叶金丝桃干,液相检测纯度为97.28%,32.7mg adhyperforin液相检测纯度为97.81%两种疏水性化合物；以乙酸乙酯：甲醇：正丁醇：水体积比为5:2:2.5:12溶剂系统的下层溶液做为ASE的提取溶剂和高效逆流色谱地流动相，分离得到12.7mg的3,4,5-Otricaffeoylquinic acid（液相检测纯度为98.82%），15.2mg 的1,3,5-Otricaffeoylquinic acid（液相检测纯度高达99.46%）和42.5mg 的连翘苷（液相检测纯度为96.9%），该技术一步实现了中药中有效成分的提取分离。

逆流色谱技术起源于上世纪八十年代，在短短的几十年里已发展成为现代分离领域的领航者，以其独特地分离优势，受到广大科研工作者的青睐和重视。