Key Laboratory for Applied Technology of Sophisticated Analytical Instruments of Shandong Province, Shandong Analysis and Test Center, Qilu University of Technology (Shandong Academy of Sciences), Jinan, P. R. China.
Key Laboratory for Natural Active Pharmaceutical Constituents Research in Universities of Shandong Province, School of Pharmaceutical Sciences, Qilu University of Technology (Shandong Academy of Sciences), Jinan, P. R. China.
J Sep Sci. 2023 Nov;46(22):e2300497. doi: 10.1002/jssc.202300497. Epub 2023 Sep 22.
In this work, eight compounds from Phellodendron chinense were separated and purified by pH-zone refining counter-current chromatography and traditional counter-current chromatography coupled with online-storage inner-recycling counter-current chromatography (IRCCC). The pH-zone-refining mode was adopted for separating 2.0 g of crude extract with the solvent system of chloroform-methanol-water (4:3:3, v/v), in which 10 mM hydrochloric acid and 10 mM triethylamine were added in the stationary and mobile phases, respectively. Meanwhile, traditional counter-current chromatography coupled with online-storage IRCCC separation was performed by the solvent system of n-hexane-ethyl acetate-methanol-water (5:5:2:8, v/v). Finally, eight compounds, including six alkaloids as 6-methylpiperidin-2-one(1), isoplatydesmine(4), berlambine(5), epiberberine(6), palmatine(7), berberine(8) and two phenolic acids as ferulic acid(2), isoferulic acid(3), were successfully obtained using these three different CCC modes with the purities over 95.0%.
在这项工作中,采用 pH 区带精制逆流色谱法和传统逆流色谱法结合在线储存内循环逆流色谱法(IRCCC),从黄柏中分离和纯化了 8 种化合物。采用 pH 区带精制模式,以氯仿-甲醇-水(4:3:3,v/v)为溶剂系统,分别在固定相和流动相中加入 10mM 盐酸和 10mM 三乙胺,从 2.0g 粗提物中分离。同时,采用正己烷-乙酸乙酯-甲醇-水(5:5:2:8,v/v)为溶剂系统,进行传统逆流色谱法结合在线储存 IRCCC 分离。最后,采用这三种不同的 CCC 模式,成功地获得了 8 种化合物,包括 6 种生物碱(如 6-甲基哌啶-2-酮(1)、异platydesmine(4)、berlambine(5)、epiberberine(6)、palmatine(7)、berberine(8))和 2 种酚酸(如阿魏酸(2)、异阿魏酸(3)),纯度均超过 95.0%。