Two-dimensional counter-current chromatography: 1st Traditional counter-current chromatography, 2nd acid-base elution counter-current chromatography
Two-dimensional counter-current chromatography: 1st Traditional counter-current chromatography, 2nd acid-base elution counter-current chromatography
复制标题
二维逆流色谱：第一传统逆流色谱、第二酸碱洗脱逆流色谱
DOI：
10.1016/j.chroma.2010.12.084
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发表时间：
2011-09-09
影响因子：
4.1
通讯作者：
Pan, Yuanjiang
中科院分区：
文献类型：
--
作者：
Hu, Ruilin;Dai, Xiaojing;Pan, Yuanjiang
建立了一种固相捕集界面在线柱切换逆流色谱（CCC）。采用固相捕集中间相，避免了大体积进样。因此，可以利用完全不同化学组成的两相溶剂体系来增强体系的正交性。在本工作中，在第一维中使用140 mL容量的CCC仪器，并且在第二维分离中使用平行的三线圈CCC离心机（每个线圈40 mL），允许同时进样三次。采用由正己烷：乙酸乙酯：甲醇：水（1：1：1：1，v/v）组成的双相溶剂系统。在第一维中获得五个分离良好的级分。两个组分在线浓缩，并在由甲基叔丁基醚：乙腈：水（2：2：3，v/v）组成的溶剂系统中进行第二维分离。其中将三氟乙酸（10 mM）添加到上层有机相中作为保留剂，并将三乙胺（10 mM）添加到水性移动的相中作为洗脱剂。从中药大黄中一步分离纯化出4个羟基蒽醌类化合物。(C)2011 Elsevier B. V.保留所有权利。
An on-line column-switching counter-current chromatography (CCC) with solid-phase trapping interphase is presented in this paper. The large volume injection is avoided using solid-phase trapping interphase. Thereby, totally different chemical composition biphasic solvent system can be utilized to enhance system orthogonality. In the present work, a 140 mL-capacity CCC instrument was used in the First dimension, and a parallel three-coil CCC centrifuge (40 mL each coil) was used in the second dimensional separation allowing three injections at the same time. With biphasic solvent system composed of n-hexane: ethyl acetate: methanol: water (1:1:1:1, v/v). five well-separated fractions were obtained in the First dimension. Two fractions were online concentrated and further separated in the second dimension with solvent system composed of methyl tert-butyl ether: acetonitrile: water (2:2:3, v/v). where trifluoroacetic acid (10 mM) was added to the upper organic phase as a retainer and triethylamine (10 mM) to the aqueous mobile phase as an eluter. Four hydroxyanthraquinones were successfully separated and purified from Chinese medicinal plant Rheum officinale in only one step. (C) 2011 Elsevier B.V. All rights reserved.