Two-dimensional preparative liquid chromatography system for preparative separation of minor amount components from complicated natural products
Two-dimensional preparative liquid chromatography system for preparative separation of minor amount components from complicated natural products
复制标题
用于从复杂天然产物中制备分离微量成分的二维制备液相色谱系统
DOI：
10.1016/j.aca.2014.02.023
复制
发表时间：
2014-04-11
影响因子：
6.2
通讯作者：
Wu, Zhen
中科院分区：
文献类型：
--
作者：
Qiu, Ying-Kun;Chen, Fang-Fang;Wu, Zhen
开发了一种在线综合二维制备液相色谱系统，用于从复杂的天然产物中制备分离微量成分。中压液相色谱仪（MPLC）作为第一维，制备型HPLC作为第二维，与捕获柱和补充泵结合使用。从柱尺寸、稀释比、径高比以及中压液相色谱仪的系统压力等方面评价捕获柱的性能。使用市售的 15 mm x 30 mm i.d. 可以获得令人满意的捕获效率。 ODS 预柱。通过粗大孔树脂富集的和涛大黄水提取物的克级分离说明了该 MPLC x 制备型 HPLC 系统的仪器操作和性能。该系统可在短时间内实现25种化合物的自动多步制备分离，并通过MS、H-1 NMR甚至灵敏度较低的C-13 NMR鉴定其结构，与传统方法相比在分析效率和样品处理能力方面表现出巨大优势。 (C) 2014 Elsevier B.V. 保留所有权利。
An on-line comprehensive two-dimensional preparative liquid chromatography system was developed for preparative separation of minor amount components from complicated natural products. Medium-pressure liquid chromatograph (MPLC) was applied as the first dimension and preparative HPLC as the second one, in conjunction with trapping column and makeup pump. The performance of the trapping column was evaluated, in terms of column size, dilution ratio and diameter-height ratio, as well as system pressure from the view of medium pressure liquid chromatograph. Satisfactory trapping efficiency can be achieved using a commercially available 15 mm x 30 mm i.d. ODS pre-column. The instrument operation and the performance of this MPLC x preparative HPLC system were illustrated by gram-scale isolation of crude macro-porous resin enriched water extract of Rheum hotaoense. Automated multi-step preparative separation of 25 compounds, whose structures were identified by MS, H-1 NMR and even by less-sensitive C-13 NMR, could be achieved in a short period of time using this system, exhibiting great advantages in analytical efficiency and sample treatment capacity compared with conventional methods. (C) 2014 Elsevier B.V. All rights reserved.