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银离子色谱法用于峰分辨率增强:应用于使用在线分段 LC-LC 技术的两种倍半萜的制备分离。

Silver ion chromatography for peak resolution enhancement: Application to the preparative separation of two sesquiterpenes using online heart-cutting LC-LC technique.

机构信息

Key Laboratory of Resource Biology and Biotechnology in Western China (Northwest University), Ministry of Education, Xi'an 710069, China; Biomedicine Key Laboratory of Shaanxi Province, College of Life Science, Northwest University, Xi'an 710069, China.

Key Laboratory of Resource Biology and Biotechnology in Western China (Northwest University), Ministry of Education, Xi'an 710069, China; Sorbonne Université, Institut Parisien de Chimie Moléculaire, CNRS UMR 8232, 4 Place Jussieu, 75005 Paris, France; Biomedicine Key Laboratory of Shaanxi Province, College of Life Science, Northwest University, Xi'an 710069, China.

出版信息

Talanta. 2018 Sep 1;187:252-258. doi: 10.1016/j.talanta.2018.05.043. Epub 2018 May 17.

DOI:10.1016/j.talanta.2018.05.043
PMID:29853043
Abstract

Silver ion chromatography, utilizing columns packed with silver ions bonded to silica gel, has proved to be an invaluable technique for the analysis of some positional isomers. In this work, silver ion chromatography by combination with online heart-cutting LC-LC technique for the preparative separation of two sesquiterpenes positional isomers from a natural product was investigated. On the basis of the evaluation that silver ion content impacts on the separation, the laboratory-made silver ion columns, utilizing silica gel impregnated with 15% silver nitrate as column packing materials, were used for peak resolution improvement of these two isomers and the preparative separation of them in heart-cutting LC-LC. The relationship among the maximal sample load, flow rate and peak resolution in the silver ion column were optimized, and the performance of the silver ion column was compared with conventional C column and silica gel column. Based on the developed chromatographic conditions, online heart-cutting LC-LC chromatographic separation system in combination with a silica gel column and a silver ion column that was applied to preparative separation of these two isomers from a traditional Chinese medicine, Inula racemosa Hook.f., was established. The results showed that the online heart-cutting LC-LC technique by combination of a silica gel column and a silver ion column for the preparative separation of these two positional isomers from this natural plant was superior to the preparative separation performed on a single-column system with C column or silica gel column.

摘要

银离子色谱法,利用填充有硅胶键合银离子的柱子,已被证明是分析某些位置异构体的非常有价值的技术。在这项工作中,结合在线心切割 LC-LC 技术,研究了银离子色谱法用于从天然产物中制备分离两种倍半萜类位置异构体。基于对银离子含量对分离影响的评估,使用实验室制备的银离子柱,其柱填充材料为 15%硝酸银浸渍的硅胶,用于改善这两种异构体的峰分辨率,并在心切割 LC-LC 中进行它们的制备分离。优化了银离子柱中最大样品负荷、流速和峰分辨率之间的关系,并比较了银离子柱与常规 C 柱和硅胶柱的性能。基于开发的色谱条件,建立了一种在线心切割 LC-LC 色谱分离系统,该系统结合硅胶柱和银离子柱,用于从传统中药旋覆花中制备分离这两种异构体。结果表明,与使用 C 柱或硅胶柱的单柱系统相比,硅胶柱和银离子柱在线心切割 LC-LC 技术结合用于从天然植物中制备分离这两种位置异构体的方法更优越。

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