基于双回路技术的二维色谱在线/离线接口设计与评价  

Design and Evaluation of Online/offline Interface Based on Double Loop for Two-dimensional Chromatography

作　　者：唐涛[1,2] 张维冰 张政[3] 夏明珠[1] 贡雪东[1] 王风云 李彤[2] TANG Tao;ZHANG Wei-Bing;ZHANG Zheng;XIA Ming-Zhu;GONG Xue-Dong;WANG Feng-Yun;LI Tong(Institute of Industrial Chemistry,Nanjing University of Science and Technology,Nanjing 210094,China;College of Chemistry and Chemical Engineering,Qiqihar University,Qiqihar 161006,China;Dalian Elite Analytical Instruments CO.,Ltd.Dalian 116023,China)

机构地区：[1]南京理工大学工业化学研究所,南京210094 [2]大连依利特分析仪器有限公司,大连116023 [3]齐齐哈尔大学化学与化学工程学院,齐齐哈尔161006

出　　处：《分析化学》2018年第3期311-316,共6页Chinese Journal of Analytical Chemistry

基　　金：本文系国家重大科学仪器设备开发专项(No.2012YQ12004401)和国家自然科学基金项目(No.51472121)资助

摘　　要：双回路技术是一套机械传动组件和流路系统,具有自动进样和馏分收集的双重功能。本研究基于双回路技术设计了一种二维液相色谱在线/离线接口,用以有效连接两种不同分离模式构建分离系统,提高系统峰容量,并对其功能进行了评价。以4种芳香族化合物为分离对象,利用设计的接口连接1套液相色谱系统,实现了进样、馏分收集、再进样纯度分析的多重操作集成;连接2套液相色谱系统,采用强阳离子交换模式对5种蛋白质样品进行初步分离,收集难分离组分,并通过再次进样到反相色谱模式的分离系统中,组分得到良好分离。进一步基于此接口连接1套强阳离子交换系统和1套微柱反相色谱系统,对牛血清白蛋白酶解产物进行在线二维分离,以1 m AU为积分阈值,共识别292个色谱峰。新型在线/离线接口可灵活实现样品微量制备、难分离组分的精细拆分和复杂样品的二维分离,为二维色谱系统的构建及分离研究提供了有力工具。By using a double loop technique based on a set of mechanical transmission components and a flow path system,a double function of injection and fraction collection was realized.On the basis of double loop technique,a novel type of online/offline interface for two-dimensional liquid chromatography was designed to construct an efficient separation system coupling two different separation modes with a higher peak capacity,and the functions of the interface were evaluated.By means of connecting the interface to an HPLC system,the multiple functions of injection,fraction collection and injection again were fulfilled for preparation and purity analysis of 4 kinds of aromatic compounds.As for combination of 2 sets of HPLC system,5 kinds of protein samples were separated preliminarily by strong cation exchange chromatography,and the components difficult to separate were collected and injected into reversed phase chromatographic system for further separation.Furthermore,the interface was applied to coupling two chromatographic systems in both strong cation exchange mode and microcolumn reversed-phase mode for the two-dimensional separation of bovine serum albumin enzymatic digest.When 1 mAU was set as the integral threshold,a total number of 292 peaks were identified.With the help of the online/offline interface,the preparation of microscale samples,fine separation of hardly separated samples and two-dimensional separation of complex samples were achieved flexibly.The result indicated that the system was a potent tool for the construction of two-dimensional chromatographic system and separation research.

关 键 词：双回路 在线接口 离线接口 馏分收集 自动进样 二维液相色谱 

分 类 号：TH833[机械工程—仪器科学与技术]