浊点萃取在线富集-毛细管电泳电化学检测联用技术及食品中痕量汞形态分析

Hyphenation of different technology which could improve the analysis efficiency for the complex samples and extend the application is the main tend of development and hotspot in analytical science. At present Study on capillary electrophoresis electrochemical detection (CE-ED) coupled with on-line cloud point extraction (on-line CPE) has not been reported. The problem is how to operate in an on-line cloud point extraction system and how to design the joint of the Hyphenation of an on line-CPE system with CE-ED. .A suitable answer has been put forward in the project. Flow injection technology of which the flow path could be designed variably and a mini-column which could adsorb surfactant were implied in the on-line CPE system. By the way the operation of on-line CPE could be accomplished through an on-line procedure of dilution, admixture, extraction and elution by adding surfactant, chelate complex and other organic solvent orderly through different flow path. A microchip will be made as the joint of CE-ED coupled with on line-CPE. Study on the application of the speciation analysis of ultratrace mercury in food based on the above on-line-CPE-CE-ED system will also be carried out. A new method will be established involved enrichment on line and determination of ultratrace mercury in food.

联用技术是目前分析科学发展的主要趋势和研究热点。通过各类仪器或技术联用可显著改善分析体系的性能，实现对复杂样品的分析。目前国内外尚未见有浊点萃取在线富集(on-line CPE)与毛细管电泳电化学检测技术(CE-ED)联用方面的报道。困扰这一问题的关键是浊点萃取技术的在线操作难题和仪器联用接口设计的难题。.本项目利用流动注射技术具有流路设计灵活多变，易于实现复杂流路切换的特点，提出浊点萃取的在线操作采用流动注射技术方式进行和微柱吸附表面活性剂的新思路，通过流路切换使表面活性剂、螯合剂和洗脱剂等循序加入，实现在线稀释、在线混合、在线萃取和洗脱，解决浊点萃取的在线操作难题；通过芯片技术制作on-line-CPE-CE-ED联用系统的接口。同时将上述建立的on-line-CPE-CE-ED联用系统应用于食品中超痕量汞的形态分析，建立一种在线浓缩富集-测定一体化的食品中超痕量汞形态分析的新手段。

本项目是开展浊点萃取在线富集-毛细管电泳电化学检测联用系统的研制及食品中痕量汞形态分析。项目完成了浊点萃取在线富集-毛细管电泳仪联用系统的设计和研制，同时开展了浊点萃取技术用于痕量金属离子及其形态分析方面的应用工作。在建立方法的过程中，独创性地采用统计学方法优化浊点萃取条件，克服了单因素法忽略各因素之间交互效应的缺陷，取得了较好的研究成果，发表科研论文8篇（SCI收录3篇），2篇已录用，申请专利4项。