【作者】 周涛；

【导师】 周杰；

【作者基本信息】 山东农业大学 ， 分析化学， 2013， 硕士

【摘要】 整体柱是采用原位聚合的方法制备得到的整体、连续的柱体，又称连续床。近几年整体柱技术愈来愈受到人们的重视。整体柱技术的出现使分子印迹技术的发展又进一步，模板分子可直接在整体柱的制备过程中使用，免去了传统制备方法中的磨碎等步骤简化了制备方法且提高了重复性。分子印迹整体柱结合分子印迹技术和整体柱技术的优势，扩展了两种技术的研究领域，而且增加了原有技术的实用性。分子印迹整体柱技术吸引了许多学者的研究，并正在高速发展。多氯联苯(Polychlorinated biphenyls, PCBs)是一类人工合成的广泛存在于生物圈的持久性有机污染物(Persistent organic pollutants, POPs),其分子结构为联苯苯环上的氢原子被氯原子取代而形成。3,3-二氯联苯胺(3,3-dichlorobenzidine，DCB)是生产联苯胺黄和永固橘黄等不可替代的原料。DCB是动物致癌物质，可诱导大鼠、小鼠、仓鼠及狗等多种动物发生肿瘤，对人为可疑致癌物。对环境有危害，对水体可造成污染。DCB作为永久性有机污染物,易挥发性使得其污染途径及危害成为关注的焦点。因此，明确DCB的环境行为，准确检测环境中DCB的残留，对消除其危害极为重要。目前，常用的DCB检测方法有紫外分光光度法、高效液相色谱法。但这些方法前处理过程复杂，且成本较高。分子印迹聚合物(MIP)整体柱制备方法简单，选择性好且成本低，在色谱分离、固相萃取等方面得到了广泛的应用。用原位聚合法制备分子印迹整体柱已有许多报道，但这些报道多数使用有机溶剂作为致孔剂，对强极性有机化合物的识别受到一定限制。本研究选用离子液体为致孔剂可克服上述的缺点，制备了DCB的分子印迹整体柱对模板分子DCB表现为较高的选择性。本文做了如下研究内容：1.以3,3-二氯联苯胺为模板分子，甲基丙烯酸为功能单体，偶氮二异丁腈为引发剂，乙二醇二甲基丙烯酸酯作为交联剂，1-丁基-3-甲基咪唑六氟磷酸盐离子液体为致孔剂，乙腈和氯仿混合溶液为溶剂，合成了3,3-二氯联苯胺分子印迹整体柱。2.考察了3,3-二氯联苯胺分子印迹整体聚合物的结合性质及其在3,3-二氯联苯胺分子聚合物上的选择性分离富集特性。更多还原

【Abstract】 Monolithic column is a continuous column obtained by in situ polymerization preparation,also known as the continuous bed. People pay more and more attention to the monolithiccolumn technology in recent years. The monolithic column technology and the appearance ofthe further development of molecular imprinting technique, the template can be used in theproduction process of the imprinted monolithic column, in which the traditional grinding andother steps are omitted. The molecularly imprinted monolithic column is prepared based onmolecular imprinting coupled to monolithic column technology, expand the research field oftwo kinds of technology and increase the practicability of the original technology. Techniquesof molecular imprinted monolithic column has attracted many researchers, and is developingrapidly.Polychlorinated biphenyls (PCBs) are persistent organic pollutants (POPs) widespread inthe biosphere. The hydrogen atom on the benzene to biphenyl is replaced by chlorine atomsto form.3,3–dichlorobenzidine (DCB) which is an irreplaceable material of benzidineyellow and orange and. DCB is an animal carcinogen, can induce rat, mouse, hamster anddogs and other animal tumor, and it is the man suspected carcinogen.It is harm to theenvironment, resulting in water contamination. DCB as persistent organic pollutants, volatilemakes the pollution and harm has become the focus of attention. Therefore, the clear DCBenvironmental behavior and residual accurate detection in the environment of DCB is veryimportant to eliminate the harm.At present, DCB detection methods include ultraviolet spectrophotometric method, highperformance liquid chromatography. But these methods before the process is complex and thecost is high. Molecularly imprinted polymers (MIP) monolithic column has simplepreparation method, good selectivity and low cost, and has been widely used inchromatographic separation and solid phase extraction. For preparation of molecularlyimprinted monolithic columns, many organic solvents are used as porogen, thus strongrecognition of polar organic compounds are subject to certain restrictions. In this study, ionicliquid was used as the pore-forming agent and overcome the above shortcomings, andmolecularly imprinted monolithic column for the template DCB showed higher selectivity. The following studies are done in this paper.1. Using3,3-dichlorobenzidine as the template, methacrylic acid (MAA) as the functionalmonomer, azobisisobutyronitrile (AIBN) as a initiator, ethylene glycol dimethacrylate(EGDMA) as the cross-linker, BMIMPF6as the porogent, and the mixture of acetonitrile andchloroform as the solvent, a3,3-dichlorobenzidine imprinted monolithic column wasprepared by in situ molecular imprinting technique, and its binding properties and selectivitywere investigated.2. The binding character of DCB imprinted monolithic column was investigated and itexhibted specific recognition ability for DCB comparedted to its structural analogues underselected conditions．更多还原