分子印迹微萃取样品前处理技术在环境污染物分析中的应用研究

发布时间：2018-02-12 00:58

本文关键词： 分子印迹聚合物样品前处理整体材料固相微萃取　出处：《昆明理工大学》2017年硕士论文　论文类型：学位论文

【摘要】：分子印迹微萃取技术结合了分子印迹技术和微萃取技术两者的优点,并应用于样品前处理过程中。由于分子印迹聚合物具有选择性高、抗干扰能力强、样品用量小、有机溶剂用量少,可用于复杂样品中痕量目标分析物的分离与富集。本论文介绍了分子印迹微萃取材料的特点,并综述了其原理、制备方法、表征手段以及材料形式。同时开展了以雌二醇、双酚F和硝基苯酚为模板的分子印迹聚合物的应用研究,主要内容如下:1.雌二醇分子印迹整体材料的制备与应用研究:以雌二醇为模板分子,采用原位聚合法合成分子印迹整体材料;研究了雌二醇分子印迹整体材料的表面形貌和萃取性能,优化了萃取条件;建立了雌二醇MIP整体材料联用HPLC的分析方法,线性范围为0.5-50μg/L,检出限为0.1 μg/L(S/N=3);将雌二醇分子印迹整体材料联用高效液相色谱应用于实际水样中三种雌激素的萃取分析,加标浓度为20 μg/L时,两种水样加标的回收率在68.22%-102.52%,以及67.65%-103.72%,RSDs 在 3.18%-6.43%和 2.43%-5.70%之间(n=5)。2.双酚F替代模板分子印迹整体材料的制备和应用研究:以双酚F为替代模板分子制备得到分子印迹聚合物材料;研究了 BPF分子印迹整体材料的表面形貌、萃取性能,优化了 MIP整体材料的萃取条件,建立了 BPF-MIP整体材料联用HPLC的分析方法,并用于实际水样中BPA的萃取分析,线性范围为0.01-15μg/L(r=0.9998),检出限为0.003 μg/L(S/N=3);两种水样的回收率分别为65.56%-88.84%和70.48%-87.06,RSDs分别 2.15%-8.93%和1.30%-8.21%。3.对硝基苯酚环糊精分子印迹吸附萃取涂层的制备及其应用研究:对硝基苯酚为模板分子,采用四种新型环糊精衍生物为功能单体,通过原位聚合法合成分子印迹整体材料;研究了对硝基苯酚分子印迹吸附萃取涂层的表面形貌、萃取性能及协同作用,优化了 MIP吸附萃取涂层的萃取条件,建立了 MIP吸附萃取涂层联用HPLC的分析方法,线性范围均为10-200 μg/L,硝基苯酚的检出限为3μg/L,双酚A检出限为1.5μg/L;应用于河水中三种硝基苯酚和BPA的萃取分析,其中对硝基苯酚、邻硝基苯酚、间硝基苯酚和双酚A的回收率在88.17%-104.54%之间,RSDs为0.54%-8.28%。
[Abstract]:The molecularly imprinted microextraction technology combines the advantages of both the molecular imprinting technique and the microextraction technology, and is applied in the sample pretreatment process. Because of the high selectivity, strong anti-interference ability and small sample dosage of the molecularly imprinted polymer, In this paper, the characteristics of molecularly imprinted microextraction materials are introduced, and their principles and preparation methods are summarized. At the same time, the application of imprinted polymers with estradiol, bisphenol F and nitrophenol as templates was studied. The main contents are as follows: 1. Preparation and application of estradiol molecularly imprinted monolayer: using estradiol as template molecule, in situ polymerization method was used to synthesize molecularly imprinted monolithic material; The surface morphology and extraction performance of estradiol molecularly imprinted monolithic materials were studied and the extraction conditions were optimized. A method for the analysis of estradiol MIP monolithic materials with HPLC was established. The linear range is 0.5-50 渭 g 路L ~ (-1) and the detection limit is 0.1 渭 g 路L ~ (-1) N ~ (-1) N ~ (3 +). When the standard concentration is 20 渭 g / L, the Estradiol molecularly imprinted whole material is used in the extraction analysis of three kinds of estrogens in the real water samples by high performance liquid chromatography. The recoveries of two kinds of water samples were between 68.22 and 102.52, and the RSDs were between 3.18-6.43% and 2.43-5.70%. The preparation and application of bisphenol F substitute template molecular imprinting materials were studied: using bisphenol F as substitute template molecule to obtain molecularly imprinted polymer materials; The surface morphology and extraction properties of BPF molecularly imprinted monolithic materials were studied. The extraction conditions of MIP monolithic materials were optimized. The analytical method of BPF-MIP monolithic materials combined with HPLC was established and applied to the extraction analysis of BPA in real water samples. The linear range was 0.01-15 渭 g / L ~ 0.9998 渭 g 路L ~ (-1) 路L ~ (-1) L ~ (-1), the detection limit was 0.003 渭 g / L ~ (-1) 渭 g 路L ~ (-1) N ~ (-1) N, the recoveries of the two water samples were 65.56% -88.84% and 70.48% -87.06% RSDs, respectively, 2.15-8.93% and 1.30-8.21 路3.The preparation and application of p-nitrophenol cyclodextrin molecular imprinting extraction coating were studied. Four new cyclodextrin derivatives were used as functional monomers to synthesize molecularly imprinted monolithic materials by in situ polymerization. The extraction conditions of MIP adsorption and extraction coating were optimized, and the analytical method of MIP adsorption and extraction coating combined with HPLC was established. The linear range is 10-200 渭 g / L, the detection limit of nitrophenol is 3 渭 g / L, and the detection limit of bisphenol A is 1.5 渭 g / L. The recoveries of m-nitrophenol and bisphenol A ranged from 88.17% to 104.54% and the RSDs were 0.54 -8.28%.
【学位授予单位】：昆明理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：X502;O631.3

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