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分子印迹聚合物的制备及其在固相萃取中的应用

Preparation of Molecularly Imprinted Polymer and the Application in Solid Phase Extraction

【作者】 杨淑玲

【导师】 郑红;

【作者基本信息】 青海师范大学 , 无机化学, 2011, 硕士

【摘要】 近些年,食品安全事故不断发生,尤其是农产品的药物残留问题,越来越受到国家的重视。由于固相萃取(SPE)在痕量物质的预富集和分离中,样品处理简便、富集分离效果好、易与不同的检测仪器相结合等优点,已成为目前最流行的样品预处理方法,广泛应用于药物、环境、食品、临床和化工等领域。本论文主要基于分子印迹技术,制备出具有理想机械和物理化学性能的分子印迹聚合物,用做固相萃取材料,对目标分析物进行高效率的富集和分离,得到的样品处理液直接用于测样,获得可靠的分析检测结果。本论文主要进行了如下的创新性工作:1、采用放热少、反应慢的逐步聚合反应制备出了尺寸更大、性能更优越的环氧树脂聚合物。2、分子印迹技术与环氧树脂基聚合物相结合,用于目标分析物的固相萃取,为色谱、荧光作为检测手段提供了相关的分析方法。3、基于Fe2+催化H2O2氧化KI为13-,13-与丁基罗丹明B反应的产物导致体系的共振散射强度急剧增强,建立一种以丁基罗丹明B为探针的测定痕量H202的催化共振散射光谱新方法。本论文研究的主要内容如下:1利用环氧树脂,二乙烯三胺,聚乙二醇为原料,采用逐步聚合反应制备出了对硫磷,甲基对硫磷,敌敌畏,马拉硫磷,丁基罗丹明B五种印迹聚合物,应用于溶液样品中标准品的预富集和分离。用建立的方法测定食物中标准品的痕量残余方法简单,准确度高。2共振光散射法研究了缓冲体系,酸度及试剂用量对水中双氧水测定的影响。建立的这种方法可以测定自来水,饮用水,矿泉水等中双氧水的含量。

【Abstract】 In recent years, food safety accidents take place uninterrupted and the problem has been paid more and more national attention, especially the pesticide residue in agricultural products. Solid phase extraction (SPE) was used in the pre-concentration and separation to the trace substances, and owns some merits as follows:sample preparation simple, enrichment and separation effective, combination with different testing instruments etc. So SPE is the most popular sample pretreatment methods, which are widely used in medicine, environment, food, clinical and chemical industry etc.This paper mainly studied molecular imprinting technique, basing on this technique, prepared with the ideal imprinted polymers which own perfect mechanical and physical-chemical properties and be used as solid phase extraction materials. By means of the polymers, analyte was been concentrated and separated efficiently, and the obtained sample liquid directly used to be analyzed, ultimately, analytical results are reliable.In this thesis, we carried the following innovative work:First, epoxy monolithic column was synthesized via the exothermic and stepwise.polymerization reaction, moreover the column having bigger cavity and the more superior performanceSecond, the epoxy-based polymer combined with molecular imprinting technique, was used to handle target analyte through solid-phase extraction. It is designed to provide relevant analysis method for chromatographic, fluorescence detection means.Third, otassium iodide (KI) was oxidize to I3- by oxyful at the catalysis of Ferrous ion(Fe2+),based on the point, the product of I3- reacted with butyl-rhodamine B was lead to the system resonance scattering intensity sharp increase, therefore, using butyl-rhodamine B as a probe establishes a catalytic resonance scattering spectra new methods to detect the trace hydrogen peroxide solution(H2O2).The main content of this paper are as follows: Using the epoxy resin, ethylenetriamine, polyethylene glycol as raw materials, parathion, methyl parathion, dichlorvos, malathion, butyl-rhodamine B five imprinted polymer was prepared by the stepwise polymerization, which are used as sample pre-enrichment and separation towards the standard. By this method we can detect the trace residual in food simple and accurately.We studied the influence of buffer system, acidity and reagent dosage etc. to detect H2O2 in H2O by resonance light scattering method. By this method we test the quantity of hydrogen peroxide in tap water, drinking water, mineral water.

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