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亲水分子印迹整体树脂制备及其在植物激素检测中的应用

发布时间:2018-11-08 15:25
【摘要】:分析复杂基质样品中的痕量目标药物时,由于基质组成的复杂性,需要对目标药物进行预分离和富集后才能进行检测,因此,开发吸附容量高、传质速率快、特异选择性强的吸附剂材料至关重要。分子印迹聚合物由于具有特异分子识别性和良好的稳定性,广泛应用于药物分析领域,但是目前仍存在水相识别性能较差、作用机制较单一和吸附剂颗粒填充不均匀影响萃取效率的问题。本文探索制备了亲水分子印迹整体树脂(hydrophilic molecularly imprinted monolithic resin,MIMR)和凹凸棒石/分子印迹整体树脂复合材料(attapulgite/molecularly imprinted monolithic resin composite material,AT/MIMR)并将优化后的MIMR和AT/MIMR作为固相萃取吸附剂,对豆芽和黄瓜中的痕量植物激素进行萃取检测。第一章,概述了分子印迹材料和整体材料的研究进展,并重点介绍了基于亲水树脂的分子印迹材料和基于凹凸棒石的分子印迹材料的优势。第二章,采用原位聚合法制备了亲水分子印迹三聚氰胺?尿素?甲醛整体树脂,并对制备参数进行了优化,将其作为固相萃取吸附剂,建立了准确、快速、简便的分析豆芽中植物激素的新方法。所建方法对豆芽中三种植物激素的检测限(LOD,S/N=3)在0.001?0.008μg g?1之间,定量限(LOQ,S/N=10)在0.004?0.027μg g?1之间,在0.03?5.00μg g?1范围内该方法的线性相关性良好,其相关系数(r)≥0.9997。第三章,制备了凹凸棒石/分子印迹整体树脂复合材料,考察了致孔剂种类以及凹凸棒石的掺杂质量分数对材料吸附性能的影响,将其作为固相萃取吸附剂,实现了黄瓜中三种植物激素的检测。所建方法对黄瓜中三种植物激素的检测限(LOD,S/N=3)在0.4?0.5 ng g?1之间,定量限(LOQ,S/N=10)在1.2?1.6 ng g?1之间,日内精密度在0.8%-2.7%之间,日间精密度在4.7%-7.8%之间。
[Abstract]:In the analysis of trace target drugs in complex matrix samples, due to the complexity of matrix composition, it is necessary to pre-separate and enrich the target drugs before they can be detected. Therefore, the development of high adsorption capacity and rapid mass transfer rate, Special and selective adsorbent materials are very important. Molecularly imprinted polymers are widely used in the field of drug analysis because of their special molecular recognition and good stability. The single mechanism and the uneven filling of adsorbent particles affect the extraction efficiency. In this paper, hydrophilic molecularly imprinted monolithic resin (hydrophilic molecularly imprinted monolithic resin,MIMR) and attapulgite / molecularly imprinted monolithic resin composite (attapulgite/molecularly imprinted monolithic resin composite material,) were prepared. AT/MIMR) and the optimized MIMR and AT/MIMR were used as solid phase extraction adsorbents to detect trace plant hormones in bean sprouts and cucumbers. In the first chapter, the research progress of molecular imprinting materials and monolithic materials is reviewed, and the advantages of molecular imprinting materials based on hydrophilic resin and attapulgite are emphasized. In chapter 2, hydrophilic molecularly imprinted melamine was prepared by in situ polymerization. Urea? The preparation parameters of formaldehyde monolithic resin were optimized and used as solid phase extraction adsorbent. A new method for the analysis of plant hormones in bean sprouts was established. The detection limit (LOD,S/N=3) of three plant hormones in bean sprouts was 0.001 ~ 0.008 渭 g / g, and the quantitative limit (LOQ,S/N=10) was 0.004 ~ 0.027 渭 g / g ~ (-1). The linear correlation of this method is good in the range of 0.03 ~ 5.00 渭 g 路g ~ (-1), and its correlation coefficient (r) 鈮,

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