酚醛印迹树脂制备及痕量组分萃取分离方法研究

发布时间：2018-04-20 07:46

  本文选题：亲水树脂 + 分子印迹　； 参考：《河北大学》2017年硕士论文

【摘要】：近年来随着食品药品安全问题日益突出,生物样品中低浓度药物组分的准确、快速和定量检测成为药物分析领域的热点和难点。由于样品基质复杂,需要对其进行前处理后才能用于检测。在众多的样品前处理方法中,固相萃取因具有操作简单、省时、高效、有机试剂用量少等优点而被广泛应用于生物、医药、食品等多个领域。固相萃取的核心是吸附剂的选择,分子印迹聚合物由于其高特异选择性和实用性的特点被广泛用作固相萃取吸附剂,但其仍存在一定局限性。针对传统分子印迹聚合物水相识别性能差、功能单体与交联剂种类较为单一等问题,本文开发了两种新型亲水印迹树脂材料,并结合固相萃取技术,实现了复杂基质样品中痕量目标药物的快速分离和富集。第一章,概述了固相萃取技术、亲水树脂与分子印迹技术的原理与现状,重点介绍了亲水分子印迹树脂的研究进展及发展前景。第二章,采用低共熔溶剂为反应溶剂,制备了间苯三酚 甲醛 三聚氰胺亲水印迹树脂(MIPFMR),优化了制备过程中的参数。将优化后的MIPFMR作为固相萃取的吸附剂,建立了准确、快速分离检测尿样中激动剂药物残留的新方法,对盐酸氯丙那林与盐酸班布特罗的平均回收率在91.7-100.1%的范围内(RSD≤7.6%)。第三章,制备了3-氨基苯酚 乌洛托品亲水印迹树脂(MIAPH),对制备过程中的参数进行了优化,将优化好的MIAPH应用于固相萃取 高效液相色谱法,实现了对豆芽样品中植物激素的选择性萃取,并应用于市售豆芽样品,检测到了6-苄基腺嘌呤的残留,浓度为0.11 mg kg~(-1)。
[Abstract]:In recent years, with the increasingly prominent food and drug safety problems, the accurate, rapid and quantitative detection of low concentration drug components in biological samples has become a hot and difficult point in the field of drug analysis. Because the sample matrix is complex, it needs to be pretreated before it can be used for detection. Solid-phase extraction (SPE) has been widely used in many fields, such as biology, medicine, food and so on, because of its advantages of simple operation, time saving, high efficiency and low dosage of organic reagent. The core of solid phase extraction (SPE) is the selection of adsorbent. Molecularly imprinted polymers (MIPs) are widely used as adsorbents for solid phase extraction due to their high selectivity and practicability, but they still have some limitations. In this paper, two new hydrophilic imprinted resin materials were developed and combined with solid phase extraction (SPE) technology to solve the problems of poor water phase recognition performance of traditional molecularly imprinted polymers and single functional monomer and crosslinking agent. The rapid separation and enrichment of trace target drugs in complex matrix samples were achieved. In the first chapter, the principle and present situation of solid-phase extraction, hydrophilic resin and molecular imprinting technology are summarized, and the research progress and development prospect of hydrophilic molecularly imprinted resin are emphatically introduced. In the second chapter, the hydrophilic imprinted resin MIPFMRA was prepared by using low eutectic solvent as the reaction solvent, and the preparation parameters were optimized. The optimized MIPFMR was used as an adsorbent for solid phase extraction and a new method for the rapid separation and determination of agonist drug residues in urine samples was established. The average recoveries of clopramine hydrochloride and bambuterol hydrochloride were 91.7-100.1% and 鈮，

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