酚醛印跡樹脂制備及痕量組分萃取分離方法研究
發(fā)布時間:2018-04-20 07:46
本文選題:親水樹脂 + 分子印跡 ; 參考:《河北大學》2017年碩士論文
【摘要】:近年來隨著食品藥品安全問題日益突出,生物樣品中低濃度藥物組分的準確、快速和定量檢測成為藥物分析領域的熱點和難點。由于樣品基質復雜,需要對其進行前處理后才能用于檢測。在眾多的樣品前處理方法中,固相萃取因具有操作簡單、省時、高效、有機試劑用量少等優(yōu)點而被廣泛應用于生物、醫(yī)藥、食品等多個領域。固相萃取的核心是吸附劑的選擇,分子印跡聚合物由于其高特異選擇性和實用性的特點被廣泛用作固相萃取吸附劑,但其仍存在一定局限性。針對傳統(tǒng)分子印跡聚合物水相識別性能差、功能單體與交聯(lián)劑種類較為單一等問題,本文開發(fā)了兩種新型親水印跡樹脂材料,并結合固相萃取技術,實現(xiàn)了復雜基質樣品中痕量目標藥物的快速分離和富集。第一章,概述了固相萃取技術、親水樹脂與分子印跡技術的原理與現(xiàn)狀,重點介紹了親水分子印跡樹脂的研究進展及發(fā)展前景。第二章,采用低共熔溶劑為反應溶劑,制備了間苯三酚 甲醛 三聚氰胺親水印跡樹脂(MIPFMR),優(yōu)化了制備過程中的參數(shù)。將優(yōu)化后的MIPFMR作為固相萃取的吸附劑,建立了準確、快速分離檢測尿樣中激動劑藥物殘留的新方法,對鹽酸氯丙那林與鹽酸班布特羅的平均回收率在91.7-100.1%的范圍內(RSD≤7.6%)。第三章,制備了3-氨基苯酚 烏洛托品親水印跡樹脂(MIAPH),對制備過程中的參數(shù)進行了優(yōu)化,將優(yōu)化好的MIAPH應用于固相萃取 高效液相色譜法,實現(xiàn)了對豆芽樣品中植物激素的選擇性萃取,并應用于市售豆芽樣品,檢測到了6-芐基腺嘌呤的殘留,濃度為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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