分子印迹—固相微萃取萃取头的制备及在食品中雌激素的分析应用

发布时间：2018-07-04 11:58

本文选题：名义模板 + 分子印迹聚合物　；参考：《南京医科大学》2012年硕士论文

【摘要】：本文制备了用于分离富集雌激素的分子印迹-固相微萃取萃取头,结合高效液相色谱测定食品中微痕量雌激素。该分子印迹-固相微萃取萃取头以石英纤维为基底。通过化学合成的方法,合成雌激素的结构类似物17-乙基雌二醇,并将其作为名义模板,解决了传统分子印迹中存在的模板泄漏衍生出的定量不准确的问题。采用分子模拟技术对功能单体及致孔剂进行了优选,选择三氟甲基丙烯酸-丙烯酸(摩尔比=1：1)为混合功能单体,提高了印迹涂层的吸附容量和选择性。扫描电镜显示萃取头的涂层表面均匀致密。采用Freundlich等温吸附方程对印迹涂层吸附位点的均质性和吸附性能进行评价,试验表明该萃取头具有较高的吸附能力及选择性；动力学试验表明其具有较快的吸附和解吸动力学特性。结合分子印迹固相微萃取和高效液相色谱,建立了奶粉中雌激素含量测定的方法。该方法的检测限范围为0.83-2.5ng mL-1,回收率分别为86-92%(E1)、88-97%(E2)、90-93%(E3)、95-99%(EE),RSD6.7%。此方法具有较低的检测限、较高的准确度及较好的精确度,并具有操作简单,快速高效的优点。
[Abstract]:In this paper, a molecularly imprinted solid phase microextractor for the separation and enrichment of estrogens was prepared, and a high performance liquid chromatography (HPLC) method for the determination of trace estrogens in food was developed. The molecular imprinting-solid phase microextraction head is based on quartz fiber. 17 ethylestradiol, a structural analogue of estrogen, was synthesized by chemical synthesis and used as a nominal template to solve the problem of quantitative inaccuracy derived from the leakage of template in traditional molecular imprinting. The adsorption capacity and selectivity of the imprinted coatings were improved by using molecular simulation technique to select functional monomers and pore-causing agents, and 1: 1 molar ratio of trifluoromethacrylic acid to acrylic acid was selected as the mixed functional monomers to improve the adsorption capacity and selectivity of the imprinted coatings. Scanning electron microscopy showed that the coating surface of the extractor was uniform and compact. Freundlich isothermal adsorption equation was used to evaluate the homogeneity and adsorption performance of the imprinted coating. The results showed that the extraction head had high adsorption ability and selectivity. The kinetic tests show that it has fast adsorption and desorption kinetics. A method for the determination of estrogen in milk powder by molecular imprinted solid phase microextraction and high performance liquid chromatography was established. The detection limit of this method is 0.83-2.5ng mL-1, and the recoveries are 86-92% (E1), 88-97% (E2), 90-93% (E3), 95-99% (EE), respectively. This method has the advantages of lower detection limit, higher accuracy and better accuracy, and has the advantages of simple operation, fast and efficient operation.
【学位授予单位】：南京医科大学
【学位级别】：硕士
【学位授予年份】：2012
【分类号】：R155.5

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