题名均一分子印迹聚合物微球的制备及在兽药残留检测中的应用研究
作者寇星
学位类别硕士
答辩日期2011-06-02
授予单位中国科学院研究生院
导师雷建都 ; 马光辉
关键词分子印迹聚合物 微球 快速膜乳化 沉淀聚合 红霉素 氯霉素
其他题名Preparation of Uniform Molecularly Imprinted microspheres and their Application in Detection of Veterinary Drug Residues
学位专业生物化工
中文摘要分子印迹技术能够针对目标分子制备具有特异选择性的聚合物,制得的聚合物称为分子印迹聚合物(Molecularly Imprinted Polymers, MIPs)。由于MIPs具有高的选择性,已广泛应用于药物分离、食品与环境检测、抗体或受体模拟、传感器等诸多领域。目前,MIPs的制备方法多采用本体聚合法和悬浮聚合法。这两种方法获得的MIPs主要用作固相萃取介质和色谱固定相,粒径较大且不均一、重复性不好,难以满足较高的应用要求(如超高效液相色谱介质、传感器材料等)。本论文采用沉淀聚合法和快速膜乳化法这两种方法来制备粒径均一的亚微米级球形分子印迹聚合物,分别以兽药红霉素(Erythromycin, EM)和氯霉素(Chloroamphenicol, CAP)为模板分子,制备得到了粒径均一的红霉素和氯霉素分子印迹聚合物微球。主要研究工作包括: 1. 沉淀聚合法制备红霉素分子印迹聚合物微球 以红霉素为模板分子、甲基丙烯酸为功能单体、乙二醇二甲基丙烯酸酯为交联剂,采用沉淀聚合法制备了粒径均一的亚微米级红霉素分子印迹聚合物微球,优化了分子印迹聚合物微球的合成条件,确定了模板分子、功能单体和交联剂的最佳摩尔比为1:3:3。红霉素分子印迹聚合物微球的表征结果表明,其粒径在400~600 nm之间,比表面积为243.66 m2 g-1,孔径为4.448 nm,理论最大吸附量可达到194.81 mg g-1,远高于文献报道,如Song等采用本体聚合法制备出红霉素分子印迹聚合物印迹红霉素,其理论最大表观吸附量只达到72.09 mg g-1。微球吸附红霉素在约200 min时达到平衡。制备得到的红霉素分子印迹聚合物微球具有好的选择性吸附能力。 2. 快速膜乳化法制备氯霉素分子印迹聚合物微球 以氯霉素为模板分子、甲基丙烯酸为功能单体、乙二醇二甲基丙烯酸酯为交联剂,采用快速膜乳化法制备了粒径均一的亚微米级氯霉素分子印迹聚合物微球,优化了氯霉素分子印迹聚合物微球的合成条件:当膜孔径为1.4 μm,膜压为2 MPa,过膜次数为5次,聚乙烯醇(PVA)在水中浓度为1.5%,油水体积比为1:20时,制备得到聚合物微球的粒径最均一。微球的表征结果表明,其粒径在300~800 nm之间,理论最大吸附量可达到121.88 mg g-1,远高于文献报道,如王荣艳等人采用本体聚合法制备出氯霉素分子印迹聚合物微球印迹氯霉素,其理论最大表观吸附量只达到4.670 mg g-1。微球对氯霉素的吸附可在约60 min时达到平衡。氯霉素分子印迹聚合物微球具有好的选择性吸附能力。
英文摘要Molecular imprinting technology can prepare polymers materials with specific selectivity for the target molecule. The obtained polymers materials are called molecularly imprinted polymers (MIPs). Since MIPs possess high selectivity, they have been widely used in drug separation, food and environmental testing, antibody or receptor analog, sensors and many other areas. Currently, MIPs were mainly prepared by bulk polymerization and suspension polymerization. The MIPs obtained by the two methods generally were used for solid phase extraction media and chromatographic stationary phase. Nevertheless, their sizes were relatively large, non-uniform, with poor repeatability, and difficult to meet higher application requirements such as ultra-high performance liquid chromatography media, sensor materials. In this paper, we utilized two methods, precipitation polymerization and premix membrane emulsification technique, to prepare the uniform MIPs microsphers with submicron size for erythromycin (EM) and chloramphenicol (CAP), respectively. The main works are shown as the follows: 1. Preparation of MIPs microspheres for EM with precipitation polymerization Uniformly MIPs microsphers for EM with submicron size were prepared by precipitation polymerization using EM as a template molecule, methacrylic acid (MAA) as functional monomer and ethyleneglycol dimethacrylate (EGDMA) as a cross-linker. The synthesis condition of MIPs microspheres was optimized. The optimum molar ratio of EM, MAA and EGDMA was 1:3:3. The molecularly imprinted microspheres prepared for EM were uniform with the size between 400~600 nm, the specific surface area was 243.66 m2 g-1, the pore size was 4.448 nm, the maximum apparent adsorption capacity of MIPs microspheres was 194.81 mg g-1, much higher than that reported in the literature, for example, the molecular imprinted polymer for EM used to imprint EM was prepared by Song using bulk polymerization, its maximum apparent adsorption capacity was only 72.09 mg g-1. The adsorption equilibrium time was around 200 min. The results of the selective adsorption experiments suggested that the MIPs microsphers for EM possessed high selectivity adsorption capacity. 2. Preparation of MIPs microspheres for CAP using premix membrane emulsification technique Uniformly submicron MIPs microspheres with submicron size for CAP were prepared by premix membrane emulsification technique using CAP as a template molecule, MAA as a functional monomer and EGDMA as a cross-linker. The synthesis condition of MIPs microspheres was optimized: when the membrane pore size was 1.4 μm, transmembrane pressure was 2 MPa, transmembrane passes were 5 times, the concentration of polyvinyl alcohol (PVA) in the water phase was 1.5%, the volume ratios of oil to the water phase was 1:20, the size of the microspheres prepared were most uniform. The molecularly imprinted microspheres obtained for CAP were uniform spheres with the size between 300~800 nm, the maximum apparent adsorption capacity of MIPs microspheres was 121.88 mg g-1, much higher than that reported in the literature, for example, the molecular imprinted polymer for CAP used to imprint CAP was prepared by Wang using bulk polymerization, its maximum apparent adsorption capacity was only 4.670 mg g-1. The adsorption equilibrium time was around 60 min. The results of the selective adsorption experiments of the MIPs microspheres for CAP indicated that the MIPs microspheres for CAP had high selectivity adsorption capacity.
语种中文
公开日期2013-09-23
页码70
内容类型学位论文
源URL[http://ir.ipe.ac.cn/handle/122111/1681]  
专题过程工程研究所_研究所(批量导入)
推荐引用方式
GB/T 7714
寇星. 均一分子印迹聚合物微球的制备及在兽药残留检测中的应用研究[D]. 中国科学院研究生院. 2011.
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