氟喹诺酮类分子印迹材料的制备及其性能研究

发布时间：2018-05-19 04:33

本文选题：加替沙星 + 氧氟沙星　；参考：《宁夏大学》2017年硕士论文

【摘要】：本论文分别以氟喹诺酮类抗生素中的加替沙星(GTFX)和氧氟沙星(OFLX)为模板分子,制得了 4种分子印迹聚合物。利用紫外分光光度计对分子印迹聚合物的吸附性能进行了详细考察。将其作为吸附剂,结合高效液相色谱(HPLC)分析,可用于牛奶、湖水、牛血清样品中GTFX、OFLX的分离富集与分析测定。主要工作如下:1.在甲醇-乙腈(1:1,V/V)混合溶液中,基于单分散交联聚甲基丙烯酸环氧丙酯(PGMA/EDMA)微球,以GTFX为模板分子,甲基丙烯酸(MAA)为功能单体,制得加替沙星表面分子印迹聚合物(MIP/GMA/EDMA)。利用紫外分光光度计研究了 GTFX与MAA的相互作用。通过静态吸附实验考察了MIP/PGMA/EDMA对GTFX的吸附容量和选择性吸附能力,利用Scathard曲线计算了最大表观吸附量和离解常数;通过动态吸附实验考察了 MIP/PGMA/EDMA对GTFX的吸附速率,利用动力学方程分析了其动力学行为。将该MIP/PGMA/EDMA制成分子印迹固相萃取(MIP-SPE)柱,考察其重复使用性能。结合HPLC分析,建立了一种分离、检测牛奶和湖水中GTFX的方法。2.采用共沉淀法合成Fe3O4纳米粒子,利用溶胶-凝胶技术在Fe3O4表面包覆SiO2,随后引入双键得到Fe3O4@SiO2-MPS。以此为载体,GTFX为模板分子,制得加替沙星磁性表面分子印迹聚合物(M-MIPs)。用透射电镜(TEM)、X射线衍射分析(XRD)、磁化强度分析(VSM)等手段对各步磁性粒子进行了表征。通过吸附实验考察了 M-MIPs对GTFX的吸附性能。将该M-MIPs作为吸附剂,结合HPLC分析,用于分离、检测牛奶中的GTFX。3.利用紫外分光光度计分析模板分子OFLX与两种功能单体MAA和4-乙烯基吡啶(4-VP)的结合情况,确定了最佳功能单体;选取OFLX与最佳功能单体的摩尔比为1:4、1:6、1:8和1:10,分别制备印迹聚合物和非印迹聚合物,通过对比吸附量和印迹因子,确定了最佳制备比例。采用沉淀聚合法,以50 mL甲醇-水(9:1,V/V)混合溶液为溶剂,制得氧氟沙星限进介质分子印迹聚合物(RAM-MIPs)。选取GTFX、恩诺沙星(ENRO)和磺胺甲基嘧啶(SMR)作为竞争分子,考察了 RAM-MIPs对OFLX的选择性吸附性能。选取牛血清白蛋白(BSA)作为模型蛋白,考察了 RAM-MIPs对蛋白质大分子的排阻能力。将该RAM-MIPs制成MIP-SPE柱,考察其循环使用性能;与HPLC联用,用于净化、萃取和检测牛奶中的OFLX。4.以5.0 μm硅胶为载体,OFLX为模板分子,MAA为功能单体,甲基丙烯酸缩水甘油酯(GMA)为亲水性功能单体,采用表面原子转移自由基技术(SI-ATRP),制得硅胶表面氧氟沙星限进介质分子印迹聚合物(Sil-RAM-MIPs)。利用Scatchard模型评价Sil-RAM-MIPs对OFLX的结合特性;利用Langmuir和Freundlich等温模型分析Sil-RAM-MIPs对OFLX的吸附行为。结合固相萃取技术,考察了 Sil-RAM-MIPs对BSA的排阻效果,并将其用于分析牛血清样品中的OFLX。
[Abstract]:In this paper, four molecularly imprinted polymers were prepared using gatifloxacin (GTFX) and ofloxacin (OFLX) as template molecules in fluoroquinolones. The adsorption properties of molecularly imprinted polymers were investigated by UV spectrophotometer. It can be used for the separation, enrichment and determination of GTFX OFLX in milk, lake water and bovine serum samples by high performance liquid chromatography (HPLC). The main work is as follows: 1. In methanol-acetonitrile (1: 1 / 1 V / V) solution, a molecularly imprinted polymer (MIP / GMA / EDMAA) on the surface of gatifloxacin was prepared on the basis of monodisperse crosslinked poly (propyl methacrylate) (PGMA / EDMA) microspheres, using GTFX as template molecule and MAA as functional monomer. The interaction between GTFX and MAA was studied by UV spectrophotometer. The adsorption capacity and selective adsorption capacity of MIP/PGMA/EDMA to GTFX were investigated by static adsorption experiment, the maximum apparent adsorption capacity and dissociation constant were calculated by Scathard curve, and the adsorption rate of MIP/PGMA/EDMA on GTFX was investigated by dynamic adsorption experiment. The dynamic behavior is analyzed by using the kinetic equation. The MIP-SPE column was prepared by molecularly imprinted solid phase extraction (MIP-SPE). A method for the separation and detection of GTFX in milk and lake water was established by HPLC analysis. Fe3O4 nanoparticles were synthesized by coprecipitation method. Sio _ 2 was coated on the surface of Fe3O4 by sol-gel technique, and then Fe _ 3O _ 4 @ Sio _ 2-MPS was obtained by introducing double bonds. The gatifloxacin magnetic surface molecularly imprinted polymer (M-MIPsN) was prepared by using GTFX as the template molecule. The magnetic particles were characterized by means of transmission electron microscopy (TEM) and X-ray diffraction (XRD), and magnetization analysis (VSM). The adsorption properties of M-MIPs to GTFX were investigated by adsorption experiments. The M-MIPs was used as an adsorbent for the separation and detection of GTFX. 3. 3 in milk by HPLC analysis. The combination of template molecule OFLX with two functional monomers MAA and 4-vinylpyridine 4-VPwas analyzed by UV spectrophotometer and the best functional monomer was determined. The molar ratio of OFLX to the best functional monomer was 1: 4: 1: 6: 8 and 1: 10, respectively. The imprinted polymer and non-imprinted polymer were prepared respectively. The optimum preparation ratio was determined by comparing the adsorption amount and the imprinting factor. A molecular imprinted polymer (RAM-MIPsN) of ofloxacin was prepared by precipitation polymerization with 50 mL methanol-water (9: 1 V / V) mixed solution as solvent. GTFX, enrofloxacin enro and sulfamethylpyrimidine (SMR) were selected as competitive molecules to investigate the selective adsorption of OFLX by RAM-MIPs. Bovine Serum Albumin (BSA) was selected as model protein to investigate the resistance of RAM-MIPs to protein macromolecules. The RAM-MIPs was prepared into a MIP-SPE column to investigate its recycling performance, and was combined with HPLC for purification, extraction and detection of OFLX. 4 in milk. Using 5.0 渭 m silica gel as carrier, OFLX as functional monomer, glycidyl methacrylate (GMAA) as hydrophilic functional monomer, surface atom transfer radical technique was used to prepare silica gel surface ofloxacin molecular imprinted polymer, Sil-RAM-MIPs. Scatchard model was used to evaluate the binding characteristics of Sil-RAM-MIPs to OFLX, and Langmuir and Freundlich isothermal models were used to analyze the adsorption behavior of Sil-RAM-MIPs to OFLX. Combined with solid phase extraction (SPE) technique, the inhibition effect of Sil-RAM-MIPs on BSA was investigated and used for the analysis of OFLX in bovine serum samples.
【学位授予单位】：宁夏大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O631.3;O652

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