【作者】 陆国栋；

【导师】 吕运开；

【作者基本信息】 河北大学 ， 分析化学， 2009， 硕士

【摘要】 利用溶胶-凝胶技术与分子印迹技术相结合的方法,在水相体系中制备氟喹诺酮类药物的分子印迹吸附材料,实现了水相体系中实际样品的选择性分离检测。详细考察了印迹吸附剂的合成条件和识别特性及其主要影响因素,通过Scatchard分析分别计算了其饱和吸附量和离解常数。发展了具有疏水作用、离子对作用的印迹方法和有机/无机互穿网络共聚分子印迹杂化材料的制备方法,并将洛美沙星分子印迹吸附材料用于固相萃取-高效液相色谱法测定牛奶中痕量洛美沙星残留量。全文分为如下四个部分：第一章：简要介绍了分子印迹技术和溶胶-凝胶技术的基本原理及溶胶-凝胶分子印迹技术在药物分离检测中的研究进展及展望。第二章：采溶用胶-凝胶法以诺氟沙星为模板,3-氨基丙基三乙氧基硅烷(APS)为功能单体,四乙氧基硅烷(TEOS)为交联剂,添加甲基三甲氧基硅烷(MTMS)增加其疏水性,制备印迹吸附材料。考察了MTMS用量、吸附体系的pH值对聚合物吸附量的影响。通过吸附实验考察聚合物的吸附能力,通过Scatchard分析,计算了聚合物的离解常数和饱和吸附容量,分别为：Kd1=27.2 mg/L (Qmax1=44.48 mg/g)和Kd2=124.1mg/L (Qmax2=46.44mg/g)。第三章：采用溶胶-凝胶法以洛美沙星为模板,APS为功能单体,MTMS为交联剂,调节反应体系pH值,以功能单体与模板分子的离子对作用方式,合成了印迹聚合物。红外光谱实验和静态吸附实验研究了印迹聚合物的材料性能和吸附特性。将制备的分子印迹聚合物,用于固相萃取柱填料,考察其萃取条件,并用于牛奶中的痕量洛美沙星的富集分离和液相色谱分析,平均回收率为71.1%。第四章：以甲基丙烯酰氧丙基三甲氧基硅烷与甲基丙烯酸为功能单体,氧氟沙星为印迹模板,四乙氧基硅烷为交联剂,AIBN为引发剂进行了有机-无机共聚合成研究,发展有机/无机互穿网络共聚分子印迹杂化材料的制备方法。研究了合成条件和印迹聚合物的吸附性能。通过Scatchard分析,计算了聚合物的离解常数和饱和吸附容量,分别为：Kd1=51.11mg/L (Qmax1=51.34 mg/g)和Kd2=159.02 mg/L (Qmax2=77.41 mg/g)。更多还原

【Abstract】 The aim of this dissertation is to develop the molecular imprinting polymers(MIPs) for 6the absorption of fluoroquinolones in the preparation of aqueous system by the combination of sol-gel technique and molecular imprinting technique, which is in order to facilitate selective analysis of the actual samples in the water-phase system. The MIPs recognition properties for the target molecule were investigated by the static adsorption experiments, the maximal adsorption capacity and dissociation constant were calculated by the Scatchard equation. The new imprinting method based on hydrophobic interaction and ion-pairing interaction between the functional monomer and the template molecule were developed, and the synthesis method of organic-inorganic imprinted polymer hybrids having interpenetrating polymer networks structure was investigated. The lomefloxacin-MIPs were used to solid-phase extraction for pre-concentration and determination the lomefloxacin in milk combined with high-performance liquid chromatography technique. The thesis includes four chapters as follows:Chapter one:A review mainly introduce the principle of sol-gel molecular imprinting technique, the application in drugs, the application in drug of quinolones, as well as the prospect of the sol-gel molecular imprinting technique.Chapter two:A novel molecularly imprinting polymer was synthesized by combining molecular imprinting technique and sol-gel process with norfloxacin as template, 3-aminopropyltriethoxysilane as functional monomer, and tetraethoxysilane as crosslinker, added methyltrimethoxysilane (MTMS) to increase hydrophobic interaction. The influence of MTMS and the pH of adsorption solution on recognition properties was investigated. The binding capacity was evaluated by static absorption experiment and Scatchard analysis,which showed that the dissociation constant (KD) and the maximum binding capacity(Qmax) were 124.1mg/L and 46.44 mg/g for high affinity binding site, and 27.2 mg/L and 44.48 mg/g for lower affinity binding site respectively.Chapter three:A molecularly imprinted solid-phase extraction sorbent was synthesized using lomefloxacin as template,3-aminopropyltriethoxysilane as functional monomer, and methyltrimethoxysilane as crosslinker, by sol-gel technique, adjust pH value of the reaction system, use ions pairing action to combine template and functional monomer. The reaction mechanism was reasoned by the infrared spectroscopy analysis, The adsorption capacity of the polymer was evaluated by the static absorption experiment. The lomefloxacin MIPs were used to solid-phase extraction for pre-concentration the rudimental lomefloxacin in milk, the average recovery was 71.1%.Chapter four:A novel organic-inorganic interpenetrating hybird sorbent was synthesized with ofloxacin as template methacryloxypropyltrimethoxysilane and methacrylic acid as functional monomer and tetraethoxysilane as crosslinker, azobisisbutyronitrile as initiator, the synthesis method of organic-inorganic imprinted polymer hybrids having interpenetrating polymer networks structure was developed. The binding capacity was evaluated by static adsorption experiment and Scatchard analysis,which showed that the dissociation constant(KD) and the maximum binding capacity(Qmax) were 51.11mg/L and 51.34mg/g for high affinity binding site, and 159.02 mg/L and 77.41 mg/g for lower affinity binding site,respectively.更多还原