拥挤试剂协助制备分子印迹材料及性能评价

发布时间：2018-03-13 03:09

本文选题：分子印迹聚合物　切入点：拥挤试剂　出处：《天津医科大学》2014年硕士论文　论文类型：学位论文

【摘要】：分子印迹是合成分子识别材料的新兴技术。分子拥挤技术是一种有效促进分子印迹效果的新方法,将大分子拥挤试剂应用于MIPs的药物传递系统具有较长远的研究前景。分子印迹技术在整体柱领域同样非常具有研究潜力,尤其是在合成材料方面需要不断发展新的功能单体,以满足合成特定结构模板MIPs的需要。本文的第一部分利用沉淀聚合法,以甲基丙烯酸为功能单体,二甲基丙烯酸乙二醇酯为交联剂,加入分子拥挤试剂聚苯乙烯的四氢呋喃为致孔剂,制备氨鲁米特分子印迹聚合物,用作药物的控缓释材料。经体外释放研究表明,与未加入聚苯乙烯的印迹聚合物比较,聚苯乙烯的加入明显增强了印迹聚合物对印迹分子的特异性识别性能,且具有明显的缓释效果,表明对氨鲁米特-甲基丙烯酸体系,存在明显的分子拥挤效应。通过平衡吸附试验,对比研究了加入拥挤试剂的MIPs和传统的MIPs的吸附性能,证明了加入拥挤试剂的分子印迹聚合物具有较强的吸附性能。通过释放模型对印迹和非印迹聚合物的释放曲线进行拟合比较,研究其释放机制。发现最佳拟合模型是零级模型,而不加PS体系不是零级释放。结果表明,分子拥挤试剂增强了聚合物的印迹效果,且释放机制为零级释放。本文的第二部分首次利用离子液体1-乙烯基-3-丁基咪唑氯盐作为功能单体,在极性溶剂为致孔剂条件下,利用原位热引发聚合法,以二甲基丙烯酸乙二醇酯为交联剂,甲醇、异辛烷及聚苯乙烯(PS)／四氢呋喃为致孔剂,一步反应合成酮洛芬分子印迹整体柱。系统考察了整体柱制备条件,如模板分子与功能单体的比例,功能单体与交联剂的比例,致孔剂中聚苯乙烯在四氢呋喃中的含量及聚苯乙烯的分子量和拥挤试剂种类变化等对整体柱印迹因子的影响。并结合扫描电镜、压汞及氮吸附形貌表征和高效液相色谱实验条件的考察,进一步证明了整体柱的印迹效果。模板与功能单体与交联剂的比例为1/4/20,分子量为35万的PS在THF中的含量为40mg/mL时,整体柱的印迹因子最大,可达2.297。结果证明离子液体1-乙烯基-3-丁基咪唑氯盐可作为新型的功能单体,在极性致孔剂甲醇条件下,合成具有印迹效果的分子印迹整体柱。
[Abstract]:Molecular imprinting is a new technology for the synthesis of molecular recognition materials. The application of macromolecular crowding reagents to the drug delivery system of MIPs has a long term prospect. Molecular imprinting technology also has great potential in the field of monolithic columns, especially in the synthesis of new functional monomers. To meet the needs of the synthesis of specific structure template MIPs. In the first part of this paper, using methacrylic acid as functional monomer, ethylene glycol dimethacrylate as crosslinking agent, tetrahydrofuran of polystyrene as molecular crowding reagent was added as pore-forming agent by precipitation polymerization. Amilomide molecularly imprinted polymer was prepared and used as a controlled and sustained release material for drugs. In vitro release studies showed that it was compared with imprinted polymers without polystyrene. The addition of polystyrene obviously enhanced the specific recognition performance of imprinted polymer to imprinted molecule, and had obvious slow-release effect, which indicated that the system of p-aminolunomide-methacrylic acid, By equilibrium adsorption test, the adsorption properties of MIPs and traditional MIPs were studied. It was proved that the molecularly imprinted polymer with crowding reagent had strong adsorption properties. The release mechanism of imprinted and non-imprinted polymers was studied by fitting and comparing the release curves of imprinted and non-imprinted polymers. It was found that the best fit model was a zero-order model. The results showed that the molecular crowding reagent enhanced the imprinting effect of the polymer, and the release mechanism was zero order release. In the second part of this paper, the ionic liquid 1-vinyl-3-#china_person0# imidazole chloride salt was used as the functional monomer for the first time, under the condition of polar solvent as the pore-forming agent, the in situ thermal initiation polymerization method was used, using dimethacrylate as crosslinking agent, methanol, Ketoprofen molecularly imprinted monolithic column was synthesized by one-step reaction of isooctane and polystyrene PSN / tetrahydrofuran as pore-forming agent. The preparation conditions of monolithic column, such as the ratio of template molecule to functional monomer and the ratio of functional monomer to crosslinking agent, were systematically investigated. The effects of the content of polystyrene in tetrahydrofuran, the molecular weight of polystyrene and the type of crowding reagent on the whole column imprinting factor were studied by SEM, SEM, SEM, SEM, SEM, SEM, SEM, SEM, SEM, SEM, SEM, SEM, SEM, SEM, SEM. The adsorption morphology of mercury and nitrogen and the experimental conditions of HPLC further proved the imprinting effect of the monolithic column. When the ratio of template to functional monomer to crosslinking agent was 1 / 4 / 20, the content of PS with molecular weight of 350,000 in THF was 40 mg / mL. The imprinting factor of the monolithic column was the highest, up to 2.297. The results showed that the ionic liquid 1-vinyl-3-#china_person0# imidazole chloride salt could be used as a new functional monomer to synthesize molecularly imprinted monolithic column with imprinting effect under the condition of methanol, a polar pore-inducing agent.
【学位授予单位】：天津医科大学
【学位级别】：硕士
【学位授予年份】：2014
【分类号】：R917

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