2-甲氧基雌二醇限进介质分子印迹聚合物的制备及应用

发布时间：2019-01-11 19:18

【摘要】：限进介质分子印迹聚合物具有较高的选择性、亲水性、稳定性等优点，已成为分析工作者关注的热点，在药物传递系统、食品、药品及环境监测等领域中具有良好的应用前景。本研究采用沉淀聚合法制备了2-甲氧基雌二醇（2-ME）限进介质分子印迹聚合物，该聚合物对2-ME具有良好的特异性识别同时可避免蛋白的不可逆吸附。将其作为固相萃取填料，在复杂生物样品中2-ME的专属分析和检测中可发挥重要作用。主要研究内容摘要如下： 1.2-ME限进介质分子印迹聚合物的制备及评价本研究采用17β-雌二醇为伪模板分子，以沉淀聚合法制备2-ME限进介质分子印迹聚合物避免了模板渗漏对痕量分析的影响，并对制备条件进行了优化。以傅立叶红外光谱、扫描电子显微镜、热重分析仪及激光纳米粒度仪对聚合物进行表征。实验考察了聚合物对2-ME的吸附选择性及蛋白吸附能力，并以等温吸附法测定聚合物吸附特性，以Scatchard模型对等温吸附曲线进行拟合。本研究制备的聚合物呈微球状结构、具有良好的亲水性，能明显减少蛋白的不可逆吸附，并对2-ME具有特异性识别能力。 2.限进介质分子印迹聚合物固相萃取-高效液相色谱联用分析血浆中2-ME 本研究以限进介质分子印迹聚合物为固相萃取填料，通过固相萃取-高效液相色谱联用技术，建立了特异性强、回收率高的血浆样品2-ME分析新方法。方法检测限为0.02μg/ml，，线性范围为0.06-20μg/ml，日内精密度为2.9%-9.3%，日间精密度为3.5%-11.9%，回收率为99.10%-101.00%。该方法应用于2-甲氧基雌二醇血浆样品的分析，所得结果较满意。为建立快速、有效、专属的复杂生物样品检测方法奠定了基础。 3.限进介质分子印迹聚合物整体柱的制备及应用本研究采用原位聚合法制备了限进介质分子印迹整体柱。考察了整体柱蛋白吸附性及选择性。将制备的整体柱应用于血浆中2-ME的在线萃取、富集。结果表明，该整体柱能在线去除生物样品中大分子蛋白及干扰物质，同时对分析药物具有较好的保留，可实现血样中2-ME快速、便捷、有效的富集分析。
[Abstract]:Molecularly imprinted polymers (MIPs) with limited media have become the focus of attention due to their high selectivity, hydrophilicity and stability, and have a good application prospect in the fields of drug delivery system, food, medicine and environmental monitoring. In this study, 2-methoxyestradiol (2-ME) molecularly imprinted polymer was prepared by precipitation polymerization. The polymer has good specificity for 2-ME recognition and can avoid irreversible adsorption of protein. It can play an important role in the analysis and detection of 2-ME in complex biological samples. The main contents of this study are summarized as follows: preparation and evaluation of imprinted polymer with 1.2-ME as limiting medium in this study, 17 尾 -estradiol was used as pseudo-template molecule, and 17 尾 -estradiol was used as pseudo-template molecule. Molecular imprinted polymers with 2-ME limiting medium were prepared by precipitation polymerization to avoid the influence of template leakage on trace analysis and the preparation conditions were optimized. The polymer was characterized by Fourier transform infrared spectroscopy, scanning electron microscope, thermogravimetric analyzer and laser nanocrystalline analyzer. The adsorption selectivity and protein adsorption ability of polymer to 2-ME were investigated. The adsorption characteristics of polymer were measured by isothermal adsorption method. The isothermal adsorption curve was fitted by Scatchard model. The polymer prepared in this study has a microsphere structure, good hydrophilicity, can significantly reduce the irreversible adsorption of protein, and has a specific recognition ability to 2-ME. 2. Determination of 2-ME in Plasma by Solid-Phase extraction and High performance liquid Chromatography with Molecular imprinting Polymer as Solid-Phase extraction packing, the study was carried out by using solid-phase extraction-high performance liquid chromatography (HPLC), using molecularly imprinted polymer as solid phase extraction filler. A new method for 2-ME analysis of plasma samples with strong specificity and high recovery was established. The detection limit was 0.02 渭 g / ml, the linear range was 0.06-20 渭 g / ml, the intra-day precision was 2.9-9.3, and the daytime precision was 3.5-11.9.The recovery was 99.10-101.00. The method has been applied to the analysis of 2-methoxyestradiol plasma samples with satisfactory results. It lays a foundation for the establishment of a rapid, effective and exclusive method for the detection of complex biological samples. 3. Preparation and Application of molecularly imprinted Polymer monolithic column with confined medium in this study the molecular imprinted monolithic column was prepared by in-situ polymerization. The adsorption and selectivity of monolithic column protein were investigated. The prepared monolithic column was applied to the on-line extraction and enrichment of 2-ME in plasma. The results showed that the monolithic column could remove macromolecular proteins and interfering substances from biological samples on line, and had a good retention for the analysis of drugs, and could achieve rapid, convenient and effective enrichment and analysis of 2-ME in blood samples.
【学位授予单位】：郑州大学
【学位级别】：硕士
【学位授予年份】：2014
【分类号】：R943

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