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目的:采用原位热引发聚合法制备分子印迹整体柱,在高效液相色谱上考察印迹整体柱在不同色谱条件下分子印迹整体柱选择性的变化。利用计量置换模型对实验数据进行模拟,研究决定分子印迹整体柱选择性识别能力的主要因素。方法:以甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,甲苯和异辛烷为致孔剂,偶氮二异丁腈为引发剂,选择原位热引发聚合法,制备以对-羟基苯甲酸为模板的分子印迹整体柱。在高效液相色谱上考察印迹整体柱对模板分子的特异选择性;系统考察了向流动相中依次加入水、甲醇、乙醇和异丙醇4种强氢键竞争溶剂后对-羟基苯甲酸、邻-羟基苯甲酸和对-硝基苯甲酸容量因子的变化,利用计量置换模型对实验数据进行模拟。结果:制得的分子印迹整体柱对模板分子具有特异选择性;在流动相中加入强氢键竞争溶剂后,各种样品的容量因子以及印迹整体柱的选择性均降低;计量置换模型模拟结果显示lnk值用来表示分子印迹聚合物的分离效率,n值用来表示当溶质和印迹聚合物间的相互作用是氢键时,被分离样品和印迹聚合物之间相互作用的空间效应。结论:当强氢键竞争性溶剂加入流动相中时印迹聚合物孔穴结构的匹配性决定了印迹体系的特异识别能力。
OBJECTIVE: To prepare the molecularly imprinted monolith using in-situ thermal polymerization. The selectivity of monolithic column under different chromatographic conditions was investigated by high performance liquid chromatography. The experimental data were simulated by metrological replacement model to study the main factors that determine the ability of molecularly imprinted monolith to selectively recognize monolithic column. Methods: With methacrylic acid as functional monomer, ethylene glycol dimethacrylate as crosslinking agent, toluene and isooctane as porogen and azobisisobutyronitrile as initiator, in situ thermal polymerization Method, the preparation of p-hydroxybenzoic acid as a template for molecularly imprinted monolithic column. The specific selectivity of the imprinted monolith on template molecules was investigated by high performance liquid chromatography. The effects of p-hydroxybenzoic acid, p-hydroxybenzoic acid, p-hydroxybenzoic acid and p- O-hydroxybenzoic acid and p-nitrobenzoic acid capacity factor changes, the use of metrological replacement model to simulate the experimental data. Results: The prepared molecularly imprinted monolithic column has specific selectivity to the template molecule. After adding strong hydrogen bond to the mobile phase, the capacity factor and the selectivity of the imprinted monolithic column were decreased. The simulation results The value of lnk is shown to indicate the separation efficiency of the molecularly imprinted polymer and the value of n is used to indicate the spatial effect of the interaction between the sample being separated and the imprinted polymer when the interaction between the solute and the imprinted polymer is hydrogen bonding. CONCLUSION: The matching of pore structure of imprinted polymer determines the specific recognition ability of imprinting system when a strong hydrogen bond competing solvent is added to the mobile phase.