烯唑醇分子印迹固相萃取膜的制备及其应用

Preparation and Application of a Molecularly Imprinted Solid-phase Extraction Membrane with High Selectivity to Diniconazole

摘要:

以烯唑醇为模板分子，丙烯酰胺(AM)为功能单体，采用原位聚合法制备出对烯唑醇具有高选择性的分子印迹固相萃取膜；通过紫外光谱试验优化了功能单体，考察了不同功能单体与模板分子的结合能力，同时考察了制备印迹膜时致孔剂的选择和分子印迹膜印迹次数对液体通过性的影响；建立了基于分子印迹固相萃取膜-高效液相色谱法测定粮谷中烯唑醇残留的方法。结果表明，与功能单体α-甲基丙烯酸(MAA)相比，丙烯酰胺(AM)与烯唑醇的结合能力更强，以乙腈为制孔剂制备烯唑醇印迹膜，印迹一次印迹膜较稳定，且液体通透性良好。烯唑醇在0.5~15 μg/mL浓度范围内有良好的线性关系（r=0.9987），平均回收率在80.34%~87.03%之间，检出限为2.0 μg/g。该方法选择性强、灵敏、可靠，适用于粮谷等复杂基质中烯唑醇的残留检测。

Abstract:

Molecularly-imprinted, solid-phase extraction membrane with high selectivity to diniconazole was prepared by in situ polymerization using diniconazole as the template molecule and acrylamide (AM) as the functional monomer. AM was optimized and the binding ability of different functional monomers with the template molecule was investigated by ultraviolet (UV) spectroscopy. This property was also used to select porogens for preparation of molecularly imprinted membrane and the influence of imprinting time on liquid permeability. A method based on molecularly imprinted, solid-phase membrane, high-performance liquid chromatographic was developed for the determination of diniconazole residues in grains. The results showed that compared with the functional monomer α-methacrylic acid (MAA), AM showed a stronger binding capacity to diniconazole. When the molecularly-imprinted diniconazole membrane was prepared using acetonitrile as the porogen, the once-imprinted membrane was stable with a good liquid permeability. A good linear range of diniconazole was obtained in the range of 0.5~15 μg/mL (r = 0.9987). The average recoveries ranged from 80.34% to 87.03%, and the detection limit of diniconazole was 2.0 μg/g. Thus, the method developed in this study is highly selective, sensitive, and reliable, which can be applied for determination of diniconazole residues in grain and other complex matrices.