He Yahui, Tan Sijia, Abd Ei-Aty A M, Hacımüftüoğlu Ahmet, She Yongxin
Beijing Technology and Business University 100048 P. R. China
Institute of Quality Standards & Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences Beijing 100081 P. R. China
RSC Adv. 2019 Sep 23;9(51):29998-30006. doi: 10.1039/c9ra05782j. eCollection 2019 Sep 18.
A method for dummy molecular imprinting-magnetic dispersive solid-phase extraction (MI-MDSPE) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the selective determination of aminopyralid in milk. The magnetic material and polymers were combined a series of modifications in FeO. FeO@SiO-NH@MIP, FeO@SiO-COOH@MIP and two types of aminopyralid-specific magnetic molecularly imprinted polymers (MMIPs) were prepared on the surface of magnetic nanoparticles modified with amino and carboxyl groups. The morphology and magnetic properties of the polymer were characterized. FeO@SiO-NH@MIP exhibits not only good dispersibility and magnetic properties, but also an outstanding recognition pattern to the target analyte. Adsorption experiments demonstrated that FeO@SiO-NH@MIP, with a high specific surface area and fast mass transfer rate, had a higher affinity than FeO@SiO-COOH@MIP towards aminopyralid. Under the optimized MI-MDSPE conditions, the method had good linearity ( > 0.9972), excellent recoveries (83.3-90%), and good precision (relative standard deviations (RSDs) < 12.6%). This method has limits of detection (LOD) and quantification (LOQ) of 0.231 and 0.77 μg kg, respectively, indicating that these MMIPs can be used to analyse trace levels of aminopyralid in real samples.
建立了一种用于牛奶中氨氯吡啶酸选择性测定的虚拟分子印迹-磁性分散固相萃取(MI-MDSPE)结合液相色谱-串联质谱(LC-MS/MS)的方法。将磁性材料与聚合物相结合,对FeO进行了一系列修饰。在氨基和羧基修饰的磁性纳米颗粒表面制备了FeO@SiO-NH@MIP、FeO@SiO-COOH@MIP和两种氨氯吡啶酸特异性磁性分子印迹聚合物(MMIPs)。对聚合物的形态和磁性进行了表征。FeO@SiO-NH@MIP不仅具有良好的分散性和磁性,而且对目标分析物具有出色的识别模式。吸附实验表明,具有高比表面积和快速传质速率的FeO@SiO-NH@MIP对氨氯吡啶酸的亲和力高于FeO@SiO-COOH@MIP。在优化的MI-MDSPE条件下,该方法具有良好的线性(>0.9972)、出色的回收率(83.3-90%)和良好的精密度(相对标准偏差(RSDs)<12.6%)。该方法的检测限(LOD)和定量限(LOQ)分别为0.231和0.77μg kg,表明这些MMIPs可用于分析实际样品中痕量的氨氯吡啶酸。