Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Qilu University of Technology (Shandong Academy of Sciences), 19 Keyuan Street, Jinan 250014, China.
College of Food Science and Engineering, Shandong Agricultural University, Taian 270018, China.
Anal Chim Acta. 2018 Feb 25;1001:179-188. doi: 10.1016/j.aca.2017.12.001. Epub 2017 Dec 14.
New imine-linked molecularly imprinted covalent organic frameworks (MICOFs) were successfully prepared, using fenvalerate as the dummy template. Schiff base reaction between 1,3,5-tris(4-aminophenyl)benzene and 1,3,5-triformylphloroglucinol was rapidly achieved at room temperature, using Sc(OTf) as the catalyst. The surface groups and morphologies of MICOFs were assessed by Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller surface area analysis, and scanning electron microscopy. The MICOFs exhibited high selectivity toward four structurally similar cyano pyrethroids, including fenvalerate, flucythrinate, β-cyfluthrin and λ-cyhalothrin. A method based on solid phase extraction using MICOFs coupled to high performance liquid chromatography was established for the determination of cyano pyrethroids in plant samples. Linearity in the range 0.1-200 ng g, with correlation coefficients of 0.9981-0.9993, was obtained for the four cyano pyrethroids. Detection limits and quantification limits were in the range 0.011-0.018 ng g and 0.036-0.060 ng g, respectively. Recoveries at three spiked levels ranged from 94.3% to 102.7%. The developed method is thus a promising technique for the selective extraction of cyano pyrethroids from complex matrices.
成功制备了新型亚胺键联的分子印迹共价有机框架（MICOFs），以氰戊菊酯为虚拟模板。使用 Sc(OTf) 作为催化剂，在室温下 1,3,5-三（4-氨基苯基）苯和 1,3,5-三（三氟甲酰基）间苯三酚之间迅速发生席夫碱反应。通过傅里叶变换红外光谱、Brunauer-Emmett-Teller 比表面积分析和扫描电子显微镜评估了 MICOFs 的表面基团和形态。MICOFs 对四种结构相似的氰基拟除虫菊酯（包括氰戊菊酯、氟氯氰菊酯、β-氯氟氰菊酯和 λ-氯氰菊酯）表现出高选择性。建立了一种基于固相萃取结合高效液相色谱法的方法，用于测定植物样品中的氰基拟除虫菊酯。四种氰基拟除虫菊酯在 0.1-200ng g 范围内具有线性关系，相关系数为 0.9981-0.9993。检测限和定量限分别为 0.011-0.018ng g 和 0.036-0.060ng g。在三个加标水平下的回收率范围为 94.3%-102.7%。因此，该方法是一种从复杂基质中选择性提取氰基拟除虫菊酯的有前途的技术。
