School of Food and Biological Engineering, Shaanxi University of Science and Technology, Xi'an, 710021, China.
Key Laboratory of Life-Organic Analysis of Shandong Province, Qufu Normal 13 University, Qufu, 273165, China.
Mikrochim Acta. 2020 Apr 20;187(5):278. doi: 10.1007/s00604-020-04257-z.
β-Cyclodextrin-functionalized magnetic covalent organic framework (FeO@COF@Au-β-CD) was developed as sorbent for magnetic solid phase extraction of trace sulfonamides in meat samples prior to HPLC-MS/MS analysis. The sorbent was synthesized by loading gold nanoparticles onto a FeO@COF surface and then functionalized by thiolated-β-cyclodextrin immobilization via Au-S bonding formation. The prepared composite material was employed for sulfonamides extraction. The main parameters were optimized to obtain the best extraction efficiency. The experiments of adsorption kinetics were carried out to investigate the adsorption mechanism. Results showed the pseudo-second-order kinetic was better fitted with the adsorption kinetics of sulfonamides. Under optimized conditions, the magnetic solid phase extraction-HPLC method showed good linearity (R ≥ 0.9936), and the limits of detection were in the range of 0.8-1.6 μg kg. The proposed method was successfully used for quantitation of sulfonamides in real samples. The recoveries ranged from 78.9 to 112.0% with relative standard deviations (RSDs) < 10% (n = 5). The proposed method exhibited great potential for enrichment and determination of sulfonamides in many other food or environment samples. Graphical abstract.
β-环糊精功能化磁性共价有机框架（FeO@COF@Au-β-CD）被开发为用于 HPLC-MS/MS 分析之前从肉样中萃取痕量磺胺类药物的磁性固相萃取剂。该吸附剂是通过在 FeO@COF 表面负载金纳米粒子，然后通过 Au-S 键形成将巯基-β-环糊精固定化来合成的。将制备的复合材料用于磺胺类药物的萃取。优化了主要参数以获得最佳的萃取效率。进行了吸附动力学实验以研究吸附机制。结果表明，磺胺类药物的吸附动力学更符合拟二级动力学。在优化条件下，磁固相萃取-HPLC 法具有良好的线性（R≥0.9936），检出限在 0.8-1.6μg kg 范围内。该方法成功用于实际样品中磺胺类药物的定量。回收率在 78.9%至 112.0%之间，相对标准偏差（RSD）<10%（n=5）。该方法在富集和测定许多其他食品或环境样品中的磺胺类药物方面具有很大的潜力。
