School of Chemistry and Environmental Engineering, Wuhan Institute of Technology, Wuhan, 430205, China.
School of Pharmacy, Health Science Centre, Xi'an Jiaotong University, Xi'an, 710061, China.
Mikrochim Acta. 2019 May 31;186(6):393. doi: 10.1007/s00604-019-3513-7.
A hybrid material was synthesized by growing a covalent organic framework (COF) in-situ on the surface of functionalized metal organic framework (MOF). Specifically, the amino-modified MOF (type MIL-68) was obtained by reacting indium(III) nitrate and 2-aminoterephthalic acid. Subsequently, it was reacted with tris(4-formylphenyl)amine and tris(4-aminophenyl)amine to obtain the final hybrid COF. This material overcomes the disadvantage of MOF concerning poor stability in aqueous solution and it combines the advantages of MOF and COF. This MOF@COF hybrid material is shown to be a viable adsorbent for the extraction of sulfonamides by pipette tip solid-phase extraction). Following elution with acetonitrile, the sulfonamides were quantified by high performance liquid chromatography using variable wavelength detection (HPLC-VWD). The structure and morphology of the material was characterized by various techniques. Extraction parameters such as amount of adsorbent, sampling rate, sample pH, elution solvent and sample volume were investigated. Under the optimum conditions, the sulfonamides tested (sulfadimethoxine sulfamethoxazole, sulfamonomethoxine, sulfamethazine, sulfamerazine and sulfadiazine) can be determined over a wide linear range (10-2000 ng·mL), with low limits of detection (1 ng·mL) and high precision (RSD <5.2%). The method was applied the determination of sulfonamide residues in (spiked) environmental water, milk and meat samples and gave recoveries in the range from 68.9-103.8%, with RSDs of <6.6%. The packed pipette tip column exhibits excellent stability, reproducibility and high adsorption capacity. Graphical abstract A hybrid sorbent was prepared by controlled growth of a covalent organic framework on amino-modified MIL-68 and packed into a pipette tip for sulfonamide extraction. The sensitivity was dramatically increased after optimized extraction, with limit of detection as low as 1 ng·mL.
一种杂化材料是通过在功能化金属有机骨架（MOF）表面原位生长共价有机骨架（COF）合成的。具体而言，通过三（4-醛基苯基）胺和三（4-氨基苯基）胺与氨基修饰的 MOF（类型 MIL-68）反应，得到最终的杂化 COF。该材料克服了 MOF 在水溶液中稳定性差的缺点，并结合了 MOF 和 COF 的优点。这种 MOF@COF 杂化材料被证明是一种可行的萃取磺胺类药物的萃取剂。用乙腈洗脱后，用高效液相色谱法（HPLC-VWD）用可变波长检测法（HPLC-VWD）定量测定磺胺类药物。通过各种技术对材料的结构和形态进行了表征。研究了萃取参数，如吸附剂的量、采样速度、样品 pH 值、洗脱溶剂和样品体积。在最佳条件下，所测试的磺胺类药物（磺胺二甲氧嘧啶、磺胺甲恶唑、磺胺甲噁唑、磺胺间甲氧嘧啶和磺胺嘧啶）可在较宽的线性范围内（10-2000ng·mL）进行测定，检测限低（1ng·mL），精密度高（RSD<5.2%）。该方法应用于（加标）环境水、牛奶和肉类样品中磺胺类药物残留的测定，回收率在 68.9-103.8%之间，RSD<6.6%。填充的微量进样器柱具有良好的稳定性、重现性和高吸附容量。
