Martínez-Pérez-Cejuela Héctor, Pravcová Kateřina, Česlová Lenka, Simó-Alfonso Ernesto F, Herrero-Martínez José Manuel
Department of Analytical Chemistry, University of Valencia, C/Dr. Moliner, 50, 46100, Burjassot, Valencia, Spain.
Department of Analytical Chemistry, Faculty of Chemical Technology, University of Pardubice, Studentská 573, 532 10, Pardubice, Czech Republic.
Mikrochim Acta. 2021 May 26;188(6):197. doi: 10.1007/s00604-021-04872-4.
A composite built with aminated zeolitic imidazolate framework and gold nanoparticles (AuNPs) for solid-phase extraction (SPE) of neonicotinoids in agricultural samples is presented. The composite was prepared through the assembly of AuNPs onto the surface of metal-organic framework based on the strong interaction between the amino group and AuNP. These metallic surfaces provided additional interactions based on the affinity of amino and cyano groups present in the target compounds. The composite was characterized by scanning electron microscopy, powder X-ray diffraction, Fourier-transform infrared spectroscopy, and surface area measurements. Regarding the SPE protocol, several parameters that can influence the extraction performance were optimized, such as sample volume or composition of elution solvent, among others. After elution, the analytes were determined via HPLC with diode-array detection. Under the selected conditions, satisfactory recoveries of five pesticides (thiamethoxan, clothianidin, imidacloprid, acetamiprid, and thiacloprid) were obtained (between 80 and 110%) in real samples, whereas the limits of detection ranged from 0.019 to 0.041 μg L in aqueous samples and 0.3 to 0.8 μg g in solid samples.
本文介绍了一种由胺化沸石咪唑酯骨架和金纳米颗粒（AuNPs）构建的复合材料，用于农业样品中新烟碱类的固相萃取（SPE）。该复合材料是基于氨基与AuNP之间的强相互作用，通过将AuNPs组装到金属有机骨架表面而制备的。这些金属表面基于目标化合物中存在的氨基和氰基的亲和力提供了额外的相互作用。通过扫描电子显微镜、粉末X射线衍射、傅里叶变换红外光谱和表面积测量对该复合材料进行了表征。关于SPE方案，对几个可能影响萃取性能的参数进行了优化，如样品体积或洗脱溶剂的组成等。洗脱后，通过带二极管阵列检测的高效液相色谱法测定分析物。在选定的条件下，实际样品中五种农药（噻虫嗪、噻虫胺、吡虫啉、啶虫脒和噻虫啉）的回收率令人满意（80%至110%），而水样中的检测限为0.019至0.041μg/L，固体样品中的检测限为0.3至0.8μg/g。
