Metal-organic framework MIL101 (Cr)-NH2 functionalized magnetic graphene oxide for ultrasonic-assisted magnetic solid phase extraction of neonicotinoid insecticides from fruit and water samples.

In this work, a magnetic nanocomposite composed of graphene oxide (GO), silica-coated cobalt ferrite (CoFe2O4@SiO2) nanoparticles and amino-functionalized metal-organic framework (MIL 101 (Cr)-NH2) was fabricated and employed for ultrasonic-assisted magnetic solid phase extraction (UA-MSPE) of neonicotinoid insecticides. Various techniques such as Fourier transform infrared (FT-IR) spectrometry, vibrating sample magnetometry (VSM), energy-dispersive X-ray spectroscopy (EDS) and field emission scanning electron microscope (FE-SEM) measurements were executed to investigate features and morphology of the adsorbent. The magnetic graphene oxide functionalized MIL-101 (Cr)-NH2 (MGO/MIL) combines the advantages of magnetic GO and MIL 101(Cr)-NH2 such as excellent thermal and chemical stability, high surface area, accessible coordinative unsaturated sites, sufficient stability in aqueous solutions and rapid and easy separation from the solution. Some of the important extraction factors such as type and volume of desorption solvent, desorption time, salt concentration, adsorbent amount, pH and extraction time were investigated in detail to achieve high MSPE recovery. In optimal condition, the limits of detection (LODs) for Acetamiprid and Imidacloprid were achieved 0.022 and 0.019 ng mL-1, respectively. Good determination coefficients (R2 more than 0.9990) with satisfactory linearity in the range of 0.064-3500 ng mL-1 were found for this method. The relative standard deviations for intra- and inter-day analyses were in the range of 3.93-4.56% and 7.80-8.50%, respectively. The method was successfully used for analyzing of neonicotinoid insecticides in water and fruit samples and acceptable recoveries from 82.13% to 102.27% were obtained. The results indicated that the nanocomposite is feasible for the adsorption of trace amounts of the target analytes from the fruit and water samples.