Abstract
In this study, diethylenetriamine-functional magnetic core-shell polymer modified graphene oxide (DETA-MPs-GO) was prepared via precipitation polymerization and amidation reaction, and it was characterized by transmission electron microscopy (TEM), Fourier-transformed infrared spectroscopy (FTIR), and X-ray diffractometer (XRD). Subsequently, a magnetic solid-phase extraction (MSPE) procedure was applied to the as-synthesized DETA-MPs-GO for the detection of nine fungicides in fruit samples, prior to ultra-performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS). The homogenized fruit samples, spiked with D-labelled internal standards, were firstly extracted by 5 mL of acetonitrile twice and then purified by DETA-MPs-GO adsorbents. The optimization of the adsorption and elution conditions of DETA-MPs-GO toward fungicides was carried out to attain a satisfactory adsorption performance and desorption efficiency. The adsorption mechanism was carefully investigated, and the results revealed that a synergistic adsorption mechanism, including hydrogen bond and a π–π stacking interaction, was confirmed. Moreover, the limits of quantitation (LOQs) of the proposed approach were in the range of 0.01 to 0.30 μg/kg under the optimum conditions. The average recoveries at three spiking levels were 84.9% to 105.2%, with relative standard deviations (RSDs) varying from 0.8% to 8.2% (n = 6). The developed method was successfully utilized for the screening and detection of fungicides in 81 fruit samples purchased from markets. A detailed survey was carried out about the concentration distribution, types of fungicides, and combined use of fungicides in different fruits.
Highlights
Fungicides are among the most extensively exploited pesticides to destroy or prevent the growth of many plant pathogenic fungi in modern agriculture
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A rapid, accurate, and sensitive DETA-MPs-Graphene oxide (GO) based magnetic solid-phase extraction (MSPE)-UPLC-high resolution mass spectrometer (HRMS) method was established for the simultaneous detection of nine fungicides in fruit samples
Summary
Fungicides are among the most extensively exploited pesticides to destroy or prevent the growth of many plant pathogenic fungi in modern agriculture. Commonly used fungicides are highly toxic, and many of them have been proved to enervate the liver function, change the urinary bladder structure, and decrease kidney weight [3]. The development of a high resolution mass spectrometer (HRMS) provides an effective approach to solve the above problems. It was often used in peptides sequencing [13,14]; there is an increasing focus on and interest in investigating the quantification of small molecules [15,16,17]. The research on highly efficient extraction materials has drawn much attention [19,20,21,22]
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