Magnetic solid-phase extraction (m-SPE) is a promising sample preparation approach due to its convenience, speed, and simplicity. For the first time, a rapid and reliable m-SPE approach using magnetic multi-walled carbon nanotubes (m-MWCNTs) as the adsorbent was proposed for purification of type A trichothecenes including T-2 toxins (T2), HT-2 toxins (HT-2), diacetoxyscirpenol (DAS), and neosolaniol (NEO) in coix seed. The m-MWCNTs were synthesized by assembling the magnetic nanoparticles (Fe3O4) with MWCNTs by sonication through an aggregation wrap mechanism, and characterized by transmission electron microscope. Several key parameters affecting the performance of the procedure were extensively investigated including extraction solutions, desorption solvents, and m-MWCNT amounts. Under the optimal sample preparation conditions followed by analysis with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), high sensitivity (limit of quantification in the range of 0.3-1.5 μg kg(-1)), good linearity (R (2) > 0.99), satisfactory recovery (73.6-90.6 %), and acceptable precision (≤2.5 %) were obtained. The analytical performance of the developed method has also been successfully evaluated in real coix seed samples. Graphical Abstract Flow chart of determination of type A trichothecenes in coix seed by magnetic solid-phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry.
The presence of pesticide residues has become one of the main risk factors affecting the safety and quality of agro-food. In this study, a multi-residue method for the analysis of 284 pesticides in five local fruit cultivars in Shanghai was developed based on ultrahigh-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF/MS). The limits of determination and the limits of quantitation of pesticides were 0.6–10 and 2–30 μg/kg, respectively. A total of 44, 10, 10, 18, and 7 pesticides were detected in strawberries, watermelons, melons, peaches, and grapes, respectively. The pesticide levels in 95.0% of the samples were below the maximum residual limits (MRLs) prescribed by China, and in 66.2% of the samples below the EU MRLs. The dietary risk assessment study showed big differences in the chronic and acute exposure risk values among different Chinese consumer groups. Through fruit consumption, children/females showed higher exposure risks than adults/males. But both the risk values were less than 100%, indicating that potential dietary risk induced by the pesticides was not significant for Chinese consumers. Nevertheless, certain measures are needed for both growers and the government in order to decrease the MRL-exceeding rate of pesticide residues and ensure the quality and safety of fruits for consumers.
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