In this study, we synthesized, characterized the magnetic graphene oxide coated with polyvinyl alcohol (PVA@MGO), and used it as an adsorbent for the magnetic solid-phase extraction (MSPE) of organophosphorus pesticides (OPPs) residue in the apple juice and environmental water samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Effective factors on the extraction efficiency, including the adsorbent dosage, desorption conditions, sample pH, extraction and desorption time, and ionic strength were optimized. The dynamic range of the MSPE-GC-MS method was obtained in the concentration range of 0.07–500 ng mL−1 OPPs with the limits of detection (LODs) in the range of 20–80 pg mL−1. Also, the intra- and inter-day precisions were determined to be in the range of 3.3–5.7% and 5.9–8.2%. The relative recoveries of pesticides for spiked real water samples and apple juice were in the range of 94.5 and 107.1%, with relative standard deviations between 2.6 and 6.5%. These results propose that the PVA@MGO is appropriate for simultaneous determination and high throughput analysis of OPPs residues.

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