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In this study, a method was developed for determination of three organophosphorus pesticides (OPPs) using graphene aerogel solid-phase extraction (SPE) combined with gas chromatography–mass spectrometry (GC–MS). The experimental results showed that the target analytes could be extracted on packed SPE cartridges and then eluted with tetrahydrofuran. The final sample solution was analyzed by GC–MS, which demonstrated good linearity between 0.5 and 500 μg L−1 with a correlation coefficient (r) of 0.9991–0.9998. The limits of detection (S / N  = 3) and the limits of quantification (S / N  = 10) for the three OPPs ranged from 0.38 to 0.82 μg L−1 and 1.32 to 2.75 μg L−1, respectively. The accuracy of the proposed method was evaluated by measuring the recovery of the spiked samples, which ranged from 91.2 to 103.7%, with relative standard deviations of 2.1–7.2%. This method was successfully applied for the determination of the target analytes in water samples taken from tap, wetlands and canal water. [ABSTRACT FROM AUTHOR]