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Superhydrophilic graphene oxide/electrospun cellulose nanofibre (GO/CNF) was synthesized, characterized and successfully used in a solid-phase membrane tip adsorption (SPMTA) as an adsorbent towards a simultaneous analysis of polar organophosphorus pesticides (OPPs) in several food and water samples. Separation, determination and quantification were achieved prior to ultra-performance liquid chromatography coupled with ultraviolet detector. The influence of several parameters such as sample pH, adsorption time, adsorbent dosage and in