In this research, the nanohybrid of the polyoxometalate/graphene oxide (POM/GO) is synthesized and characterized. The porosity and quality of the POM/GO nanohybrid was studied and evaluated by applying Fourier transform infrared (FTIR) and transmission electron microscopy (TEM). The POM/GO nanohybrid was applied as an efficient sorbent for the dispersive micro solid-phase extraction (D-μSPE) of the non-steroidal anti-inflammatory drugs (NSAIDs) in the environmental water samples. Based on the results, by comparing different types of sorbents, POM/GO nanohybrid has the highest adsorption affinity. Under the optimum conditions limits of detection (LODs, at an S/N ratio of 3) and linear ranges were achieved in the range of 0.02–0.03 ng mL−1 and 0.08–200 ng mL−1 , respectively. The relative standard deviations (RSDs) for five replicates at three concentration levels (0.1, 5 and 100 ng mL−1 32 ) of analytes were ranged from 4.1 to 6.1%. Ultimately, the applicability of this method was successfully confirmed by analyzing real water samples and satisfactory results were obtained in the range of 95.6 to 99.6%.

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