In this research, an effective sample preparation method called solvent‐assisted dispersive solid‐phase extraction followed by corona discharge ion mobility spectrometry was proposed for the trace determination of organophosphorus pesticides in environmental water samples. In this method, to maximize the interaction surface between target analytes and sorbent, the sorbent was dispersed into the aqueous sample. In this technique, the sorbent was dispersed at very low levels using a solution of sorbent and disperser solvent into the aqueous sample. Then, a cloudy solution was created by dispersing the sorbent particles in aqueous solution. After the interaction of organophosphorus pesticides and benzil, the cloudy solution was centrifuged and organophosphorus pesticides in the solid phase were dissolved in ethanol. In order to obtain the best extraction efficiency, the optimization of parameters affecting this method was examined. After optimization, the results were obtained as follows: pH of solution: 7.0, sorbent: benzil, 2% w/v, disperser solvent: ethanol, 500 µL, and centrifuge: centrifuged at 6000 rpm for 2 min. The presented method showed low method detection limit (0.3 ng mL−1), excellent preconcentration factor (368–376), good linearity (>0.994), repeatability (RSD < 4.1%), and high recoveries (92–94%).