Benzoylurea (BU) insecticides have contributed greatly to the output of crops. Their residue in the environment put serious threats on human health and environmental safety. In this study, we have established a new, rapid, and reliable method for the monitoring of typical BU insecticides such as diflubenzuron, flufenoxuron, triflumuron, and chlorfluazuron with dispersive liquid-liquid microextraction prior to HPLC. Chlorobenzene and ethanol were employed as the extraction solvent and disperser solvent, respectively. The possible parameters which would influence the extraction efficiency such as the kinds and volumes of extraction and disperser solvents, extraction time, sample pH, centrifuging time, and salting-out effect were optimized in detail. Under the optimal conditions, the linear range of proposed method was in the range of 1.0-70 μg/L. The detection limits varied from 0.24 to 0.82 μg/L and the precision of the method was <6.5% (RSD, n = 6). The proposed method was validated with real water samples and satisfactory spiked recoveries were achieved. All these results indicate that the proposed method is a low cost, easy to operate, efficient, and sensitive method for the analysis of BU insecticides in water samples.