A method for determination of chlorophenols (CPs) in sediments was developed using ultrasonic solvent extraction followed by solid-phase extraction, derivatization, and gas chromatography–mass spectrometry (GC-MS) analysis. Some effective operational details and parameters on mixing of samples and extraction solvent, adsorption loss, and extraction cycles of the derivatives were studied and optimized. The calibration curves of standard solutions were observed in the range of 0.5–100 μg L−1 and correlation coefficients ranged from 0.998 to 0.999. The limits of detection (LODs) for individual CPs are in the range of 0.026–0.072 ng g−1. The method showed good performance with the recovery efficiencies of target CPs in spiked sediment at 73.2–105.6%. In addition, the feasibility of applying the proposed method to determine the concentration of CPs in field core sediment samples collected in three shallow lakes in Eastern China was examined. The obtained results show that the present method is a sensitive, simple, low cost and highly feasible method for determination of CPs in sediment samples.