In this study, three‐dimensional flower‐like tin disulfide materials were prepared, and a highly efficient dispersive solid‐phase extraction method was developed using the obtained three‐dimensional tin disulfide adsorbents for the preconcentration and determination of six endocrine‐disrupting phenols in combination with high‐performance liquid chromatography‐ultraviolet detection. Several important experimental parameters influencing extraction efficiency were investigated, including the amount of adsorbent, ultrasound time, sample solution pH, sample volume, type of elution solvent, desorption time, and the number of desorption times. Under the optimized experimental conditions, the developed method showed good linearity with the determination coefficients of 0.993–0.998 in the linear range of 0.5–400 ng/ml and low limits of detection in the range of 0.15–1.0 ng/ml, as well as satisfactory intra‐day and inter‐day precisions with relative standard deviations of 0.1–9.8%. Finally, the proposed method was successfully applied for the enrichment and determination of trace endocrine‐disrupting phenols in milk, tea beverage, and plastic bottled water samples, and acceptable recoveries were obtained from 70.1% to 119.1% under four different spiked concentration levels. The results showed that the three‐dimensional tin disulfide materials had great potential for the extraction of endocrine‐disrupting phenols contaminants in environmental and food samples.