Based on solid-phase microextraction (SPME) and on-fiber silylation, five kinds of exogenous endocrine disrupting chemicals (EDCs) concentrations were analyzed in Yangtze River Estuary and adjacent areas in August 2008. The selected target compounds were nonylphenol(NP), octylphenol(OP), diethylstilbestrol (DES), estrone (E1) and 17-estradiol (E2). The result showed that the concentrations of EDCs above were between 0.013–0.186 µgL−1, 0.004–0.096 µgL−1, 0.002–0.014 µgL−1, 0.018–0.048 µgL−1 and 0.006–0.024 µgL−1, respectively. The high concentration zone in surface water was located along the direction of Yangtze River freshwater plume with maximum concentrations recorded at the rim of the Maximum Turbidity Zone. Freshwater and suspended solids in Yangtze River were the main sources of EDCs in the study area. The distribution pattern of EDCs influenced by the hydrodynamic conditions, suspended solid transportation and microbial activity.