The detection and quantification of four phthalate esters-dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), and diethylhexyl phthalate (DEHP)-in water, sediment, and some fish species were carried out using flame ionization gas chromatography. The samples were collected from the Ogun river catchments, Ketu, Lagos. The DMP was not detected in the water and fish samples but was detected in sediments collected from four of the six sampling sites. The concentration of DEP, DBP, and DEHP in the fish species ranged from 320.0-810.0, 380.0-1,080.0, and 40.0-150.0 μg/kg in Tilapia sp.; 310.0-860.0, 400.0-1,170.0, and 40.0-110.0 μg/kg in Chrysichthys sp.; and 320.0-810.0, 400.0-3,970.0, and 30.0-300.0 μg/kg (DEHP) in Synodontis sp.,respectively. The differences in fish phthalate levels are not statistically significant at p < 0.05, an indication that phthalate esters accumulation is not fish species dependent. The DEP, DBP, and DEHP values recorded are considerably higher than the maximum allowed concentrations for drinking water prescribed by the US Environmental Protection Agency. The phthalate pollution index and biosediment accumulation factor values were also calculated.