An analytical method has been developed to determine bisphenol A and five degradation products of alkylphenol ethoxylates in sewage and sludge. The parameters of accelerated solvent extraction (ASE) were optimized. C18 cartridge was used to clean up the sewage and the extract of sludge. The sensitivity of the mass detector was improved by adjusting the voltage of the lens manually. The instrumental detection limit was 3.2―17.8 pg. The method detection limits were 2.5―11.4 ng/L and 0.3―2.1 ng/g for sewage and sludge analysis respectively. The recovery and relative standard deviation for sewage analysis were 79.2%―111.4% and 6.9%―12.6%; for sludge analysis were 68.5%―114.0% and 8.9%―16.0%. Finally this method was applied to determining the phenolic endocrine disrupting chemicals in sewage and sludge from a sewage treatment plant in Beijing.