An analytical method has been developed and applied to determine the concentrations of the nonionic alkylphenol polyethoxylate surfactants and their metabolites, alkylphenoxy carboxylates and alkyphenols, in sewage sludges. The compounds were extracted with methanol/acetone (1:1 v/v) from sludge, and concentrated extracts were cleaned by silica solid-phase extraction prior to determination by liquid chromatography tandem mass spectrometry. The recoveries, determined by spiking sewage sludge at two concentrations, ranged from 51% to 89% with method detection limits from 6 microg kg(-1) to 60 microg kg(-1). The methodology was subsequently applied to sludge samples obtained from a carbonaceous activated sludge plant, a nitrifying/denitrifying activated sludge plant and a nitrifying/ denitrifying activated sludge plant with phosphorus removal. Concentrations of nonylphenolic compounds were two to three times higher than their octyl analogues. Long-chain nonylphenol polyethoxylates (NP3-12EO) ranged from 16 microg kg(-1) to 11754 microg kg(-1). The estrogenic metabolite nonylphenol was present at concentrations ranging from 33 microg kg(-1) to 6696 microg kg(-1).