Linear alkylbenzene, sulfonates (LAS) have been determined in samples of the influent and the effluent, and in the sludge, from sewage-treatment plants (STP). LAS and sulfophenyl carboxylate compounds (SPC) were isolated by solid-phase extraction (SPE) with the polymeric phase Isolute ENV, then determined by liquid chromatography-electrospray mass spectrometry (LC-ESI-MS). The method enabled unequivocal identification of C-10-C-13 LAS by monitoring the ion at m/z 183 and the base peak corresponding to the [M-H](-) ion. Average recoveries varied from 77-93% and the linear range of the method varied from 0.2 to 10 mug L-1, with a limit of detection ranging from 10 ng L-1 to 1.5 etag L-1 when 200 mL waste water were preconcentrated. For sewage sludge, recoveries varied from 58 to 90% and the linear ran-e was between 0.2 and 100 mug L-1, with a detection limit ranging from 0.4 to 120 mug kg(-1) when 2.5 g sewage sludge was extracted. Unequivocal identification and determination of some metabolites of the LAS, the sulfophenyl carboxylate compounds (SPC), was achieved by monitoring [M-H](-) ions.