Polyethoxylated alkylphenols (APnEO, where n is the number of ethylene oxide molecules), are non-ionic surfactants widely used for domestic and industrial purposes. Most of APnEO are polyethoxylated nonylphenols (NPnEO). NPnEO are widespread environmental pollutants with relatively low toxicity for mammals and higher toxicity for aquatic organisms. In addition, they have been described as endocrine disrupters in recent publications. One of the main problems related to these surfactants is their uncomplete degradation, even in the most effective sewage treatment plants. Usually, the final products, more toxic and resistant to biological degradation than NPnEO, are nonylphenol (NP), monoethoxylated nonylphenol (NP1EO), diethoxylated nonylphenol (NP2EO), nonylphenoxy acetic acid (NP1EC), and nonylphenoxyethoxy acetic acid (NP2EC). In this paper, the degradation of NPnEO was studied in the different processes of a sewage treatment plant. For this purpose, NP, NP1EO and NP2EO were analysed in composite samples collected at different points along the plant (influent, pre-treatment effluent, primary effluent, plant effluent). Analyses were carried out by isotopic dilution-HRGC/MS, using available labelled nonylphenols (13C6-NP, 13C6-NP1EO, 13C6-NP2EO) as internal standards. Extraction of NPnEO from aqueous samples, previous to analysis, was performed by the Likens-Nickerson method (simultaneous steam distillation/solvent extraction, SDE).