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Alcohol polyethoxylates (AEOs) are the most commercially important type of nonionic surfactants, used in a wide variety of products such as household cleaning detergents, industrial cleaners, textiles, adjuvants in pesticides, wetting and dispersing agents, and emulsifiers. Our main objective in this work was to develop a methodology for the extraction, isolation and analysis of these compounds and their main degradation products and precursors (polyethylene glycols, PEGs) in solid environmental matrices. First, analytes were extracted by pressurized liquid extraction (PLE) using methanol at 120°C as solvent and 3 cycles (5 min per cycle). Clean-up and concentration of the extracts were carried out by solid-phase extraction (SPE), using Oasis HLB cartridges and a mixture dicloromethane/methanol 1:1 as eluting solvent. Recovery percentages were usually between 54% and 106% for most compounds. Identification and quantification of analytes were performed using a liquid chromatography-mass spectrometry (LC-MS) system equipped with an electrospray interface (ESI) operating in positive ionization mode. Water content, cone voltage and adduct formation were optimized to this end. Limits of detection were usually below 50 ng g(-1), being higher for some shorter ethoxymers (>100 ng g(-1)) because of poor ionization. Finally, the protocol proposed here was applied to the determination of the concentration of AEOs and PEGs in selected surface sediment samples collected in Mar Menor Lagoon (Murcia, Spain). In this sense, this paper presents some of the first data relative to the occurrence of these analytes in coastal sediments, showing relatively high concentrations of PEGs (up to 9000 ng g(-1)) compared to those measured for AEOs (<100 ng g(-1))., (Copyright © 2013 Elsevier B.V. All rights reserved.)