Because of their weakly estrogenic properties, interest in nonylphenol polyethoxylates and their carboxylated metabolites is resurging. To assess their occurrence in surface waters impacted by municipal and industrial effluents, an analytical method was developed for the quantitative determination of nonylphenol polyethoxy carboxylate (NPEC) metabolites of nonylphenol polyethoxylate surfactants in paper mill effluents, municipal sewage treatment plant effluents, and river waters. Strong anion exchange solid phase extraction disks were used far NPEC isolation from aqueous samples, and NPEC elution from the disk is simultaneously combined with derivatization. Extracts were analyzed by gas chromatography and positive mode chemical ionization mass spectrometry. The detection limit of the method ranged from 0.2 mu g/L for NP1EC to 2 mu g/L for NP4EC. The total concentration of NPECs in a group of paper mill and municipal sewage effluents ranged from below detection to 1300 mu g/L. The total concentration of NPECs in several river waters ranged from below detection to 13.8 mu g/L.