Evaluation of triclosan and biphenylol in marine sediments and urban wastewaters by pressurized liquid extraction and solid phase extraction followed by gas chromatography mass spectrometry and liquid chromatography mass spectrometry

Analytical methods, based on GC-MS and LC-MS, for the determination of traces of 2,4,4'-trichloro-2'-hydroxydiphenyl ether (triclosan) and biphenylol in urban wastewater and marine sediments were developed. These methods involve the use of diverse analytical techniques, such as solid phase extraction (SPE) and pressurized liquid extraction for sample preparation, and GC-negative chemical ionization MS and LC-electrospray ionization (ESI) MS-MS for identification and quantification. The recoveries of triclosan and biphenylol were 84 and 80% in wastewater and 100 and 73% in sediments, respectively. Detection limits obtained were in the range of ppb and ppt. To prove their applicability to real samples and as part of a more extensive monitoring program, the developed methods were applied to the analysis of wastewater samples, coming from an urban wastewater treatment plant (UWWTP), and of marine sediment samples collected at the outflow of two UWWTPs to the sea. Results obtained reveal the presence of triclosan in all the samples at concentrations that ranged from 0.8 to 37.8 mug/l in wastewater and from 0.27 to 130.7 mug/kg in sediments. These preliminary data reinforce the interest for further research on this topic. (C) 2003 Elsevier Science B.V. All rights reserved.