Optimization of solid-phase microextraction conditions for the determination of triclosan and possible related compounds in water samples

Abstract

A solid-phase microextraction (SPME) method for the determination of triclosan, methyl triclosan, 2,4-dichlorophenol and 2,3,4-trichlorophenol (considered as possible triclosan metabolites) in water samples was optimised. Analytes were first concentrated on a SPME fibre, directly exposed to the sample, and then triclosan and the two chlorinated phenols on-fibre silylated using N-methyl- N-( tert.-butyldimethylsilyl)-trifluoroacetamide (MTBSTFA). Methyl triclosan remained unaffected during the derivatization step. Compounds were determined using gas chromatography in combination with mass spectrometry (GC–MS). Influence of different factors on the efficiency of extraction and derivatization steps was systematically investigated. Using a polyacrylate (PA) fibre quantification limits below 10 ng/l, and acceptable relative standard deviations, were obtained for all compounds after an extraction time of 30 min. On-fibre silylation was carried out in only 10 min. Moreover, the efficiency of the procedure was scarcely affected by the type of water sample. The method was applied to several samples of treated and raw wastewater, triclosan was found in all samples, at concentrations from 120 to 14,000 ng/l, and 2,4-dichlorophenol in most of them, at levels up to 2222 ng/l.