A new method based on solid-phase extraction (SPE) on-line coupled to gas chromatography-mass spectrometry through an on-column interface has been applied to determine three antifouling compounds in water samples. Parameters affecting the SPE process and transfer step have been optimised and the method developed has been applied to the analysis of marinas, fishing ports and Ebro river water. The method allows the analytes to be detected at 0.01 microgram l-1 in SIM acquisition mode by preconcentrating only 10 ml of water sample. Different marina and fishing port water samples have been analysed and Irgarol 1051 has been found in some of them at a concentration level equal or lower than 0.05 microgram l-1.
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