Two solid-phase microextraction (SPME) procedures have been developed to determine short ethoxy chain nonylphenols and metabolites in water. A direct-SPME method has been used for the determination of short ethoxy chain nonylphenols and their brominated derivatives, whereas the in-sample derivatization headspace-SPME method has proved to be suitable for the simultaneous determination of short ethoxy nonylphenols and their acidic metabolites. Several parameters affecting both SPME procedures, such as extraction mode, fiber selection, extraction time, effect of organic modifiers, derivatization reagents and temperature, were optimized. Both methods were able to determine all these compounds at the sub-mg/L level and the results obtained were compared to a solid phase extraction method (SPE). The procedures developed were applied to raw and treated water from Barcelona (NE Spain).

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