A headspace solid-phase microextraction (HS-SPME) method has been developed for the determination of iodinated trihalomethanes (ITHMs) in treated water samples. Mixed THMs (bromochloroiodo-, bromodiiodo-, chlorodiiodo-, dibromoiodo- and dichloroiodo-) were previously synthesized since commercial standards are not available. HS-SPME has shorter equilibration times than direct SPME, a cleaner background and a longer fiber life. Experimental parameters such as the selection of SPME coatings, sample volume, extraction time and addition of salts were studied. The Carbowax-divinylbenzene fiber appears to be the most suitable for the determination of ITHMs. Analytical parameters such as linearity, limit of detection and precision were also evaluated. HS-SPME was compared to liquid-liquid microextraction for the analyses of spiked treated water samples, obtaining a good agreement. It is concluded that HS-SPME has a great potential for drinking water analysis. (C) 1999 Elsevier Science B.V. All rights reserved.