Ozonation is commonly used in drinking water treatment technology. Ozone reacts with natural organic substances present in water to produce a number of by-products. Aldehydes are the important class of ozonation byproducts due to their health effects. The determination of aldehydes in water by conventional analytical techniques is difficult because they are polar, unstable and exist at low concentration. A modern method for the determination of aldehydes in drinking water applies derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine (PFBOA) and liquid-liquid extraction (LLE). The objective of this study was to improve the method by application of solid-phase derivatization and extraction. C-18, C(18)polar plus and Phenyl Baker SPE sorbents were used for simultaneous derivatization and enrichment of aldehydes. Detection limits with GC-electron-capture detection technique were in the low ppt range.