A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF). 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect. temperature. adsorption and desorption times. The method is simple and accurate (RSD < 8%), showed good recoveries (77-107%) and good limits of detection (CC-FID: 1.37 mu g L-1 for 2-F, 8.96 mu g L-1 for 5-MF, 6.52 mu g L-1 for 5-HMF; GC-TOF-MS: 0.3, 1.2 and 0.9 ng mL(-1) for 2-F. 5-MF and 5-HMF, respectively). It was applied to different commercial food matrices: honey, white. demerara, brown and yellow table sugars, and white and red balsamic vinegars. This one-step, sensitive and direct method for the analysis of furfurals will contribute to characterise and quantify their presence in the human diet. (C) 2008 Elsevier B.V. All rights reserved.