Multiple headspace solid-phase microextraction (MHS-SPME) with gas chromatography-mass spectrometry is proposed for quantification of nine volatile oak compounds in aged wines. These compounds are formed and extracted by wine when it is matured in oak barrels and are responsible for particular organoleptic properties and the high quality of these wines. Some important variables of the extraction process, for example volume of sample and extraction time, were studied. Extraction of 50 microL wine was performed with a divinylbenzene-Carboxen-polydimethylsiloxane fibre at 55 degrees C for 60 min. For calibration the same conditions were used, except that the wine was substituted by 50 microL of a standard solution in synthetic wine. The linearity, detection limits, and repeatability of the method were determined by use of standard solutions in synthetic wine. Detection limits were between 0.01 and 10 microg L(-1) (for eugenol and furfural, respectively) and repeatability, expressed as relative standard deviation, was from 2 to 6%. The method was used to analyse six red wines and the concentrations obtained were statistically compared with those obtained by the standard addition method for the same wines.