This investigation is based on the gas chromatographic analysis of the volatile fraction of Sicilian goat cheese. Volatile analytes were extracted through static headspace solid phase microextraction (HS-SPME) with the support of a modern automatic instrument designed specifically for this sampling procedure. Component identification was carried out by GC-MS and the employment of internal standard compounds. In the preliminary part of this research, different fibres and capillary columns were tested and their effectiveness compared in order to optimize solute extraction and separation. Furthermore, the HS-SPME sampling conditions were properly tuned in order to maximize solute absorption. Evaluations were also made on the SPME instrumentation and its capability to supply reproducible data. The optimized method was applied to the investigation of six goat cheese samples and their aroma profiles were evaluated, leading to the identification of 44 components. Copyright © 2005 John Wiley & Sons, Ltd.