Headspace Solid Phase Micro Extraction (HS-SPME) is a modem solvent-free extraction technique widely used for the characterization of the volatile fraction of food samples.The volatile compounds responsible for the typical aroma of the food sample often characterize the quality profile of the product.Sampling the headspace with a SPME fibre enriches those compounds and allows sensitive analysis by gas chromatographic methods.A deeper insight in a complex flavour composition is possible by coupling this sampling technique with a comprehensive two-dimensional gas chromatographic system (GC × GC), taking advantage of its enhanced separation power.