In the present study, headspace solid phase microextraction combined to capillary gas chromatography (HS-SPME-GC) has been applied for the determination of changes in the volatile profile of rose petals (Rosa hybrida, cvs David Austin) following processing (heat treatment and addition as an ingredient to a food product--for example yoghurt). Four SPME fibres at two sampling temperatures (40 and 60 degrees C) with a sampling time of 30 min were examined. Volatile profiles were detected either by FID or/and by olfactometry (ODP-II, Gerstel). Fibre testing was performed using raw rose petals for sampling temperature selection and an 18 characteristic rose volatile standard mixture in water was used to compare fibre performances at the sampling temperature of 60 degrees C. Polydimethylsiloxane-divinylbenzene (PDMS-DVB) fibre at the sampling temperature of 60 degrees C was the most suitable to sample the rose alcohols phenyl ethanol, citronellol, nerol, geraniol and eugenol, as assessed by GC-olfactometry, not only from raw petals, but also from processed rose petals and the food product. PDMS-DVB fibre also showed a desired low affinity to volatiles from yoghurt, which reduces the influence of food matrix on the volatile profile. The method was linear over two orders of magnitude and had satisfactory repeatability, with limits of detection for the rose alcohols ranging from <1 to 10 ng/ml concentration levels.