Dynamic Headspace and Gas Chromatography and Mass Spectrometry (GC and MS) methods have been adapted for rye bread flavour analysis, optimising parameters: the amount of sample, trapping time, cold trap temperature and sample preparation method. Commercial rye bread was used as a reference. Experiments indicated that 25 g of sample could be taken for the test. Due to insufficient isolation of volatiles and flavour compounds in a short time period a prolonged trapping time of 40 min was chosen for the trapping the volatiles in the tube. Higher relative concentrations were obtained applying +5 C cold trap temperature in the GC device and using sample preparation method without water (dry sample preparation method). These parameters were successfully applied for rye bread flavour investigations.