Biogenic amines are interesting compounds which may be of use for medical diagnosis or therapeutic monitoring. The present paper deals with the problems that occur with concentration determination of dimethylamine (DMA) and trimethylamine (TMA). These occur in the breath of people suffering from renal disease. The measurement of amines present in trace concentrations requires the application of suitable analytical methods during sampling, storage and preconcentration. This is particularly so due to their polar and basic properties. In this paper, the application of solid phase microextraction (SPME) and thermal desorption (TD) with subsequent measurement by GC-MS for the determination of amines is discussed. For DMA, preconcentration by SPME did not give satisfactory results. TMA may be analysed using SPME preconcentration with an LOD of 1.5 ppb. Thermal desorption with Tenax as the adsorbing material allows reliable concentration determination for TMA (LOD = 0.5 ppb) and DMA (LOD = 4.6 ppb). DMA cannot be stored reliably in Tedlar bags and longer storage on Tenax (with subsequent TD) does not give good repeatability of results. For TMA, storage can be done on Tenax or in bags, the best results for the latter being achieved with Flex Foil bags.