Volatile sulphur substances originating during technological processes in malt and beer production can be a cause of various off-flavors and aromas. Their precursors are sulphur-containing amino acids. Sulphur substances play an important role in brewing as even in very low concentrations they can negatively affect total character of beer. Therefore, it is necessary to monitor volatile sulphur substances and their precursors to eliminate undesirable processes. Because sulphur substances occur in beer and raw materials at trace levels, microanalytical methods are used for their detection. This diploma thesis describes the problems of sulphur substances and their determination using the SPME/GC method.