Volatile sulphur compounds are metabolites with particular biological activity found in plants, animals, and microorganisms, but the most varieties of these compounds have been found in plants. Some of the volatile sulphur compounds are also degradation products of glucosinolates. Glucosinolates are biologically inactive and non-volatile compounds found in 16 families of the Brassicales order. Volatile compounds known for their biological activity are formed by thermal, enzymatic or chemical degradation of glucosinolates. Volatile sulphur compunds from selected parts of four Lepidium spp. (Brassicaceae family) plants: L. graminifolium, L. latifolium, L. meyenii and L. sativum; and horseradish tree (Moringa oleifera) of the Moringaceae family were isolated and analysed. Glucosinolate compositions of these plants were determined by an indirect method using their degradation products. The volatile isolates collected by hydrodistillation in Clevenger-type apparatus, and extraction with dichlormethane after the hydrolysis with exogenous enzyme myrosinase were analysed with gas chromatography coupled to mass spectrometry (GC-MS) and Fourier transform infrared spectroscopy (FTIR). Analysis showed that the most widespread glucosinolate in the Lepidium spp. plants was glucotropaeolin, which had been found in all four plants. Besides glucotropaeolin, glucolimnanthin, gluconasturtiin, sinigrin, glucocohlearin and n-phenyl glucosinolate were identified. Regarding the free volatile sulphur compounds, only one was identified: diisopropyl disulphide in L. sativum. Neither glucosinolates nor free volatile sulphur compounds were found using GC-MS analysis of the distillate and the extract of the M. oleifera plant, but FTIR analysis showed a presence of unidentified compounds.