Glucosinolates, β-thioglucoside-N-hydroxysulphates with variable side chains, are secondary metabolites synthesized from amino acids. Glucosinolates are chemically stable and biologically inactive compounds, and their degradation produces a number of different biologically active degradation products. They can be degraded enzymatically, thermally and chemically. Different isolation methods have been applied in this work, including hydrodistillation in the modified Clevenger apparatus, autolysis, and microwave distillation and extraction in order to investigate the thermal, enzymatic, and microwave- assisted glucosinolate degradation. The aim of the study was to isolate and identify volatile sulfur compounds from the hedge mustard (Sisymbrium officinale (L.) Scop.). Hedge mustard, a plant species of the Brassicaceae family, was collected in Split and in the Krka River area during May 2019. Glucosinolates were identified indirectly by GC-MS analysis of their degradation products and directly by HPLC-DAD analysis of desulfated glucosinolates. In all plant parts of the hedge mustard (root, stem, leaf, flower), in both areas, three glucosinolates were identified: glucoputranjivin (0.68-16.00 µmol/g), 4-hydroxyglucobrassicin (0.035-2.732 µmol/g) and glucobrassicin (0.244-6.397 µmol/g). Furthermore, glucosinalbin, 4- methoxyglucobrassicin and neoglucobrassicin were also identified at the root of the plant. The volatile compounds analyzed by GC-MS analysis indicate that the most common degradation product is isopropyl isothiocyanate, as the breakdown product of glucoputranjivin.