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In continuation of research conducted on species of the spontaneous flora of Sicily (Italy) belonging to the Brassicaceae family, <i>Brassica fruticulosa</i> subsp. <i>fruticulosa</i> was selected. It is an edible species utilized in Sicilian traditional medicine. In this study, for the first time, the phenolic and the volatile compounds and the antioxidant properties of the hydroalcoholic extract obtained from the leaves of <i>B. fruticulosa</i> subsp. <i>fruticulosa</i> were characterized. Through HPLC-PDA/ESI-MS analysis, a total of 22 polyphenolic compounds (20 flavonoids and 2 phenolic acids) were identified, with 3-hydroxiferuloylsophoroside-7-<i>O</i>-glucoside (1.30 mg/g ± 0.01) and kaempferol-3-<i>O</i>-feruloylsophoroside-7-<i>O</i>-glucoside (1.28 mg/g ± 0.01) as the most abundant compounds. Through SPME-GC/MS several volatiles belonging to different chemical classes were characterized, with nitriles and aldehydes accounting for more than 54% of the whole volatile fraction. The extract of <i>B. fruticulosa</i> subsp. <i>fruticulosa</i> showed moderate activity in the DPPH assay (IC₅₀ = 1.65 ± 0.08 mg/mL), weak reducing power (17.47 ± 0.65 ASE/mL), and good chelating properties (IC₅₀ = 0.38 ± 0.02 mg/mL), reaching approximately 90% activity at the highest tested concentration. Lastly, the extract was non-toxic against <i>Artemia salina</i>, indicating its potential safety. According to the findings, it can be stated that <i>B. fruticulosa</i> subsp. <i>fruticulosa</i> represents a new valuable source of bioactive compounds.