In this work, the antioxidant activity of a methanolic extract, isolated hesperitin and hesperidin, and a semi-synthetic hesperitin derivative from Citrus aurantium were assessed. Citrus aurantium orange peels are extracted using a Soxhlet apparatus to get a methanolic extract. This is followed by the separation of two essential flavonoids glycosides, hesperitin and hesperidin, and the synthesis of a novel hesperitin derivative. The 1,1-diphenyl-2-picryl hydroxyls (DPPH) scavenging of free radicals techniques were used to assess the antioxidant activity. The IC50 Value was used to assess the antioxidant potential. When compared to other derivatives, the isolated hesperitin Aa shown greater biological activity, while the semi-synthesised derivative (Aa-03) had strong antioxidant activity.