Sonochemical procedure was used to synthesize Co/β-cyclodextrin complex.For the first time, Fe/β-cyclodextrin complex was also synthesized in alkaline media. Moreover, β-cyclodextrin was modified by citric acid (CA) and reacted with metal salts under ultrasonic irradiation. The prepared catalysts were characterized by using EDX, UV-vis and FTIR analytical techniques. The highest incorporation of metal into β-cyclodextrin was observed in the citric acid cross linked β-CD. The catalase like activity (peroxide scavenging) of Co/β-CD and Fe/β-CD complexes and composites was evaluated by UV-visible spectrophotometer and their superoxide scavenging capacity were measured using the pyrogallol method. The Co 3 /CA-β-CD complex showed the best catalase mimetic activity (93.2%) even in comparison to catalase enzyme extracted from potato. Therefore, cobalt complexes of citric acid/β-CD are promising candidates for H 2 O 2 scavenging. By contrast Fe 3 /CA-βCD complex had stronger capability to eliminate superoxide anion radicals.