Volatile organic compounds (VOCs) are harmful to human health due to their carcinogenicity and toxicity. In addition, they are responsible for the generation of secondary atmospheric pollutants. Catalytic oxidation is an effective alternative for the reduction of these types of emissions. In this context, CeÀ Mn oxides have been reported as excellent catalyst because of their low cost, redox capacity, and oxygen mobility. To date, the best CeÀ Mn oxide catalysts have been produced using hydrothermal synthesis. In the present work, we propose a novel, facile, environmental-friendly, and low-cost sonochemical method for the synthesis of MnÀ Ce oxides with different Ce loadings. The new materials were characterized, and catalytic activity was measured in toluene oxidation reactions. Results demonstrated that, despite the low surface area of MnÀ Ce oxides prepared by sonochemical method, these samples showed a superior catalytic activity with T 90 values of 266 °C. This performance was the result of the higher Mn 4 + content, as well as improved reducibility and activation of O lat species as compared to that of hydrothermally synthesized catalysts. However, the interaction between Mn 2 O 3 and MnO 2 in the hydrothermally synthesized catalysts resulted in a greater stability in long-term oxidation reactions.