The Cu, Cr-, Zn, Cr- and Cu,Al-layered double hydroxides have been synthesized by the coprecipitation method and characterized by elemental analysis, PXRD, SEM/EDS and BET. The mixed oxide materials obtained upon calcination at 873 K show very high catalytic activity for the combustion of toluene and ethanol. The best sample is derived from the Cu, Cr-LDH precursor with a Cu:Cr ratio of 2, composed of copper oxide and copper chromite. This catalyst gave 50% conversion of toluene and ethanol at temperatures of 45 and 15 K lower, respectively, than the reference commercial catalyst. Catalytic tests with a mechanical mixture of CuO and CuCr 2 O 4 demonstrate that the use of an LDH precursor is essential for optimum results. The importance of the simultaneous presence of both Cu and Cr, the influence of the Cu:Cr ratio on the catalytic activity and the role of the interface boundaries in the CuO-CuCr 2 O 4 mixed oxide system are discussed.