The conventional method for the preparation of metal nanoparticles loaded on a mesoporous metal oxide is tedious, and its chemical and physical properties cannot be optionally controlled. A simple and convenient method by one-step in the AcHE sol-gel system was employed for the preparation of nano-Ni/meso-Ce-TiO 2 samples with different Ni nanoparticle loadings. Their physical and chemical properties were characterized by XRD, liquid N 2 adsorption-desorption, EDX, ICP, FT-IR, H 2 -TPR and TEM techniques, and their catalytic performance was investigated in the hydrogenolysis of xylitol. The results show that these samples with ordered mesoporous structures, uniform pore size and large specific surface area can be obtained. The Ni nanoparticles can be well dispersed on the mesoporous Ce-TiO 2 surface. The stability of the Ni nanoparticles on the mesoporous TiO 2 would be promoted by the introduction of a small amount of cerium species. The 8% nano-Ni/meso-Ce-TiO 2 sample shows a higher catalytic performance than other samples. The conversion of xylitol was 87.9% and a total yield of diols of 83.2% can be reached. It shows high stability, and the conversion of xylitol and the total yield of diols decreased slightly after repeating the reaction 8 times. The method provides a valuable reference for the preparation of metal nanoparticles loaded on a mesoporous metal oxide, especially for nonnoble metal nanoparticles.