The uncalcined but highly dispersive oxide-supported metal catalyst for liquid phase reactions may suffer from the agglomeration of metal nanoparticles and the drop of metal catalyst in solution, which will decrease the activity and shorten their life in catalysis. Here, a one-pot successive polyol reaction was developed to prepare M-E xO y colloidal particles as heterogeneous nanocatalysts, which merge the controlled synthesis of metal catalysts and oxide supports, the in situ loading of catalyst, and even the mesopore amplification into a highly integrated process. Unlike the traditional surface-deposited catalysts, the noble metal nanoparticles even with a large amount of loading are internally dispersed in the mesoporous oxide particles, which show higher activity and stability in the hydrogenation of nitroaromatics compared to the isolated nanocatalysts or surface-deposited catalysts. The improved activity and stability comes from the physical confinement of metal nanoparticles and good mass transportation of substrate/product within the support particles. This work proposed a novel method to prepare highly dispersed metal catalysts, which could be potentially useful to heterogeneous catalytic reactions with high-throughput and long-life demands.