A novel process for the preparation of monodisperse magnetic polymer microspheres by uniquely combining swelling and thermolysis technique was reported. The monodisperse polystyrene microspheres were first prepared by dispersion polymerization and swelled in chloroform. Then, ferric oleate was dispersed in chloroform as a precursor and impregnated into the swollen polymer microspheres. Subsequently, the iron oxide nanoparticles were formed within the polymer matrix by thermal decomposition of ferric oleate. The morphology, inner structure, and magnetic properties of the magnetic polymer microspheres were studied with a field emission scanning electron microscope (SEM), transmission electron microscope (TEM), and superconducting quantum interference device (SQUID) magnetometer. The results showed that the average diameter of the magnetic polymer microspheres was 5.1 mu m with a standard deviation of 0.106, and the magnetic polymer microspheres with saturation magnetization of 12.6 emu/g exhibited distinct superparamagnctic characteristics at room temperature. More interestingly, the magnetite nanoparticles with a spinel structure are evenly distributed over the whole area of the polymer microspheres. These magnetic polymer microspheres have potential applications in biotechnology.