New preparation condition of magnetic microcapsule was designed and optimized by response surface methodology(RSM) in this study. The optimal formula was as follows: the concentration of chitosan(CTS), magnetofluid(MHD), calcium chloride(CaCl2) and sodium alginate solution(ALG) were 10.4(g/L),4.83(g/L), 5.625(g/L), and 28(g/L),respectively. The optimized magnetic microcapsules had good slow release effect, and the release time of magnetic microcapsule was up to 100 h. The chemical structure of magnetic microcapsules was determined by Fourier transform infrared(FT-IR) spectrometer. Meanwhile, the chemical composition of the magnetic microcapsule was determined by X-ray diffraction(XRD) instrument.Thermogravimetric analysis(TGA) was used to detect the thermal properties. The properties of anti-oxidation and drug release of the magnetic microcapsules were further analyzed. Most importantly, magnetic microcapsules had superparamagnetism with extremely low magnetic retention and coercivity, which could be used as a good microcapsule embolization agent for tumor endovascular embolization therapy.