Alginate microspheres loaded with superparamagnetic iron oxide nanoparticles (SPIO NPs) have been fabricated by a T-junction microfluidic device combined with an external ionic crosslinking. The obtained microspheres possess excellent visuality under magnetic resonance due to the presence of only 0.6 mg/mL SPIO NPs. The microspheres also show uniform size with narrow distribution and regular spherical shape characterized by optic microscope and environmental scanning electron microscope. Furthermore, dual drugs (5-fluorouracil and doxorubicin hydrochloride) have been loaded within the microspheres. The release behavior of dual drugs from the microspheres show typical sustained release profiles. As a novel embolic agent, such microspheres in blood vessels can be tracked by magnetic resonance scanner. Thus, the integration of embolotherapy, chemotherapy, and postoperative diagnosis can be realized.