Mesoporous silica shell was formed onto supermagnetic Fe3O4 nanoparticles to produce magnetic core-mesoporous shell silica spheres (MCMSS) by using anionic surfactant for the first time in two-pot synthesis route. Costructure directing agent (CSDA) has assisted the electrostatic interaction between the partially negatively charged silica particles and the negatively charged surfactant through S(-)N(+)1(-) pathway. Impact of synthesis parameters on shell thickness, BET surface area, pore volume, and pore ordering was studied. The particles synthesized in this work have a uniformly coated thin mesoporous shell and showed a slow drug release rate that extend over 12 h which represent promising performance in drug controlled release application.