Hollow mesoporous silica nanospheres (HMSN) were prepared through simple steps using iron oxide nanoparticles and CTAB as templates, which were removed by refluxing in acidic solution. Hollow structure of HMSN was confirmed by TEM and XRD, while N₂ adsorption-desorption study indicated mesoporous structure of the nanospheres. Gold shells on hollow mesoporous silica nanospheres (GHMSN) were also prepared using gold nanoparticles as seeds and HAuCl₄ solution as a source of Au ions, which were subsequently reduced on the surface. The prepared nanospheres indicated good biocompatibility even at very high concentration. Doxorubicin (Dox) as anticancer drug was loaded into both nanospheres which showed a pH-responsive release. Both nanospheres were applied for the treatment of human cervical cancer cells (HeLa). Results proved the effectiveness of both nanospheres in treatment of cancer cells, while GHMSN showed synergistic therapeutic effect due to Dox as chemotherapy and gold shells as photothermal therapy, using moderate power density of near-infrared (NIR) light radiation.