Four samples of modified titanium dioxide (TiO2), Fe/TiO2(2 wt%), Fe/TiO2(5 wt%), and 5-ALA/TiO2, were experimented in photodynamic therapy (PDT) on leukemia cells HL60, performing promising photocatalytic inactivation effect. Fe/TiO2and 5-ALA/TiO2were synthesized in methods of precipitation and ultrasonic methods, respectively. X-ray diffraction spectra and UV-Vis spectra were studied for the samples’ crystalline phase and redshift of absorption peak. Further, FTIR spectra and Raman spectra were obtained to examine the combination of 5-aminolevulinic (5-ALA) and TiO2nanoparticles. The toxicity of these four kinds of nanoparticles was studied through darkroom experiments. And based on the concentration which caused the same toxic effect (90%) on HL60, PDT experiments of TiO2, Fe/TiO2(2%), Fe/TiO2(5%), and ALA/TiO2were done, resulting in the fact that the photokilling efficiency was 69.7%, 71.6%, 72%, and 80.6%, respectively. Scanning electron microscope (SEM) images of the samples were also taken to study the morphology of HL60 cells before and after PDT, resulting in the fact the activation of the modified TiO2from PDT was the main cause of cell apoptosis.