The doping TiO2 were prepared by hydrothermal method with two different nonmetal, that is N-doped, and N, S codoped. The resulting materials were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS). According to the test result, nitrogen and sulfur co-doped titania give a higher photocatalytic activity in the degradation of organophosphorus pesticide. It was evidenced that the incorporation N in the anatase titania lattice in the form of O–Ti–N linkages. However, we compared with N-doped and N, S codoped it was no reservation to conclude that N, S codoped titania exhibit the further enhanced photocatalytic activity.