This paper describes a method of fabrication and photocatalytic characterization of TiO2 nanostructures such as powders, tubes and films. The TiO2 nanotubes and films were fabricated by hydrothermal method from commercial powders and DC magnetron sputtering. In this study, the terephthalic acid (AT) solution was used as a "probe" fluorescence and Methylene Blue (MB) solution as a colour indicator to indentify the generation of OH hydroxyl and superoxide O2- radicals in photocatalytic reaction. It shows that the method based on MB and AT solutions is of high reliability, suitable for preparation of TiO2 powders, tubes and films. With 25 mg TiO2 nanostructures, the photocatalytic properties of nanotubes are better than those of the films and precursor powders.