The synthesis of titania nanoparticles within thermally evaporated octadecylamine (ODA) thin films is described. Synthesis of the nanoparticles was achieved by electrostatically entrapping TiF62- ions in thin films of the fatty amine by a simple immersion technique followed by in-situ hydrolysis of the metal ions. Without any further heat treatment, it was observed that titania nanoparticles of the brookite polymorph were formed within the film. By this simple procedure, uniformly distributed fairly monodisperse titania nanoparticles of ca. 4 nm diameter were synthesized within the lipid matrix and investigated using a host of techniques.