Films based on TiO2 nanoparticles (NPs) have been successfully used as sensing elements in chemical sensors. TiO2 Colloidal suspensions can be obtained by spontaneous hydrolysis in acidic solutions of Ti(IV) compounds. The obtained TiO2 NPs can be employed to build up nanostructured films. With the purpose of preparing TiO2-based nanostructured, imprinted materials as sensing elements for piezoelectric sensors, we obtained TiO2 NP dispersions by hydrolyzing potassium titanyl oxalate in the presence of a target analyte (tyrosine). Since morphological properties of the synthesized NPs are known to influence the nanostructured film characteristics, an analytical strategy to characterize such colloidal systems can combine a size-based separation method with spectroscopic analysis to correlate the particle size distribution (PSD) with the particle-target interaction properties able to determine the sensing efficiency.