Aqueous dispersions of gold and silver nanoparticles (NPs) stabilized with sodium citrate, as well as polymeric NPs based on poly(lactide- co -glycolide) (70 : 30 mol %) stabilized with poly(vinyl alcohol) have been obtained. The sizes of NPs have been determined by transmission electron microscopy (TEM), dynamic light scattering (DLS), and analytical ultracentrifugation (AUC). It has been shown that the diameter of both metallic and polymeric particles measured by TEM is significantly lower than their hydrodynamic diameter D _h determined by DLS. Moreover, it has been found that the D _h value obtained for the studied particles from DLS distributions is overestimated compared to that determined by AUC, because the AUC method is less sensitive to the particle size polydispersity and the presence of large objects in a dispersion.