The purpose of this study was to investigate the formation mechanism of colloidal nanoparticles after dispersion of probucol/polyvinylpyrrolidone (PVP)/sodium dodecyl sulphate (SDS) ternary ground mixture (GM) into water. Probucol, PVP and SDS were mixed at a weight ratio of 1:3:1 and ground for 30 min with a vibrational rod mill. The morphology and physicochemical properties were investigated through high resolution scanning electron microscopy (SEM), environmental SEM, dynamic light scattering, C-13 NMR and zeta potential measurements. SEM images confirmed the presence of 20 nm size primary particles in the GM powder of probucol/PVP K17/SDS. Spherical nanoparticles with a size of around 100 nm, formed after dispersion of the GM into water, suggested an agglomeration of the primary particles. A further agglomeration of around 160 nm was observed with the stability experiment. Zeta potential and particle size measurements using latex beads revealed that PVPK 17/SDS complex was adsorbed on the probucol particle surface forming a layered structure. A similar agglomeration behavior was observed using the GM of probucol/PVP K12/SDS, though the molecular state of the PVPK 12/SDS complex at the particle surface was different from that of the PVPK 17/SDS complex. C-13 NMR results suggested that intermolecular interactions between PVP K12 and SDS did not reach the same level as the interactions between PVP K17 and SDS. This study proposed a formation mechanism of colloidal nanoparticles. (C) 2007 Elsevier B.V. All rights reserved.