A novel process configuration of supercritical assisted atomization (SAA) was used to produce microparticles of two model thermolabile compounds: poly l-lactide (PLLA) and bovine serum albumin (BSA). This new configuration allowed to operate the precipitation process below the atmospheric pressure, to perform the drying process at lower temperatures without any damage to thermolabile materials. Process parameters, such as gas to liquid ratio and precipitation temperature, were investigated to evaluate their influence on particle size and morphology. Well defined spherical particles were produced. PLLA microparticles coalescence was avoided using a precipitation pressure from 0.65 to 0.5 bar producing particles with a mean diameter betwee...