Abstract A new approach for the production of microspheres from oil-in-water (O/W) emulsions using supercritical fluids is presented. The composition of the emulsions, consisting of 1-monoacylglycerol (1-MAG) and polyvinylalcohol (PVA) was first optimized, then supercritical assisted atomization (SAA) was applied to produce dried microparticles. The effect of different 1-MAG/PVA ratios and emulsion preparation method on size, stability, and morphology of microparticles was investigated using scanning electron microscopy, dynamic light scattering, differential scanning calorimetry and X-ray diffraction. The emulsion composition and emulsification method affected the sizes of microparticles and the smallest 1-MAG/PVA microparticles were obtained at lower 1-MAG (<30 mg/mL) and \{PVA\} (6 mg/mL) concentrations. Prepared 1-MAG/PVA microparticles had a spherical morphology with mean diameter ranging from 0.5 to 3 μm and a semi-crystalline structure. A maximum microparticle recovery of 55% was obtained.