The present invention provides a method of producing particles from solution-in-supercritical fluid or compressed gas emulsions. In accordance with the method of the invention, a solution that includes a solute dissolved in a solvent is contacted with supercritical fluid or compressed gas to form a solution-in-supercritical fluid or compressed gas emulsion. The emulsion is sprayed through an orifice to create spray droplets. The supercritical fluid or compressed gas and the solvent are removed from the spray droplets resulting in the formation of particles that include the solute. In one embodiment of the invention, the solvent is removed from the spray droplets by lyophilization. In another embodiment of the invention, the solvent is removed from the spray droplets by evaporation.