A single droplet drying acoustic levitator has been used to examine the drying behavior of droplets of pharmaceutically relevant solutes used to produce protein-loaded particles via spray-drying. The drying behavior of solution droplets of mannitol, trehalose, or catalase was determined. Evidence of super-saturation of the solute in the droplet surface up to the critical point of drying was obtained. The trehalose achieves a lower degree of super-saturation than does the mannitol before precipitating at the droplet surface. This results in a shorter duration of the constant-rate period, but protracted further drying of this amorphous material. Mannitol achieved a higher degree of super-saturation, and a later critical point with shorter falling-rate period. Measurements of dried particle radius showed that both solutes form hollow particles. The catalase formed holed, hollow particles with characteristic drying rate profiles that correlated well with developing particle morphology. A strong similarity between the morphologies of dried particles of mannitol, trehalose, or catalase produced either in the levitator or in a spray-dryer was found.