Spray-dried microparticles with lipid cores that dissolve beta-carotene were prepared using a technique based on the complexation of soy protein and gum acacia. A freeze-pretreatment was applied to modify the resultant properties of the dried particles. An oil in water emulsion stabilized by soy protein isolate was mixed with gum acacia. The pH of the solution was adjusted to a selected value; this solution was frozen and thawed under controlled thermal protocols, then spray-dried to obtain the final products. Complexation was induced on the surface of the oil droplets owing to electrostatic interactions that occur below the isoelectric point (ca. pH 4.0) of the employed soy protein isolate. The freeze-pretreatment prior to spray-drying was expected to induce this interaction by freeze concentration and to control the kinetics of complex formation. When solutions with a pH of 4.0 and 3.0 were spray-dried, the encapsulation of beta-carotene had similar efficiencies. The freeze-pretreatment was observed to have a significant effect on the specimens prepared from the solution with a pH of 4.0. Slow freezing conditions successfully improved the encapsulation efficiency and simultaneously reduced the amount of surface oil. Moreover, this pretreatment augmented the mass transfer resistance of the shell matrix, so that the release rate of dissolved beta-carotene in the lipid core could be retarded.