Microencapsulation has been successfully implemented in various fields of science. It can be used to remove, protect, preserve and disseminate many substances. The objective of this work is to investigate the vanillin release from polysulfone macrocapsules as a first approach to characterize microcapsules afterward. The capsules were synthesized from polysulfone as polymer, dimethyl formamide as solvent, and vanillin as active agent, by phase inversion precipitation. Morphological characterization was made by scanning electron microscopy. Vanillin release from the capsules was monitored by withdrawing samples, from the release medium, at different time intervals. The vanillin concentration was determined by high performance liquid chromatography. Vanillin release from capsules was encountered to increase when increasing the stirring rate or when increasing the temperature of the release medium. Total amount of vanillin encapsulated was estimated by sequentially refreshing the release medium and corresponded to ca. 50% of the perfume initially incorporated in the polymeric solution.