In this study we explored the implementation of the vapor induced phase separation (VIPS) to produce cellulose acetate microcapsules for the encapsulation of a complex mix of fragrances. VIPS is a technique used for membrane preparation, but barely mentioned for microencapsulation. We compared the products from VIPS and a more common microencapsulation process, the immersion precipitation technique (IPS). The capsules prepared via VIPS show a core-shell structure with a thin polymeric shell surrounding the internally empty space, conversely to those produced via IPS, showing an incomplete spherical morphology. This can be attributed to a better control of the precipitation rate of the encapsulation material in the non-solvent thanks to the longer exposition time to the vapor. The activity and encapsulation efficiency of the capsules, obtained through TGA analysis, reached a maximum of ≈75% and ≈90%, respectively. Moreover, a growing trend between the initial active concentration and the encapsulation efficiency is noticed.