The objective of this work is to access the release behavior of thymol and p-cymene used as model core materials with PLA microcapsules. The microcapsules were obtained by a coacervation process developed in a previous work and present a spherical shape with mean particle size of 25 and 37 μm for thymol and p-cymene, respectively. The results have shown that the release of thymol and p-cymene is faster in the first hour keeping almost constant in the subsequent days. The diffusion coefficient in the first hour of release was 1.99 × 10–16 m2/s for thymol and 4.34 × 10–16 m2/s for p-cymene. However, the diffusion was slower if considering a period of 5 days being the diffusion coefficients of 3.34 × 10–19 m2/s for thymol and 3.45 × 10–18 m2/s for cymene.