This work is focused on the chemical characterization of Maytenus ilicifolia extracts obtained from high-pressure CO2 extraction. The experiments were performed in a laboratory-scale unit, where the effect of particle size (35-200 mesh), CO2 mass flow rate (1-3 g/min), temperature (293-323 K), pressure (100-250 bar), and extraction time was investigated in terms of liquid yield and chemical composition of the extracts. Results show that the particle size and CO2 mass flow rate did not affect the liquid yield, whereas the extraction temperature and solvent density exerted a pronounced effect on both liquid yield and chemical distribution of volatile compounds. The extracts were chemically analyzed with regard to phytol, squalene, vitamin E, stigmasterol, friedelan-3-ol, friedelin, dodecanoic acid and geranyl acetate in a GC/MSD.