| Summary: | Valorizing agri-food industrial waste is essential for a circular economy, yielding high-value products, waste reduction, technological solutions, employment opportunities, and enhanced food security. This work shows the valorization of seeds generated as residues from the agri-food industries of guava <i>pera</i> (<i>Psidium guajava</i>) and Tommy Atkins mango (<i>Mangifera indica</i> L.), through extraction with supercritical carbon dioxide (scCO<sub>2</sub>). After the optimization of the initial solid condition of the raw material (i.e., particle size and moisture content), scCO<sub>2</sub> pressure and temperature were established through the response surface methodology (RSM) to obtain an oily extract with the highest content in bioactive compounds of commercial relevance, as well as with a high antioxidant capacity. The total amount of oily extract in guava and mango seeds was 14% and 9%, respectively, while the maximum recovery of supercritical extract was 95% from guava seeds at 38 MPa and 50 °C, and 88% from mango seeds at 37 MPa and 63 °C. Bioactive fractions rich in squalene, γ-tocopherol, α-tocopherol, campesterol, β-sitosterol, and stigmasterol were obtained. The best supercritical extraction conditions, in terms of the bioactive fractions richest in minor compounds, were at 17 MPa and 50 °C for guava seeds and at 23 MPa and 63 °C for mango seeds. At these conditions, the highest antioxidant capacities were also found for the extracts. Thus, these bioactive fractions could be used in a variety of products in the cosmetic, food, pharmaceutical, and medical activities due to the beneficial properties of the identified compounds in health as antioxidants, anti-inflammatories, and cholesterol reducers.
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