The use of agro-industrial wastes to obtain compounds with a high added-value is increasing in the last few years in accordance with the circular economy concept. In this work, a cascade extraction approach was developed based on ultrasound-assisted extraction (UAE) for tomato, watermelon, and apple peel wastes. The protein and antioxidant compounds were obtained during the first extraction step (NaOH 3 wt.%, 98.6 W, 100% amplitude, 6.48 W/cm2, 6 min). The watermelon peels (WP) showed higher proteins and total phenolic contents (857 ± 1 mg BSA/g extract and 107.2 ± 0.2 mg GAE/100 g dm, respectively), whereas the highest antioxidant activity was obtained for apple peels (1559 ± 20 µmol TE/100 g dm, 1767 ± 5 µmol TE/100 g dm, and 902 ± 16 µmol TE/100 g dm for ABTS, FRAP and DPPH assays, respectively). The remaining residue obtained from the first extraction was subsequently extracted to obtain cutin (ethanol 40 wt.%, 58 W, 100% amplitude, 2 W/cm2, 17 min, 1/80 g/mL, pH 2.5). The morphological studies confirmed the great efficiency of UAE in damaging the vegetal cell walls. WP showed a higher non-hydrolysable cutin content (55 wt.% of the initial cutin). A different monomers’ profile was obtained for the cutin composition by GC-MS, with the cutin from tomato and apple peels being rich in polyhydroxy fatty acids whereas the cutin extracted from WP was mainly based on unsaturated fatty acids. All of the cutin samples showed an initial degradation temperature higher than 200 °C, presenting an excellent thermal stability. The strategy followed in this work has proved to be an effective valorization methodology with a high scaling-up potential for applications in the food, pharmaceutical, nutraceutical, cosmetics and biopolymer sectors.

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