The global sustainability policy emphasizes reusing of agri-food waste and by-products to enhance food bioactive properties. Thus, brioches were processed incorporating almond skin powder (ASP): control (CTR), without ASP addition; 5-ASP, with 5% (w/w) ASP; and 10-ASP, with 10% (w/w) ASP. Seven different brioches shapes were obtained for each recipe. Flavonoids were mainly detected in Tuono almond skin by Ultra-High Performance Liquid Chromatography coupled to High-Resolution Mass Spectrometry (UHPLC-HRMSMS), in particular, flavan-3-ol monomers. The ethanolic extract of Tuono almond skins contained polar lipids (oxylipins and phospholipids). Gas Chromatography–Mass Spectrometry (GC-MS) identified six major fatty acids, mainly oleic acid (48.01%). Photothermal degradation impact on bioactive compounds was evaluated using a first-order kinetic model. Antioxidant activity was studied using 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid), 2,2-diphenyl-1-picrylhydrazyl and β-carotene bleaching test. α-amylase, α-glucosidase, and lipase inhibitory effect were also tested. The acidification of the doughs was consistent across all trials. Lactic acid bacteria and yeast levels increased. Importantly, the final products were free from undesirable microorganisms. The addition of ASP led to reduced weight loss and specific volume for all seven brioche types. Furthermore, the firmness, crumb structure, and sensory profile of the final products were noticeably influenced. Tasters clearly favoured the Treccina brioches. The production of sweet leavened baked goods was carried out in triplicate in two independent experiments. The statistical model applied to the data considered the effects of brioche shape and the addition of ASP. Kinetic data revealed that the half-life extension for both total phenol and flavonoid content was observed in the 10-ASP sample (18.00382). 10-ASP sample exhibited promising ABTS radical scavenging activity, with inhibitory concentration 50% (IC50) values of 18.64 mg/mL after 9 days of photothermal degradation. Moreover, when testing 10-ASP Treccina against α-amylase and α-glucosidase, the IC50 values were 198.16 and 190.23 μg/mL, respectively, even after 9 days.
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