The orange byproduct is a widely accessible and valuable source of functional phenolic compounds, particularly hesperidin. Hesperidin extraction remains a challenging phase in its valorization chain due to its low solubility and limited extractability in solvents. This work aims to examine the effect of conventional solvent extraction (CSE) compared to emerging and innovative extraction methods: accelerated solvent extraction (ASE) and ultrasound-assisted extraction (UAE) when applied with or without a pretreatment process of instant controlled pressure drop (DIC) to intensify extraction, antioxidant, and antidiabetic activities. The total phenols, flavonoids, hesperidin contents, radical scavenging activities, iron chelating activity, and in vitro α-amylase inhibition of the extracts were determined for CSE (80%, 70 °C), UAE (ethanol 80%, 70 °C, 200 W), and ASE (ethanol 60%, 100 °C, 100 bars) with or without DIC pretreatment (pressure = 0.4 MPa, total thermal time = 30 s). The hesperidin amounts obtained were 0.771 ± 0.008 g/100 g DM, 0.823 ± 0.054 g/100 g DM, and 1.368 ± 0.058 g/100 g DM, for CSE, UAE, and ASE, respectively. DIC pretreatment of orange byproducts increased hesperidin recovery by 67%, 25.6%, and 141% for DIC-CSE, DIC-UAE, and DIC-ASE, respectively. The DPPH and ABTS radical scavenging and iron chelating activities of extracts were also significantly enhanced, and the in vitro antidiabetic activity of extracts was preserved.

This study aimed to investigate the effect of an innovative ecofriendly process—instant controlled pressure drop technology, also known as “détente instantanée contrôlée” or DIC—coupled with Tripolium extraction (DIC-Tripolium), on the hesperidin recovery, and antioxidant and antidiabetic activities of orange byproduct extracts. A DIC pretreatment was applied to partially dried orange byproducts (~16% wet basis). A central composite rotatable design (CCRD), composed of 13 experimental trials (four factorial points, four-star points, and five repetitions for the central point), was followed by a Tripolium process consisting of successive intermittent extraction periods using ethanol/water solvent at 20 ± 1 °C, 5 kPa for 5 min and m/v ratio = 5 g/50 mL. The DIC pretreatment, coupled with the Tripolium process, increased the extractability of hesperidin (from 1.55- to 4.67-fold compared to untreated DIC orange byproducts). The radical scavenging activities of the extracts were also enhanced or preserved in different DIC–Tripolium extracts. The α-Amylase inhibition percentage varied between 55.6 ± 0.02 and 88.30 ± 0.01% according to DIC–Tripolium conditions. The multi-criteria optimized condition of DIC–Tripolium extraction, allowing for the maximization of the hesperidin content, radical scavenging activities, iron chelating activity, and α-amylase inhibition of extracts, corresponds to a DIC saturated steam pressure of 599.4 kPa and a DIC pretreatment time of 38 s.