Savan sc250exp speed vac

A conventional solid–liquid extraction was used to evaluate the biophenols contained in PPP before and after its thermal treatment at 180 °C for 20 min. A total of 3 g of the sample was added with 30 mL of 80:20 ethanol:water extraction solvent, kept for 30 min and decanted. The supernatant phase was magnetically stirred at room temperature for 1 h. Then, the suspensions were centrifuged at a relative centrifugal force (RCF) of 12,499 for 15 min at 4 °C in a Sorvall ST 16 R centrifuge (Thermo Scientific, Leicestershire, UK) and the supernatants dried at 35 °C in the Savan SC250EXP Speed-Vac (Thermo Scientific, Leicestershire, UK). The total phenolic amount present was measured by the Folin–Ciocalteu assay in agreement with Hrncirik and Frische [27 (link)]. The flavonoid content was determined as described in [28 (link)]. The extraction procedure was carried out in triplicate.

Sample extraction was carried out by maceration with solvents considered as Green (environmentally friendly) and GRAS (Generally Recognized As Safe), allowed for food use. In this sense, different proportions of two solvents with these characteristics, water and ethanol, were assayed. Concretely, pure solvents and aqueous mixtures with 50 and 80% ethanol were tested. For all the experiments, 50 mL of the extraction solvent was mixed with 1.5 g of each dry plant, and the mixture was shaken in a vortex for 30 s. After that, solutions were maintained in agitation at room temperature for 1 h. Supernatants were removed with two subsequent centrifugation cycles at 12,096× g RCF for 10 min. Liquid extracts were evaporated to dryness at 35 °C in a Savan SC250EXP Speed-Vac (Thermo Scientific, Loughborough, Leicestershire, UK). Extracts were stored at −20 °C until further use. All the extractions were performed in duplicate in order to assure repeatability. Extraction yields are presented in Table S2, in Supplementary Materials.

Vacuum-drying of hydro-alcoholic filter cake extract. The PLE extracts were dried under a vacuum in a Savan SC250EXP Speed-Vac (Thermo Scientific, Leicestershire, UK) operating at 13 kPa and 35 °C.
Spray-drying of hydro-alcoholic filter cake extract. A laboratory spray-dryer (4M8-TriX Spray-Dryer, Procept, Zelzate Belgium) equipped with a peristaltic pump; a bifluid nozzle; a heater; drying, atomizing and cyclone gases (air); and a dry product collector was used for the spray-drying process. The drying parameters were: inlet air flow (0.35 m³/min), air flow atomizing nozzle (0.013 m³/min), inlet and outlet air temperatures (110 and 49 °C, respectively), pump speed (2 mL/min) and differential pressure over cyclone (15 mBar).
Freeze-drying of hydro-alcoholic filter cake extract. The freeze-drying process was carried out in a laboratory-scale freeze-dryer (Virtis SP Scientific, Thermo Fisher, Spain). Primary drying began with P = 400 Torr and T = −45 °C and ended at atmospheric pressure (AP) and T = 0 °C. Secondary drying had a starting point with AP and T = 0 °C, and a set point with AP and T = 25 °C. Each drying system was carried out in triplicate.