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This study used high-pressure extraction to obtain antioxidant-rich fractions from Desmodium canadense leaves harvested at five vegetation phases (intensive growing to end of blooming) and to evaluate their antioxidant activity and phytochemical profile. Supercritical CO2 extraction recovered lipophilic compounds, with the highest yield at massive flowering. The remaining plant material was fractionated by pressurized liquid extraction (PLE) using acetone, ethanol, and water; the highest PLE yield was achieved with water (16.54 g/100 g DW) at the bud formation stage. Antioxidant capacity was measured using total phenolic content (TPC) and ABTS•+, CUPRAC, and ORAC assays. Overall, ethanol PLE extracts showed the strongest antioxidant properties: maximum TPC (282.1 mg GAE/gE) and ABTS•+ (1010 mg TE/gE) at massive flowering, and highest CUPRAC (853.3 mg TE/gE) and ORAC (1882 mg TE/gE) at bud formation. UPLC-Q-TOF-MS/MS profiling identified 37 compounds, mainly C-glycosyl flavones, flavonol O-glycosides, hydroxycinnamic acid derivatives, and low molecular weight organic acids. Water extracts were rich in low molecular weight organic acids, while acetone and ethanol extracts contained the highest flavonoid levels. Citric acid and vitexin were the most abundant compounds. The findings indicate that D. canadense leaves, especially harvested at budding through massive flowering, are a promising source of flavonoid-rich antioxidant extracts for nutraceutical and functional food applications.

Fruit processing by-products contain various classes of bioactive constituents, which may find applications as ingredients for foods, nutraceuticals or cosmeceuticals. This study explored the fractionation of lipophilic rowanberry pomace extracts isolated with pure supercritical CO2 and its mixtures with a co-solvent ethanol by their on-line separation at subcritical conditions. Rowanberry pomace lipids were extracted with supercritical CO2 (42.4 MPa, 53 °C) using 0–7% of ethanol, and then fractionated by reducing the first separator’s (S1) pressure to 7 MPa and cooling it to 0, −10 and −20 °C to precipitate the ‘heavier’ fraction (HF). The second separator (S2) was depressurized at ambient temperatures to collect the ‘lighter’ fraction (LF). The yield of the LF increased by decreasing the S1 temperature and increasing the amount of the co-solvent. The concentration of β-carotene was increased in the LF by decreasing the S1 temperature and increasing the co-solvent concentration; at −20 °C it was 66.7% higher than in the non-fractionated extract. The concentrations of tocopherols and phytosterols were also remarkably higher in the LF. In total, 62 compounds were identified in the headspace volatile fraction of the LF, benzaldehyde and benzyl alcohol being the most abundant constituents. In conclusion, fractionation enabled us to obtain fractions with higher concentrations of the selected classes of lipophilic rowanberry constituents.

Novel ingredients from rowanberry pomace were developed for French-type bread applications via supercritical CO2 extraction and the enzymatic and ultrasound treatment of the defatted residue (DFR), which contained 6.367% of proteins, 8.36% of soluble, and 43.04% insoluble fiber. Proteolytic enzymes from Bacillus licheniformis and Aspergillus oryzae, and cellulolytic enzyme mixtures Viscozyme L and Celuclast, were used to increase the soluble fraction. Treating DFR with enzymes generated significant amounts of soluble substances containing oligosaccharides, fructose, and glucose, with Viscozyme L being more effective than proteases. Tri-, and tetrapeptides, chlorogenic acids, and dihydroxy coumarins were also present in the soluble extracts of fermented DFR. The antioxidant characteristics of treated DFR were evaluated by the in vitro assays. Substitution of >5% of wheat flour with untreated DFR significantly reduced bread volume and crumb porosity; however, these adverse effects were mitigated by using fermented DFR. The highest bread volume (1845 cm3) and porosity (78.38%) were observed in bread containing 5% pomace that underwent enzymatic hydrolysis and ultrasound treatment. The substitution of flour with DFR significantly increased the antioxidant characteristics of bread samples and the substances generated during the in vitro digestion. It may be concluded that rowanberry pomace ingredients may improve bread nutritional quality and assist in the sustainable use of fruit processing by-products.

Walnut (Juglans regia L.) shells are valuable agro-industrial by-products rich in polyphenols. This study investigated traditional (maceration) and advanced extraction techniques—ultrasound-assisted extraction (UAE), enzyme-assisted extraction (EAE), pressurized liquid extraction (PLE), and combined ultrasound–enzyme extraction (US-EAE)—to recover bioactive compounds from walnut shells. Extraction efficiency, total phenolic content (TPC), antioxidant capacity (ABTS•+, DPPH•), and polyphenol composition were evaluated. UPLC-ESI-MS/MS identified key polyphenols including ellagic acid, 4-hydroxybenzoic acid, vanillin, taxifolin, and quercitrin. The highest TPC (5625 mg GAE/100 g dw) was found in extracts subjected to US-EAE, in which ultrasound pretreatment (200 W, 10 min) was followed by enzymatic extraction using 0.06 mL/g Viscozyme® L at pH 3.5 and 45 °C. Under the same extraction conditions, UAE alone yielded the second highest TPC (4129 mg GAE/100 g dw). The highest ABTS•+ scavenging activity (14,478 mg TE/100 g dw) and enhanced DPPH• activity (45.38 mg TE/100 g dw) were also observed in US-EAE extracts. Chemometric techniques (PCA and HCA) revealed meaningful clustering and variation patterns among methods. These findings highlight the potential of walnut shells as a sustainable source of polyphenols and demonstrate the effectiveness of innovative extraction technologies in maximizing bioactive compound recovery for potential functional applications.

This study used high-pressure extraction to obtain antioxidant-rich fractions from Desmodium canadense leaves harvested at five vegetation phases (intensive growing to end of blooming) and to evaluate their antioxidant activity and phytochemical profile. Supercritical CO[sub.2] extraction recovered lipophilic compounds, with the highest yield at massive flowering. The remaining plant material was fractionated by pressurized liquid extraction (PLE) using acetone, ethanol, and water; the highest PLE yield was achieved with water (16.54 g/100 g DW) at the bud formation stage. Antioxidant capacity was measured using total phenolic content (TPC) and ABTS[sup.•+], CUPRAC, and ORAC assays. Overall, ethanol PLE extracts showed the strongest antioxidant properties: maximum TPC (282.1 mg GAE/gE) and ABTS[sup.•+] (1010 mg TE/gE) at massive flowering, and highest CUPRAC (853.3 mg TE/gE) and ORAC (1882 mg TE/gE) at bud formation. UPLC-Q-TOF-MS/MS profiling identified 37 compounds, mainly C-glycosyl flavones, flavonol O-glycosides, hydroxycinnamic acid derivatives, and low molecular weight organic acids. Water extracts were rich in low molecular weight organic acids, while acetone and ethanol extracts contained the highest flavonoid levels. Citric acid and vitexin were the most abundant compounds. The findings indicate that D. canadense leaves, especially harvested at budding through massive flowering, are a promising source of flavonoid-rich antioxidant extracts for nutraceutical and functional food applications.

Fruit processing by-products contain various classes of bioactive constituents, which may find applications as ingredients for foods, nutraceuticals or cosmeceuticals. This study explored the fractionation of lipophilic rowanberry pomace extracts isolated with pure supercritical CO[sub.2] and its mixtures with a co-solvent ethanol by their on-line separation at subcritical conditions. Rowanberry pomace lipids were extracted with supercritical CO[sub.2] (42.4 MPa, 53 °C) using 0–7% of ethanol, and then fractionated by reducing the first separator’s (S1) pressure to 7 MPa and cooling it to 0, −10 and −20 °C to precipitate the ‘heavier’ fraction (HF). The second separator (S2) was depressurized at ambient temperatures to collect the ‘lighter’ fraction (LF). The yield of the LF increased by decreasing the S1 temperature and increasing the amount of the co-solvent. The concentration of β-carotene was increased in the LF by decreasing the S1 temperature and increasing the co-solvent concentration; at −20 °C it was 66.7% higher than in the non-fractionated extract. The concentrations of tocopherols and phytosterols were also remarkably higher in the LF. In total, 62 compounds were identified in the headspace volatile fraction of the LF, benzaldehyde and benzyl alcohol being the most abundant constituents. In conclusion, fractionation enabled us to obtain fractions with higher concentrations of the selected classes of lipophilic rowanberry constituents.

This study used high-pressure extraction to obtain antioxidant-rich fractions from leaves harvested at five vegetation phases (intensive growing to end of blooming) and to evaluate their antioxidant activity and phytochemical profile. Supercritical CO extraction recovered lipophilic compounds, with the highest yield at massive flowering. The remaining plant material was fractionated by pressurized liquid extraction (PLE) using acetone, ethanol, and water; the highest PLE yield was achieved with water (16.54 g/100 g DW) at the bud formation stage. Antioxidant capacity was measured using total phenolic content (TPC) and ABTS , CUPRAC, and ORAC assays. Overall, ethanol PLE extracts showed the strongest antioxidant properties: maximum TPC (282.1 mg GAE/gE) and ABTS (1010 mg TE/gE) at massive flowering, and highest CUPRAC (853.3 mg TE/gE) and ORAC (1882 mg TE/gE) at bud formation. UPLC-Q-TOF-MS/MS profiling identified 37 compounds, mainly C-glycosyl flavones, flavonol O-glycosides, hydroxycinnamic acid derivatives, and low molecular weight organic acids. Water extracts were rich in low molecular weight organic acids, while acetone and ethanol extracts contained the highest flavonoid levels. Citric acid and vitexin were the most abundant compounds. The findings indicate that leaves, especially harvested at budding through massive flowering, are a promising source of flavonoid-rich antioxidant extracts for nutraceutical and functional food applications.

Fruit processing by-products contain various classes of bioactive constituents, which may find applications as ingredients for foods, nutraceuticals or cosmeceuticals. This study explored the fractionation of lipophilic rowanberry pomace extracts isolated with pure supercritical CO and its mixtures with a co-solvent ethanol by their on-line separation at subcritical conditions. Rowanberry pomace lipids were extracted with supercritical CO (42.4 MPa, 53 °C) using 0-7% of ethanol, and then fractionated by reducing the first separator's (S1) pressure to 7 MPa and cooling it to 0, -10 and -20 °C to precipitate the 'heavier' fraction (HF). The second separator (S2) was depressurized at ambient temperatures to collect the 'lighter' fraction (LF). The yield of the LF increased by decreasing the S1 temperature and increasing the amount of the co-solvent. The concentration of β-carotene was increased in the LF by decreasing the S1 temperature and increasing the co-solvent concentration; at -20 °C it was 66.7% higher than in the non-fractionated extract. The concentrations of tocopherols and phytosterols were also remarkably higher in the LF. In total, 62 compounds were identified in the headspace volatile fraction of the LF, benzaldehyde and benzyl alcohol being the most abundant constituents. In conclusion, fractionation enabled us to obtain fractions with higher concentrations of the selected classes of lipophilic rowanberry constituents.