Extraction of Phenolic and Flavonoid Compounds from Mung Bean (Vigna radiata L.) Seed Coat by Pressurized Liquid Extraction

Mung bean seed coat (MBC) is a by-product of the mung bean processing industry. It contains a large number of phenolic compounds with therapeutic anti-inflammatory, anti-diabetic and antioxidant properties. This research aimed to investigate the optimum conditions for phenolic and flavonoid extraction from MBC by pressurized liquid extraction (PLE). Response surface methodology (RSM) was used to study the effects of temperature (80–160 °C), pressure (1200–1800 psi) and ethanol concentration (5–95%) on total phenolic content (TPC), total flavonoid content (TFC) and 2,2′-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) scavenging activity (ABTS). Scale-up extraction was also performed. The optimum conditions for extraction were 160 °C, 1300 psi and 50% ethanol. Under optimum conditions, the TPC was 55.27 ± 1.14 mg gallic acid equivalent (GAE)/g MBC, TFC was 34.04 ± 0.72 mg catechin equivalent (CE)/g MBC and ABTS scavenging activity was 195.05 ± 2.29 mg trolox equivalent (TE)/g MBC. The TFC and ABTS scavenging activity of the extracts obtained at the pilot scale (10 L) was not significantly different from the laboratory scale, while TPC was significantly increased. The freeze-dried MBC extract contained vitexin and isovitexin 130.53 ± 17.89, 21.21 ± 3.22 mg/g extract, respectively. In conclusion, PLE was able to extract phenolics, flavonoids with ABTS scavenging activity from MBC with the prospect for future scale-up for food industry.     

Potato By-Products as a Source of Natural Chlorogenic Acids and Phenolic Compounds: Extraction,Characterization, and Antioxidant Capacity

Total phenolic compounds (TPC) and the chlorogenic acids content of potato by-product extracts of two hydro alcoholic solvents (methanol, ethanol) and two extraction methods (maceration and heating-assisted extraction) were studied. The content of TPC in the extracts was determined spectrometrically according to the Folin–Ciocalteu procedure and calculated as chlorogenic acid equivalents. Soluble phenolic acids, especially the chlorogenic acids, were performed by HPLC. The antioxidant activity of potato by-product extracts was determined by using the total oxygen radical absorbance capacity (ORAC) method. The highest content of TPC was found in raw and lyophilized red waters when using ethanol as a solvent around 57 mg/g fresh weight. Heating-assisted extraction enhances this quantitative increasing. At the given operating conditions, unpeeled potato samples exhibit a higher TPC than peeled ones, showing that TPC are accumulated in skin tissue. The greatest amount of chlorogenic acid (Caffeoyl-Quinic Acids, 3, 4, 5 CQA), mainly the 5-CQA (870 ± 39.66 µg/g WM for wet matter versus DM dry matter), was obtained in the pellets and lyophilized fresh peels (skin vs. flesh). In addition, the greatest amounts of chlorogenic acids were found when potato peels were extracted with methanol. Heating-assisted extraction improved the chlorogenic acid concentration of the potato peel extracts. The total ORAC amounts recorded in the different potato fractions varied between 1500 and 1650 µM TE/g. They were higher than those of some fruits, vegetables, nuts, cereals, and sweet potato cultivar. The good correlation coefficient found between TPC, chlorogenic acids determination, and the ORAC capacity indicates that the TPC can be used as a good indicator of the antioxidant capacity of potato by-products.     

Optimization Method for Phenolic Compounds Extraction from Medicinal Plant (Juniperus procera) and Phytochemicals Screening

Juniperus procera is a natural source of bioactive compounds with the potential of antitumor, antimicrobial, insecticidal, antifungal, and antioxidant activities. An optimization method was developed for total phenolic content (TPC), total flavonoid content (TFC), and total tannin content (TTC) in leaf and seed extract of Juniperus procera. Organic solvents (methanol (99.8%), ethanol (99%), and acetone (99.5%)), and deionized water (DI) were used for extraction. The estimation of TPC, TFC, and TTC in plant materials was carried out using UV-spectrophotometer and HPLC with the standards gallic acid, quercetin, and tannic acid. Recovery of TPC in leaf extract ranged from 2.9 to 9.7 mg GAE/g DW, TFC from 0.9 to 5.9 mg QE/g DW, and TTC ranged from 1.5 to 4.3 mg TA/g DW while the TPC value in the seed extract ranged from 0.53 to 2.6 mg GAE/g DW, TFC from 0.5 to 1.6 mg QE/g DW, and TTC ranged from 0.5 to 1.4 mg TA/g DW. This result revealed that methanol is the best solvent for recovery of the TPC value (9.7 mg) from leaf extract in comparison to other solvents. Ethanol recorded the highest result of TFC (5.9 mg) in leaf extract among the solvents whereas acetone was the best for TTC yield recovery from leaf extract (4.3 mg). In the case of the seed extract, ethanol was the best solvent for both TPC (2.6 mg), and TFC (1.6 mg) recovery in comparison to other solvents. Total tannin content in methanol resulted in significant recovery from seed extract (1.4 mg). Separation and quantification of gallic acid, quercetin, and tannic acid in plant materials were undertaken using HPLC. Gallic acid in leaf and seed of J. procera ranged from 6.6 to 9.2, 6.5 to 7.2 µg/g DW, quercetin from 6.3 to 18.2, 0.9 to 4.2 µg/g DW, and tannic acid from 16.2 to 29.3, 6.6 to 9.3 µg/g DW, respectively. Solvents have shown a significant effect in the extraction of phenolic compounds. Moreover, phytochemicals in plant materials were identified using GC-MS and resulted in very important bioactive compounds, which include anti-inflammatory, antibacterial, and antitumor agents such as ferruginol, phenanthrene, and n-hexadecanoic acid. In conclusion, the optimal solvent for extraction depends on the part of the plant material and the compounds that are to be isolated.     

Effect of Encapsulated Beet Extracts (Beta vulgaris) Added to Yogurt on the Physicochemical Characteristics and Antioxidant Activity

Beet has been used as an ingredient for functional foods due to its high antioxidant activity, thanks to the betalains it contains. The effects of the addition of beet extract (liquid and lyophilized) on the physicochemical characteristics, color, antioxidant activity (AA), total betalains (TB), total polyphenols (TP), and total protein concentration (TPC) were evaluated on stirred yogurt. The treatments (T1-yogurt natural, T2-yogurt added with beet juice, T3-added extract of beet encapsulated with maltodextrin, and T4-yogurt added with extract of beet encapsulated with inulin) exhibited results with significant differences (p < 0.05). The highest TB content was observed in T2 (209.49 ± 14.91), followed by T3 (18.65 ± 1.01) and later T4 (12.96 ± 0.55). The highest AA was observed on T2 after 14 days (ABTS˙ 0.819 mM TE/100 g and DPPH˙ 0.343 mM TE/100 g), and the lowest was found on T1 at day 14 (ABTS˙ 0.526 mM TE/100 g and DPPH˙ 0.094 mM TE/100 g). A high content of TP was observed (7.13 to 9.79 mg GAE/g). The TPC varied between 11.38 to 12.56 µg/mL. The addition of beet extract significantly increased AA in yogurt, betalains being the main compounds responsible for that bioactivity.     

Ultrasound-Assisted Water Extraction of Gentiopicroside,Isogentisin, and Polyphenols from Willow Gentian “Dust” Supported by Hydroxypropyl-β-Cyclodextrin as Cage Molecules

The residue after sieving (“dust”) from the willow gentian underground parts is an unexploited herbal tea by-product, although it contains valuable bioactive compounds. Cyclodextrins as efficient green co-solvents, cage molecules, and multifunctional excipients could improve the extraction and contribute to the added value of the resulting extracts. The objective of this study was to determine the optimal conditions for the extraction of gentiopicroside, isogentisin, and total phenolics (TPC) from willow gentian “dust” using ultrasound-assisted water extraction coupled with hydroxypropyl-β-cyclodextrin (HPβCD). The influence of extraction temperature (X₁: 20–80 °C), time (X₂: 20–50 min), and HPβCD concentration (X₃: 2–4% w/v) was analyzed employing the response surface methodology (RSM). The optimal extraction conditions for simultaneously maximizing the extraction yield of all monitored responses were X₁: 74.89 °C, X₂: 32.57 min, and X₃: 3.01% w/v. The experimentally obtained response values under these conditions (46.96 mg/g DW for gentiopicroside, 0.51 mg/g DW for isogentisin, and 12.99 mg GAE/g DW for TPC) were in close agreement with those predicted, thus confirming the suitability and good predictive accuracy of the developed RSM models. Overall, the developed extraction system could be an applicable alternative strategy to improve the extraction of bioactive compounds from the underutilized “dust” of willow gentian underground parts.     

Modelling and Optimization of Ultrasound-Assisted Extraction of Phenolic Compounds from Black Quinoa by Response Surface Methodology

Phenolic compounds are currently the most investigated class of functional components in quinoa. However, great variability in their content emerged, because of differences in sample intrinsic and extrinsic characteristics; processing-induced factors; as well as extraction procedures applied. This study aimed to optimize phenolic compound extraction conditions in black quinoa seeds by Response Surface Methodology. An ultrasound-assisted extraction was performed with two different mixtures; and the effect of time; temperature; and sample-to-solvent ratio on total phenolic content (TPC) was investigated. Data were fitted to a second-order polynomial model. Multiple regression analysis and analysis of variance were used to determine the fitness of the model and optimal conditions for TPC. Three-dimensional surface plots were generated from the mathematical models. TPC at optimal conditions was 280.25 ± 3.94 mg of Gallic Acid Equivalent (GAE) 100 g⁻¹ dm upon extraction with aqueous methanol/acetone, and 236.37 ± 5.26 mg GAE 100 g⁻¹ dm with aqueous ethanol mixture. The phenolic profile of extracts obtained at optimal conditions was also investigated by HPLC. The two extracting procedures did not show different specificities for phenolic compounds but differed in the extraction yield.     

Phenolic Compounds Recovery from Blood Orange Peels Using a Novel Green Infrared Technology Ired-Irrad®, and Their Effect on the Inhibition of Aspergillus flavus Proliferation and Aflatoxin B1 Production

The intensification of total phenolic compound (TPC) extraction from blood orange peels was optimized using a novel green infrared-assisted extraction technique (IRAE, Ired-Irrad^®) and compared to the conventional extraction using a water bath (WB). Response surface methodology (RSM) allowed for the optimization of ethanol concentration (E), time (t), and temperature (T) in terms of extracted TPC and their antiradical activity, for both WB extraction and IRAE. Using WB extraction, the multiple response optimums as obtained after 4 h at 73 °C and using 79% ethanol/water were 1.67 g GAE/100 g for TPC and 59% as DPPH inhibition percentage. IRAE increased the extraction of TPC by 18% using 52% ethanol/water after less than 1 h at 79 °C. This novel technology has the advantage of being easily scalable for industrial usage. HPLC analysis showed that IRAE enhanced the recovery of gallic acid, resveratrol, quercetin, caffeic acid, and hesperidin. IR extracts exhibited high bioactivity by inhibiting the production of Aflatoxin B1 by 98.9%.     

Physicochemical Properties and Antioxidant Activity of Spray-Dry Broccoli (Brassica oleracea var Italica) Stalk and Floret Juice Powders

This research presents the microencapsulation and conservation of antioxidants of broccoli juice processed by spray drying, and proposes the use of a by-product as a technological application. Broccoli juice (BJ) extracted from two sources, stalks and florets, was spray-dried employing maltodextrin (MX) as a carrier agent at concentrations of 5, 7.5, and 10%, and inlet temperatures of 150 and 220 °C. The total phenolic content (TPC), and antioxidant activity (AA) of the BJ-MX powders were determined together with the physicochemical characteristics, including particle morphology, microstructure, and thermal properties. Based on the TPC and AA, the optimal processing conditions found were 5% of MX and a drying temperature of 220 °C. However, the florets showed higher TPC, while stalks presented higher AA under those processing conditions. The particles exhibited micrometric sizes and a mixture of spherical-shape particles and pseudo-spherical particles. The diffractograms indicated an amorphous microstructure in all samples. The glass transition temperature (Tg) was determined in the range of 50 °C for the samples dried at 150 °C and 55 °C for those dried at 220 °C. This suggested that powders might be stored at temperatures below the Tg without presenting any loss of antioxidants.     

Ultrasound-Assisted Extraction of Carotenoids from Carrot Pomace and Their Optimization through Response Surface Methodology

Ultrasound-assisted extraction (UAE) was used to extract carotenoids from the carrot pomace. To investigate the effect of independent variables on the UAE, the response surface methodology (RSM) with central-composite design (CCD) was employed. The study was conducted with three independent variables including extraction time (min), temperature (°C), and ethanol concentration (%). The results showed that the optimal conditions for UAE were achieved with an extraction time of 17 min, temperature of 32 °C, and ethanol concentration of 51% of total carotenoids (31.82 ± 0.55); extraction time of 16 min, temperature of 29 °C, and ethanol concentration of 59% for a combination of β-carotene (14.89 ± 0.40), lutein (5.77 ± 0.19), and lycopene (2.65 ± 0.12). The non-significant (p > 0.05) correlation under optimal extraction conditions between predicted and experimental values suggested that UAE is the more productive process than conventional techniques for the extraction of carotenoids from the carrot pomace.     

Process Optimization of Phytoantioxidant and Photoprotective Compounds from Carob Pods (Ceratonia siliqua L.) Using Ultrasonic Assisted Extraction Method

The current study first describes the extraction of phytoantioxidant polyphenols from Carob byproducts (pods) using maceration and heating-assisted extraction as traditional methods and ultrasonic-assisted extraction (UAE) as an innovative method to determine the most efficient extraction process in terms of four targeted responses: total phenolic content (TPC), antioxidant activities (TAC and DPPH), and photoprotective properties as measured by the sun protection factor (SPF). Second, we used response surface methodology (RSM) with a central composite rotatable design (CCDR) approach to investigate the influence of process variables (extraction time, extraction temperature, and solvent concentration) on UAE, which was found to be the most effective extraction technique in our study. Carob byproduct extracts had a TPC ranging from 6.21 to 21.92 mg GAE/g dw, a TAC ranging from 22.00 to 49.30 mg AAE/g dw, DPPH scavenging activity ranging from 56.35 to 90.50%, and SPF values ranging from 8.62 to 22.37. The optimal UAE conditions for maximum TPC, TAC, DPPH, and SPF responses were determined to be 38.90% ethanol, 53.90 °C, and 50.92 min. Using Carob as a source for sustainable and bioactive products in conjunction with optimized UAE is a promising contribution to the cosmetic industry that will help to strengthen the concept of environmentally-friendly “green chemistry”. Given that Carob pulp or seeds are considered food byproducts, the research presented here encourages the use of these agri-food waste materials in cosmetics.     

Spent Grain from Malt Whisky: Assessment of the Phenolic Compounds

In order to extract antioxidant phenolic compounds from spent grain (SG) two extraction methods were studied: the ultrasound-assisted method (US) and the Ultra-Turrax method (high stirring rate) (UT). Liquid to solid ratios, solvent concentration, time, and temperature/stirring rate were optimized. Spent grain extracts were analyzed for their total phenol content (TPC) (0.62 to 1.76 mg GAE/g SG DW for Ultra-Turrax pretreatment, and 0.57 to 2.11 mg GAE/g SG DW for ultrasound-assisted pretreatment), total flavonoid content (TFC) (0.6 to 1.67 mg QE/g SG DW for UT, and 0.5 to 1.63 mg QE/g SG DW for US), and antioxidant activity was measured using 2,2-diphenyl-2-picrylhydrazyl (DPPH) free radical (25.88% to 79.58% for UT, and 27.49% to 78.30% for UT). TPC was greater at a high stirring rate and high exposure time up to a certain extent for the Ultra-Turrax method, and at a high temperature for the ultrasound-assisted method. P-coumaric acid (20.4 ± 1.72 mg/100 SG DW for UT, and 14.0 ± 1.14 mg/100 SG DW for US) accounted for the majority of the phenolic found compounds, followed by rosmarinic (6.5 ± 0.96 mg/100 SG DW for UT, and 4.0 ± 0.76 mg/100 SG DW for US), chlorogenic (5.4 ± 1.1 mg/100 SG DW for UT, and non-detectable for US), and vanillic acids (3.1 ± 0.8 mg/100 SG DW for UT, and 10.0 ± 1.03 mg/100 SG DW for US) were found in lower quantities. Protocatechuic (0.7 ± 0.05 mg/100 SG DW for UT, and non-detectable for US), 4-hydroxy benzoic (1.1 ± 0.06 mg/100 SG DW for UT, and non-detectable for US), and caffeic acids (0.7 ± 0.03 mg/100 SG DW for UT, and non-detectable for US) were present in very small amounts. Ultrasound-assisted and Ultra-Turrax pretreatments were demonstrated to be efficient methods to recover these value-added compounds.     

Phytochemical Screening by LC-ESI-MS/MS and Effect of the Ethyl Acetate Fraction from Leaves and Stems of Jatropha macrantha Müll Arg. on Ketamine-Induced Erectile Dysfunction in Rats

Jatropha macrantha Müll Arg. L is also known as “huanarpo macho” and used in the Peruvian traditional medicine as an aphrodisiac and erectile dysfunction (ED). The aim of this study was to determine the phytochemical constituents in leaves and stems ethyl acetate fraction (LEAF and SEAF) of J. macrantha and to compare the antioxidant activity and the ameliorative effect on ketamine-induced erectile dysfunction in rats. The phytochemical constituents were determined by LC-ESI-MS/MS, the total phenolic compounds and total flavonoids (TPC and TF) by Folin-Ciocalteu and aluminum chloride, respectively. The antioxidant activity was determined by DPPH, ABTS, and FRAP assays. Experimental groups were divided as follows: I: negative control; II: positive control (ketamine at 50 mg/ kg/d); III: sildenafil 5 mg/kg; IV, V, VI: LEAF at 25, 50 and 100 mg/kg, respectively, and VII, VIII, IX: SEAF at 25, 50, and 100 mg/kg, respectively. The phytochemical analysis revealed the presence mainly of coumarins, flavonoids, phenolic acids, and terpenes. TPC of LEAF and SEAF were 359 ± 5.21 mg GAE/g and 306 ± 1.93 mg GAE/g, respectively; TF in LEAF and SEAF were 23.7 ± 0.80 mg EQ/g, and 101 ± 1.42 mg EQ/g, respectively. The DPPH, ABTS, FRAP in SEAF were 647 ± 3.27; 668 ± 2.30; and 575 ± 2.86 μmol TE/g, respectively, whilst LEAF showed 796 ± 3.15; 679 ± 0.85; and 806 ± 3.42 μmol TE/g, respectively. Regarding sexual behavior, LEAF showed a better effect in mount frequency, intromission frequency, ejaculation frequency, mount latency, intromission latency, ejaculatory latency, and post ejaculatory latency than SEAF. As conclusion, LEAF of J. macrantha at 50 mg/kg showed a better effect on sexual behavior in male rats with erectile dysfunction than SEAF but not higher than sildenafil.     

Optimizing Procedures of Ultrasound-Assisted Extraction of Waste Orange Peels by Response Surface Methodology

The simultaneous effects of three continuous factors: solvent concentration (50–100%), treated times (25–85 min), treated temperatures (25–55 °C), and two categorical factors: type of solvents (methanol or ethanol) and ultrasonic frequency (28 kHz or 40 kHz) on ultrasonic-assisted extraction yield from waste orange peels were evaluated and optimized by response surface methodology. Fourier Transform Infrared (FTIR) spectroscopy with a wavelength of 500 cm⁻¹ to 4000 cm⁻¹ was employed to rapidly identify the orange extracts. The significant polynomial regression models on crude extraction, sediments after evaporation, and precipitation yield were established (p < 0.05). Results revealed that solvent concentration affected crude extraction and precipitation yield linearly (p < 0.01). The optimal and practical ultrasound-assisted extraction conditions for increasing the precipitation yield were using 61.42% methanol with 85 min at 55 °C under 40 kHz ultrasonic frequency. The spectra of extracts showed a similar fingerprint of hesperidin.     

Thermal stability of total phenolic compounds and antioxidant activities of jaboticaba peel: Effect of solvents and extraction methods

The objective was to evaluate the effect of temperature on the degradation of total phenolic compounds (TPC) and antioxidant activities (AA), in addition to the effects of solvents (water, ethanol and methanol) and methods of maceration and ultrasound in the extraction of polyphenols from the jaboticaba peel powder (JPP). The thermal stability of the TPC and AA (DPPH, FRAP and ABTS) from JPP at different temperatures (90, 110 and 130 °C) was monitored over time (0–360 min). The effect of solvents (water, ethanol and methanol) and methods of maceration and ultrasound on the extraction of polyphenols from JPP was also evaluated. The best conditions for extracting polyphenols were quantified by HPLC. After extraction, the morphology of the powders was evaluated by scanning electron microscopy (SEM). The study of thermal stability showed that the ABTS radical presented a lower stability with time when compared to the other radicals. In addition, it was observed that the thermal degradation of TPC at the studied temperatures and that there is a positive correlation between TPC and AA. In the ultrasonic extraction using ethanol and methanol in the mass ratio of JPP/volume of solvent 1:20, the maximum TPC amounts were obtained. In the analysis by HPLC, a content of gallic acid (16.28 mg L⁻¹) and hesperidin (9.26 mg L⁻¹) were found for ethanol and methanol, respectively. The SEM images indicated that the changes in the structure favored the formation of pores contributing to the solubilization of TPC and consequently AA.     

Optimization of Extraction Conditions of Carotenoids from Dunaliella parva by Response Surface Methodology

Extraction conditions can exert a remarkable influence on extraction efficiency. The aim of this study was to improve the extraction efficiency of carotenoids from Dunaliella parva (D. parva). Dimethyl sulfoxide (DMSO) and 95% ethanol were used as the extraction solvents. The extraction time, extraction temperature and the proportions of mixed solvent were taken as influencing factors, and the experimental scheme was determined by Central Composite Design (CCD) of Design Expert 10.0.4.0 to optimize the extraction process of carotenoids from D. parva. The absorbance values of the extract at 665 nm, 649 nm and 480 nm were determined by a microplate spectrophotometer, and the extraction efficiency of carotenoids was calculated. Analyses of the model fitting degree, variance and interaction term 3D surface were performed by response surface analysis. The optimal extraction conditions were as follows: extraction time of 20 min, extraction temperature of 40 °C, and a mixed solvent ratio (DMSO: 95% ethanol) of 3.64:1. Under the optimal conditions, the actual extraction efficiency of carotenoids was 0.0464%, which was increased by 18.19% (the initial extraction efficiency of 0.03926%) with a lower extraction temperature (i.e., lower energy consumption) compared to the standard protocol.     

Assessment of Conventional Solvent Extraction vs. Supercritical Fluid Extraction of Khella (Ammi visnaga L.) Furanochromones and Their Cytotoxicity

Background: Khella (Ammi visnaga Lam.) fruits (Apiaceae) are rich in furanochromones, mainly khellin and visnagin, and are thus incorporated in several pharmaceutical products used mainly for treatment of renal stones. Methods: The objective of this study was to compare the yield of khellin and visnagin obtained using different conventional solvents and supercritical fluid extraction (SCFE) with carbon dioxide (containing 5% methanol as co-solvent). Water, acetone and ethanol (30% and 95%) were selected as conventional solvents. Results: Highest extract yield was obtained from 30% ethanol (15.44%), while SCFE gave the lowest yield (4.50%). However, the percentage of furanochromones were highest in SCFE (30.1%), and lowest in boiling water extract (5.95%). HPLC analysis of conventional solvent extracts showed other coumarins that did not appear in supercritical fluid extraction chromatogram due to non-selectivity of solvent extraction. Ammi visnaga extracts as well as standard khellin and visnagin were tested for their cytotoxic activity using sulforhodamine B assay on breast cancer (MCF-7) and hepatocellular carcinoma (Hep G2) cell lines. Results revealed a strong cytotoxic activity (IC₅₀ < 20 µg/mL) for the SCFE and standard compounds (khellin and visnagin) (IC₅₀ ranging between 12.54 ± 0.57 and 17.53 ± 1.03 µg/mL). However, ethanol and acetone extracts had moderate cytotoxic activity (IC₅₀ 20–90 µg/mL) and aqueous extract had a weak activity (IC₅₀ > 90 µg/mL). Conclusions: Thus, supercritical fluid extraction is an efficient, relatively safe, and cheap technique that yielded a more selective purified extract with better cytotoxic activity.     

Umbu Fruit Peel as Source of Antioxidant,Antimicrobial and α-Amylase Inhibitor Compounds

Herein, the extraction of bioactive compounds from umbu fruit peel was optimized using thermal-assisted solid–liquid extraction. In parallel, antioxidant, antimicrobial, and inhibitory effects against α-amylase of optimized extract were also evaluated. The combination of operational conditions including the temperature (32–74 °C), ethanol concentration (13–97%), and solid/liquid ratio (1:10–1:60; w/v) was employed using a rotational central composite design for optimization. The extracts were evaluated for total phenolic compounds (TPC), total flavonoid compounds (TFC) and antioxidant capacity by ABTS^•+, DPPH^• and FRAP assays. The bioactive profile of the optimized extract was obtained by ultra-performance liquid chromatography coupled to quadrupole/time-of-flight mass spectrometry in electrospray ionization in both negative and positive modes. The statistically evaluated results showed that the optimal operational conditions for the recovery of bioactive compounds from umbu fruit peel included 74 °C, 37% ethanol, and a solid–liquid ratio of 1:38. Under these conditions, the obtained values were 1985 mg GAE/100 g, 1364 mg RE/100 g, 122 µmol TE/g, 174 µmol/TE g and 468 µmol Fe²⁺/g for TPC, TFC, ABTS^•+, DPPH^•, and FRAP assays, respectively. In addition, the optimized extract was effective against Gram-positive and Gram-negative bacteria (MBC ranged from 0.060 to 0.24 mg GAE/mL), as well as it was effective to inhibit α-amylase (IC₅₀ value of 0.076 mg GAE/mL). The optimized extract showed to be mainly constituted by phenolic acids and flavonoids.     

Extraction of Anthocyanins from Borage (Echium amoenum) Flowers Using Choline Chloride and a Glycerol-Based,Deep Eutectic Solvent: Optimization,Antioxidant Activity,and In Vitro Bioavailability

Borage flower (Echium amoenum), an annual herb native to the Mediterranean region, is an excellent source of anthocyanins and is widely used in various forms due to its biological activities. In the present study, a choline chloride and glycerol (CHGLY)-based natural deep eutectic solvent (NADES) was applied in order to extract the anthocyanins from borage flowers. The traditional solvents, including water, methanol, and ethanol, were used to evaluate the efficiency of CHGLY. The results showed that CHGLY was highly efficient compared to the traditional solvents, providing the highest amounts of the total anthocyanin content (TAC), total phenolic content (TPC), total flavonoid content (TFC), individual anthocyanins, and antioxidant activity (DPPH radical scavenging (DPPH) and ferric-reducing antioxidant power (FRAP) assays). The most dominant anthocyanin found in studied borage was cyanidin-3-glucoside, followed by cyanin chloride, cyanidin-3-rutinoside, and pelargonidin-3-glucoside. The bioavailability % was 71.86 ± 0.47%, 77.29 ± 0.57%, 80.22 ± 0.65%, and 90.95 ± 1.01% for cyanidin-3-glucoside, cyanidin-3-rutinoside, by pelargonidin-3-glucoside and cyanin chloride, respectively. However, cyanidin-3-glucoside was the anthocyanin compound showing the highest stability (99.11 ± 1.66%) in the gastrointestinal environment. These results suggested that choline chloride and glycerol-based NADES is not only an efficient, eco-friendly solvent for the extraction of anthocyanins but can also be used to increase the bioavailability of anthocyanins.     

Novel Processes for the Extraction of Phenolic Compounds from Olive Pomace and Their Protection by Encapsulation

Olive pomace, the solid by-product derived from olive oil production consists of a high concentration of bioactive compounds with antioxidant activity, such as phenolic compounds, and their recovery by applying innovative techniques is a great opportunity and challenge for the olive oil industry. This study aimed to point out a new approach for the integrated valorization of olive pomace by extracting the phenolic compounds and protecting them by encapsulation or incorporation in nanoemulsions. Innovative assisted extraction methods were evaluated such as microwave (MAE), homogenization (HAE), ultrasound (UAE), and high hydrostatic pressure (HHPAE) using various solvent systems including ethanol, methanol, and natural deep eutectic solvents (NADESs). The best extraction efficiency of phenolic compounds was achieved by using NADES as extraction solvent and in particular the mixture choline chloride-caffeic acid (CCA) and choline chloride-lactic acid (CLA); by HAE at 60 °C/12,000 rpm and UAE at 60 °C, the total phenolic content (TPC) of extracts was 34.08 mg gallic acid (GA)/g dw and 20.14 mg GA/g dw for CCA, and by MAE at 60 °C and HHPAE at 600 MPa/10 min, the TPC was 29.57 mg GA/g dw and 25.96 mg GA/g dw for CLA. HAE proved to be the best method for the extraction of phenolic compounds from olive pomace. Microencapsulation and nanoemulsion formulations were also reviewed for the protection of the phenolic compounds extracted from olive pomace. Both encapsulation techniques exhibited satisfactory results in terms of encapsulation stability. Thus, they can be proposed as an excellent technique to incorporate phenolic compounds into food products in order to enhance both their antioxidative stability and nutritional value.     

Cold Ethanol Extraction of Cannabinoids and Terpenes from Cannabis Using Response Surface Methodology: Optimization and Comparative Study

Efficient cannabis biomass extraction can increase yield while reducing costs and minimizing waste. Cold ethanol extraction was evaluated to maximize yield and concentrations of cannabinoids and terpenes at different temperatures. Central composite rotatable design was used to optimize two independent factors: sample-to-solvent ratio (1:2.9 to 1:17.1) and extraction time (5.7 min–34.1 min). With response surface methodology, predicted optimal conditions at different extraction temperatures were a cannabis-to-ethanol ratio of 1:15 and a 10 min extraction time. With these conditions, yields (g 100 g dry matter⁻¹) were 18.2, 19.7, and 18.5 for −20 °C, −40 °C and room temperature, respectively. Compared to the reference ground sample, tetrahydrocannabinolic acid changed from 17.9 (g 100 g dry matter⁻¹) to 15, 17.5, and 18.3 with an extraction efficiency of 83.6%, 97.7%, 102.1% for −20 °C, −40 °C, and room temperature, respectively. Terpene content decreased by 54.1% and 32.2% for extraction at −20 °C and room temperature, respectively, compared to extraction at −40 °C. Principal component analysis showed that principal component 1 and principal component 2 account for 88% and 7.31% of total variance, respectively, although no significant differences in cold ethanol extraction at different temperatures were observed.