Search Results (58)

This study investigates the sequential extraction of lipids and saponins from C. frondosa viscera. Lipids were extracted using supercritical carbon dioxide (scCO₂) in the presence of ethanol (EtOH) as a co-solvent. Subsequently, the lipid-extracted viscera underwent three saponin extraction approaches, scCO₂-scCO₂, scCO₂-EtOH, and scCO₂-hot water, resulting in saponin-rich extracts. Process parameter investigation for saponin extraction from scCO₂-defatted viscera revealed minimal effects of temperature, pressure, extraction time, static extraction, and EtOH concentration on saponin yields, allowing for milder operational conditions (35 °C, 20 MPa, 30 min dynamic extraction, 75% EtOH at 0.5 mL/min) to achieve energy-efficient recovery. Continuous EtOH feeding predominates the scCO₂ extraction of saponins. The sequential scCO₂ extraction of lipid and saponins yielded saponins at 9.13 mg OAE/g, while scCO₂ extraction of lipid followed by a 24 h 70% EtOH extraction of saponins achieved 16.26 mg OAE/g, closely matching the optimized ultrasonic-assisted extraction of saponins (17.31 mg OAE/g) from hexane-defatted samples. Antioxidant activities of saponin-rich extracts obtained in the sequential scCO₂-EtOH extraction (17.12 ± 4.20% DPPH scavenging) and the sequential scCO₂-scCO₂ extraction (16.14 ± 1.98%) were comparable to BHT (20.39 ± 0.68%), surpassing that of hexane-defatted ultrasonic extracts (8.11 ± 1.16%). The optimized scCO₂-EtOH method offers a sustainable alternative, eliminating toxic solvents while maintaining high saponin yields and bioactivity. Full article

Olive leaves, the main byproducts of olive cultivation, are characterized by a plethora of bioactive metabolites with significant nutritional value. Their main pentacyclic triterpenes, Oleanolic Acid (OA) and Maslinic Acid (MA), are two high added-value compounds with remarkable activities. This study aimed to develop an efficient methodology for extracting and purifying OA and MA, utilizing Supercritical Fluid Extraction (SFE) and Centrifugal Partition Chromatography (CPC)—two modern, scalable, and green techniques. A total of 21 g of olive leaves were subjected to SFE using supercritical CO₂ and ethanol as co-solvent. The extraction employed a step gradient mode, starting with 100% CO₂ and incrementally increasing ethanol (0–10% w/w) every 20 min. Fractions rich in OA and MA (500 mg) were further purified via CPC, utilizing pH zone refining to exploit the protonation and deprotonation properties of acidic triterpenes. The biphasic solvent system consisted of n-hexane, ethyl acetate, ethanol, and water (8:2:5:5 v/v/v/v), with trifluoroacetic acid added to the stationary phase and triethylamine added to the mobile phase. This two-step process yielded 89.5 mg of OA and 28.5 mg of MA with over 95% purity, as confirmed by HPLC-ELSD and ¹H-NMR. Moreover, purified compounds and SFE fractions exhibited promising elastase and collagenase inhibition, highlighting them as dermocosmetic agents. Full article

After cannabidiol was extracted from the hemp biomass using supercritical CO₂ extraction, the residual could be utilized as a source of other valuable ingredients. The stability of the extracted CBD in pre- and post- encapsulation states were evaluated. Dynamic macerations with ethanol and hexane were compared for CBD extraction. The ethanol extract yielded 0.11% ± 0.10 CBD and 1.83% ± 0.00 cannabidiolic acid (CBDA), while the hexane extraction yielded 0.08% ± 0.04 CBD, 1.06% ± 0.04 CBDA, and 0.30% ± 0.04 delta-9-tetrahydrocannabinol (Δ9-THC). Ethanol extraction was selected due to the low THC detection in the extract. The CBD extract was encapsulated using water soluble yellow mustard mucilage (WSM), maltodextrin (MD), gum Arabic (GA), and protein extracted from the hemp biomass waste (HBP) via freeze drying. The WSM-MD-GA 1:5 particle formulation exhibited superior thermal stability over 72 h, whereas the WSM-HBP-GA 1:5 formulation offered the most protection against UVa-induced degradation within the same duration. Incorporating hemp biomass protein as an encapsulation material enhanced protection against light exposure through UV absorption, although it did not grant thermal protection. These findings indicated that encapsulation significantly protects against CBD degradation when subjected to thermal and light conditions compared to non-encapsulated CBD. Full article

Rice bran (RB) is a rice processing by-product recognized to be a source of bioactive compounds, including γ-oryzanol and fatty acids, which have interesting bioactivities such as antioxidant and anti-inflammatory effects. This study aims to optimize the supercritical fluid extraction process for recovering these high-value compounds from rice bran with improved bioactivity. A Central Composite Face-Centered Design was employed to optimize the extraction process by varying the temperature (40–80 °C) and pressure (200–500 bar). The optimal extraction conditions were identified at 500 bar and 62 °C that led to the extraction of 17.3% mass yield with 784.5 mg of fatty acids and 36.6 mg of γ-oryzanol per gram of extract, striking a balance between extraction yield and bioactive concentrations. When compared with conventional extractions with n-hexane, supercritical fluid extraction showed similar global yield (18.0 vs. 17.3%) and FA concentration (130.14 vs. 135.70 mg/g of RB) but higher selectivity and extraction yield for γ-oryzanol (18.0 vs. 36.4 mg/g extract; 3.3 vs. 6.3 mg/g of RB). Cellular antioxidant activity assays showed that both extracts reduced the quantity of reactive oxygen species (ROS) up to 50% in Caco-2 cells submitted to oxidative stress. Importantly, supercritical fluid extract was more effective in inhibiting colorectal cancer cell growth (EC50 = 0.9 mg/mL vs. 1.15 mg/mL) than the hexane extract, and this effect was more pronounced than that obtained for pure γ-oryzanol in the same concentration range. These findings highlight the potential of supercritical fluid technology to develop rice bran extracts with antioxidant and antiproliferative properties, underlining the promising applications of this technology in the field of natural product extraction. Full article

Pitaya (Stenocereus spp.) is recognized for its nutritional properties, with its seeds and peel accounting for 22–29% of the fruit’s mass, often treated as agro-industrial waste. This study evaluates the potential of green solvents for oil extraction from pitaya seeds, aiming to enhance the valorization of these by-products. The efficiency of ethanol and supercritical CO₂ (SC-CO₂) was compared to hexane, a commonly used solvent. Soxhlet extractions were performed using ethanol and hexane, while SC-CO₂ extractions were conducted under two conditions: 180 bar at 50 °C and 250 bar at 35 °C. Oil yields ranged from 4.9% to 24.7%, with hexane achieving the highest yield. However, SC-CO₂ extraction demonstrated its potential as a sustainable alternative. Future studies will focus on characterizing the fatty acid profile of the extracted oil to further assess its nutritional and industrial applications. Full article

In the present study, different methodologies with potential scalability and environmental friendliness, such as winterization, supercritical fluid extraction, and multistage distillation, were evaluated for lauric acid concentration. In all cases, to facilitate fractionation, the transformation of triacylglycerols into free fatty acids or fatty acid ethyl esters was required as a previous step. For the winterization experimental assays, the amount and type of solvent was studied, resulting in a product containing ~65% lauric acid with a recovery of ~81% using a 1:10 oil-to-solvent ratio with hexane. On the other hand, the experimental extraction with supercritical carbon dioxide in a counter current packed column at 55 °C, 115 bar, and 70 g CO₂/min, resulted in a product composed of ~80% lauric acid as ethyl ester with a recovery of ~85%. Finally, flash and multistage distillation were analysed using process simulation (Aspen Plus V14), demonstrating that this methodology can achieve 80% recovery with high purity (lauric acid: 96.7%; ethyl laurate: 97.4%), but a high vacuum is required to prevent thermal degradation of the product (lauric acid: 0.2 mbar; ethyl laurate: 1.1 mbar). Overall, the employed methodologies proved highly efficient in concentrating lauric acid, yielding a product of commercial interest and high added value. Full article

Sustainable agro-waste revaluation is critical to enhance the profitability and environmental footprint of the olive oil industry. Herein, the valorization of olive leaf pruning waste from five cultivars (‘Caiazzana’, ‘Carolea’, ‘Itrana’, ‘Leccino’, and ‘Frantoio’) employed green extraction methods to recover compounds with potential health benefits. Sequential ultrasound-assisted maceration (UAM) in n-hexane and ethanol was compared with a compressed fluid extraction strategy consisting of supercritical fluid extraction (SFE) and pressurized liquid extraction (PLE) for their efficiency in recovering distinct classes of bioactives. Chemical profiling by UHPLC-HR-MS/MS (ultra-high-performance liquid chromatography high-resolution tandem mass spectrometry) and GC-MS (gas chromatography mass spectrometry) showed that UAM-EtOH effectively extracted polyphenols (especially luteolin derivatives) and triterpenes (notably maslinic acid), while PLE yielded the highest amount of secoiridoids (e.g., secologanoside). PLE extracts showed better antiradical activities, putatively due to a higher content of flavonoids, secoiridoids, and HCA derivatives than UAM-EtOH ones, as these latter also contained 20–40% (cultivar-dependent) of triterpenes. SFE extracts with a higher concentration of fatty acids and triterpenes showed moderate antioxidant activities but very high AChE inhibition. This study highlights the importance of selecting appropriate extraction methodologies based on the target bioactive compounds and underscores the potential of olive leaf extracts for sustainable bio-products. Full article

Supercritical fluid extraction using carbon dioxide (SFE-CO₂) brings a convincing advance in the production of plant oils used in cosmetics, in fortified foods and dietary supplements, and in pharmaceuticals and medicine. The SFE-CO₂-extracted, hexane-extracted, and cold-pressed plant oils of pumpkin (Cucurbita pepo L.), flax (Linum usitatissimum L.), linden (Tilia sp.), poppy (Papaver somniferum L.), apricot (Prunus armeniaca L.), and marigold (Calendula officinalis L.) seeds were investigated in terms of oil yield, fatty acid composition, unsaponifiable matter yield and composition, and the antioxidant activity of unsaponifiable matter. SFE-CO₂ proved to be the preferred extraction method for four out of six plant materials, especially for seeds with lower oil content. However, for seeds with higher oil content, such as apricots, cold pressing is a viable alternative. A comparison of fatty acid composition did not reveal significant differences between extraction techniques. SFE-CO₂ extraction improved the total phytosterol content of oils, especially pumpkin seed oil. A high variability in the antioxidant potential of the unsaponifiable matter studied was determined, with pumpkin seed oil showing the highest antioxidant activity. A correlation analysis was performed between unsaponifiable composition and antioxidant activity, and showed statistically significant correlations with squalene, cycloartenol, and an unidentified compound. This is the first comparison of the phytosterol compositions of linseed, apricot, linden, and marigold. Through continued optimization, SFE-CO₂ has the potential to revolutionize the production of plant oils and provide a sustainable and efficient alternative. Full article

The main objective of this work was to extract bioactive compounds from different cultivars of blackberry pomace using conventional Soxhlet and supercritical CO₂ (SC-CO₂) extraction methods. For Soxhlet extraction, two different solvents, ethanol and n-hexane, were used. Qualitative and quantitative composition of fatty acids was determined by GC, carotenoids and chlorophylls by HPLC, and volatile organic compounds were identified with an e-nose based on GC. The yield of the extract was influenced by the extraction, while the qualitative content of the extracts was also dependent on the cultivar. While there were no differences in the types of fatty acids extracted, their content varied significantly depending on the cultivar, extraction method, and their interaction. The results showed that linoleic acid (C18:2), oleic acid (C18:1), and α-linolenic acid (C18:3) were the most prevalent in all cultivars of blackberry pomace extracts. The linoleic acid content varied from 33.33 to 64.77% depending on the variety, and the ratio of omega-6 to omega-3 varied from 3.17% to 5.71%. Significantly higher quantities of carotenoids and chlorophylls were obtained in Soxhlet extraction with n-hexane in all extracts. The major carotenoid in the ‘Orkan’ and ‘Polar’ extracts was lutein, while in the ‘Brzezina’ extract, it was β-carotene. The extraction method has a significant impact on the flavor profile of the extracts. Full article

The valorization of industrial waste in the production of new products is a growing trend, with food waste showing significant promise as a raw material for various industries. Thus, this research aimed to investigate the production of Geotrichum candidum lipase using industrial waste, such as mozzarella cheese whey (MCW) and corn steep liquor (CSL), and to analyze how effectively it catalyzes the esterification of oleic acid with methanol. Lipase production was carried out in medium containing MCW and CSL, with fermentation conditions optimized using a fractional factorial experimental design and central composite experimental design. The highest activities (16.71 U/mL in 24 h and 17.80 U/mL in 48 h) were found in conditions of 13.6% (%w/v) CSL and 37.1% (%w/v) MCW, with corn oil fixed at 1% (%w/v) and pH fixed at 6,00. Esterification conditions were evaluated at atmospheric pressure, both in a solvent-free environment and using hexane, as well as under high pressures with supercritical carbon dioxide (SC-CO₂). The produced lipase demonstrated high catalytic activity for the esterification reaction of oleic acid with methanol under SC-CO₂ with an increase of 39.41% in the yield. The yields found confirm the feasibility of producing lipase from industrial waste, thus presenting it as a sustainable and efficient alternative for industrial processes, and show that there is no need to use toxic organic solvents in esterification reactions. Full article

Liquid fuel production from biomass-derived molecules has received great attention due to the diminished fossil fuel reserves, growing energy demand, and the necessity of CO₂ emission reduction. The deoxygenation of oils and fatty acids is a promising process to obtain “green” diesel. Herein, we report the results of the study of the deoxygenation of stearic acid to alkanes as a model reaction. Series of Ni-supported on schungite were obtained by precipitation in subcritical water (hydrothermal deposition) and for comparison via wetness impregnation followed, in both cases, by calcination at 500 °C and a reduction in H₂ at 300 °C. The catalyst obtained via hydrothermal synthesis showed a three-fold higher specific surface area with a four-fold higher active phase dispersion compared to the catalysts synthesized via conventional impregnation. The catalysts were tested in stearic acid deoxygenation in supercritical n-hexane as the solvent. Under optimized process conditions (temperature of 280 °C, hydrogen partial pressure of 1.5 MPa, and 13.2 mol of stearic acid per mol of Ni), a close to 100% yield of C₁₀–C₁₈ alkanes, containing over 70 wt.% of targeted n-heptadecane, was obtained after 60 min of reaction. Full article

This study aimed to investigate the efficacy of supercritical CO₂ (SC-CO₂) extraction in enhancing the extraction rate, purity, and antioxidant activity of Indocalamus latifolius (Keng) McClure (Poaceae) leaf terpenoids (ILLTs). Crude extracts obtained from leaves were subjected to qualitative and quantitative analyses, revealing neophytadiene, phytol, β-sitosterol, β-amyrone, squalene, and friedelin as the primary terpenoid constituents, identified through gas chromatography–mass spectrometry (GC-MS). Compared with steam distillation extraction (SD), simultaneous distillation extraction (SDE), ultra-high pressure-assisted n-hexane extraction (UHPE-Hex), ultra-high pressure-assisted ethanol extraction (UHPE-EtOH), ultrasound-assisted n-hexane extraction (UE-Hex), and ultrasound-assisted ethanol extraction (UE-EtOH), SC-CO₂ exhibited a superior ILLT extraction rate, purity, and antioxidant activity. Scanning electron microscopy (SEM) observations of the residues further revealed more severe damage to both the residues and their cell walls after SC-CO₂ extraction. Under optimal parameters (4.5 h, 26 MPa, 39 °C, and 20% ethyl alcohol), the ILLT extraction rate with SC-CO₂ reached 1.44 ± 0.12 mg/g, which was significantly higher than the rates obtained by the other six methods. The subsequent separation and purification using WelFlash C18-l, BUCHI-C18, and Sephadex LH-20 led to an increase in the purity of the six terpenoid components from 12.91% to 93.34%. Furthermore, the ILLTs demonstrated cytotoxicity against HepG2 cells with an IC₅₀ value of 148.93 ± 9.93 μg/mL. Additionally, with increasing concentrations, the ILLTs exhibited an enhanced cellular antioxidant status, as evidenced by reductions in both reactive oxygen species (ROS) and malondialdehyde (MDA) levels. Full article

Raspberry seeds are a by-product of berries, both from their primary processing, such as in juice production, and secondary processing, such as in oil extraction. These seeds contain plenty of valuable components such as crude fiber, proteins, fats, and vitamins. Quality characterization is the initial step toward using these seeds as a sustainable and functional food. The aim of studying raspberry seeds’ quality profile, both before oil extraction and after different processing methods (supercritical CO₂, subcritical CO₂, cold pressing, and hexane solvent), is to point out the benefits of this by-product and to raise consumer awareness about their health and well-being benefits. This study provides evidence that raspberry seeds have good physical parameters for use in other products as a functional food enrichment ingredient, such as in baked goods, offering considerable health benefits due to their high nutrient content. The weights, peroxide values, moisture content, nutritional energy values, and colors were determined before oil extraction to give initial seed values. The nutrient content and amounts of macroelements, P, K, Ca, and Mg, as well as microelements, B, Zn, Cu, Fe, and Mn, were determined in the tested variety ‘Polka’, both before and after oil extractions and using different methods. The raspberry seeds’ moisture was 9.2%, their peroxide content was 5.64 mEq/kg, their nutritional value was 475.25 Kcal., and their total weight was 2.17 mg (1000 units). The seeds contain 7.4% protein, 22.1% crude fiber, 11.0% crude fat and oil, and 2.8% sugar. We determined how different oil extraction methods influence the nutrient, micro-, and macro-component values. We concluded that the seeds contained the highest manganese (45.3 mg/kg), iron (29.2 mg/kg), and zinc (17.4 mg/kg) contents and the lowest content of copper (5.1 mg/kg). This research shows that raspberry seeds represent a potential natural food ingredient, and after oil extraction with subcritical or supercritical CO₂ or cold pressing, they can be used as a sustainable and functional food. Full article

Tomato seeds are a rich source of protein that can be utilized for various industrial food purposes. This study delves into the effects of using supercritical CO₂ (scCO₂) on the structure and techno-functional properties of proteins extracted from defatted tomato seeds. The defatted meal was obtained using hexane (TSMH) and scCO₂ (TSMC), and proteins were extracted using water (PEWH and PEWC) and saline solution (PESH and PESC). The results showed that scCO₂ treatment significantly improved the techno-functional properties of protein extracts, such as oil-holding capacity and foaming capacity (especially for PEWC). Moreover, emulsifying capacity and stability were enhanced for PEWC and PESC, ranging between 4.8 and 46.7% and 11.3 and 96.3%, respectively. This was made possible by the changes in helix structure content induced by scCO₂ treatment, which increased for PEWC (5.2%) and decreased for PESC (8.0%). Additionally, 2D electrophoresis revealed that scCO₂ hydrolyzed alkaline proteins in the extracts. These findings demonstrate the potential of scCO₂ treatment in producing modified proteins for food applications. Full article

Driven by growing concerns about food supply and the environment, research on alternative protein sources has become increasingly important. In this context, de-oiled seed cakes, particularly soybean cakes, have emerged as a promising option. However, the conventional methods, such as organic solvent extraction, from which these cakes are obtained present several limitations. This study aims to evaluate the efficiency of supercritical fluid extraction (SFE) as an alternative method for de-oiling soybean seeds and obtaining related protein isolates. By using SFE for de-oiling, it was possible to achieve 19% more protein isolates from soybean cakes than the conventional de-oiling method using hexane. Moreover, protein isolates from the SFE de-oiled cake reported significantly improved (p < 0.05) emulsifying abilities and water absorption capacity. Gel electrophoresis and differential scanning calorimetry indicated the presence of a higher concentration of proteins in their native state in the SFE de-oiled flour. Finally, results from the sulfhydryl group content, surface hydrophobicity, and protein dispersibility index also supported these conclusions. The SFE process produced de-oiled soybean cakes with superior functional characteristics and lower environmental impact. Thus, this study provided important information for the food industry to develop more sustainable and healthier production methods. Full article