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This study focused on the oil extraction from freeze-dried maqui (Aristotelia chilensis) by supercritical fluid extraction with carbon dioxide (SFE-CO2). The basic objective was to optimize the oil yield and the tocopherol concentration. A Box/Behnken experimental design was developed with three processing variables: supercritical pressure (74, 187, and 300 bar), temperature (35, 48, and 60 °C), and extracting time (30, 135, and 240 min). Multiple optimizations, based on the combination of factor levels at 274 bar, 240 min, and 60 °C, led to the highest oil yield and tocopherol values. The validation of the optimized conditions of maqui oil extraction led to an oil yield of 8% and values of 735, 53, and 97 (mg·kg-1 oil) for α-tocopherol, α-tocotrienol, and γ-tocopherol, respectively. A higher concentration of tocopherol compounds was observed when compared to the employment of the conventional extracting method. The optimized SFE-CO2 method led to an oil extract exhibiting higher Hydrophilic-Oxygen Radical Absorbance Capacity (H-ORAC) assay and total phenol content (22 µmol Trolox equivalents·g-1 oil and 28 mg gallic acid equivalents·g-1 oil) than the oil obtained by the conventional procedure. A practical and accurate oil extraction is proposed for obtaining tocopherol-enriched oil including high concentrations of valuable lipophilic antioxidants.

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Anti-Trypanosoma cruzi activity of compounds from fruits of Schinus terebinthifolius Raddi (pink pepper) were evaluated, using sustainable techniques such as steam distillation (SD) and supercritical fluid extraction (SFE). SD was optimised using a design of experiment and SFE was carried out using supercritical CO2 solvent (300 bar and 60 °C). Results of the anti-T. cruzi activity showed that the essential oil presented high activity (IC50 = 4.5 ± 0.3 µg/mL), whereas the supercritical extract had a moderate effect (IC50 = 19.7 ± 2.9 µg/mL). The differences in the anti-T. cruzi activity can be attributed to the extraction of non-volatile compounds in the SFE, such as moronic and (Z)-masticadienoic acids. In contrast, SD extracted only volatile compounds such as monoterpenes and sesquiterpenes. Therefore, these results suggest that the volatile compounds from pink pepper are involved with the anti-T. cruzi activity.

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Pterocaulon polystachyum is a species of pharmacological interest for providing volatile and non-volatile extracts with antifungal and amebicidal properties. The biological activities of non-volatile extracts may be related to the presence of coumarins, a promising group of secondary metabolites. In the present study, leaves and inflorescences previously used for the extraction of essential oils instead of being disposed of were subjected to extraction with supercritical CO2 after pretreatment with microwaves. An experimental design was followed to seek the best extraction condition with the objective function being the maximum total extract. Pressure and temperature were statistically significant factors, and the optimal extraction condition was 240 bar, 60 °C, and pretreatment at 30 °C. The applied mathematical models showed good adherence to the experimental data. The extracts obtained by supercritical CO2 were analyzed and the presence of coumarins was confirmed. The extract investigated for cytotoxicity against bladder tumor cells (T24) exhibited significant reduction in cell viability at concentrations between 6 and 12 µg/mL. The introduction of green technology, supercritical extraction, in the exploration of P. polystachyum as a source of coumarins represents a paradigm shift with regard to previous studies carried out with this species, which used organic solvents. Furthermore, the concept of circular bioeconomy was applied, i.e., the raw material used was the residue of a steam-distillation process. Therefore, the approach used here is in line with the sustainable exploitation of native plants to obtain extracts rich in coumarins with cytotoxic potential against cancer cells.

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Currently, Bixa orellana L. extracts are used as a color source in the food, pharmaceutical, and cosmetic industries because they are important as a potential source of antioxidant activity. The extraction is carried out by conventional methods, using alkaline solutions or organic solvents. These extraction methods do not take advantage of the lipid fraction of annatto (Bixa orellana L.) seeds, and the process is not friendly to the environment. In this work, the objective was to obtain an extract rich in nutraceuticals (bixin and tocols) of high antioxidant power from Peruvian annatto seeds as a potential source for a functional food or additive in the industry using supercritical fluid extraction (SFE). Experiments related to extraction yield, bixin, tocotrienols, tocopherols, and antioxidant activity were carried out. The SFE was performed at 40 °C, 50 °C, and 60 °C, and 100, 150, and 250 bar with 0.256 kg/h carbon dioxide as the supercritical solvent (solvent-to-feed ratio of 10.2). Supercritical extraction at 60 °C and 250 bar presented the best results in terms of global extraction yield of 1.40 ± 0.01 g/100 g d.b., extract concentration of 0.564 ± 0.005 g bixin/g extract, 307.8 mg α-tocotrienol/g extract, 39.2 mg ß-tocotrienol/g extract, 2 mg γ-tocopherol/g extract, and IC50 of 989.96 µg extract/mL. Economical evaluation showed that 60 °C, 250 bar, and 45 min presented the lowest cost of manufacturing (2 × 2000 L, COM of USD 212.39/kg extract). This extract is a potential source for functional food production.

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This review addresses the possibilities of using supercritical carbon dioxide (SC-CO2) in the flavor industry in extraction and fractionation processes and its use as a reaction medium to generate aroma esters. The advantages and disadvantages are presented, comparing SC-CO2 processing with traditional methods. The most distinguishable features of SC-CO2 include mild reaction conditions, time savings, fewer toxicity concerns, higher sustainability, and the possibility of modulating solvent selectivity according to the process conditions (such as pressure and temperature). Thus, this review indicates the potential of using SC-CO2 to obtain a high selectivity of compounds that can be applied in aroma technology and related fields.

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The aim of the present study was to evaluate the use of supercritical CO2 combined with cosolvent for the recovery of bioactive compounds of soybean fermented with Rhizopus oligosporus NRRL 2710. Soxhlet extractions using seven different organic solvents (n-hexane, petroleum ether, ethyl acetate, acetone, ethanol, methanol, and water) were initially performed for comparative purposes. The extracts obtained were characterized by physicochemical, antioxidant, total phenolic, and oxidative proprieties. For the Soxhlet extractions, the highest and lowest yields obtained were 45.24% and 15.56%, using methanol and hexane, respectively. The extraction using supercritical CO2 combined with ethanol as a static modifier (scCO2 + EtOH) presented, at a high pressure (25 MPa) and temperature (80 °C), a phenolic compound content of 1391.9 µg GAE g-1 and scavenging of 0.17 g, reaching a 42.87% yield. The extracts obtained by sCO2 + EtOH were characterized by high contents of essential fatty acids (linoleic acid and oleic acid) and bioactive compounds (gallic acid, trans-cinnamic acid, daidzein, and genistein). These extracts also showed a great potential for inhibiting hyaluronidase enzymes (i.e., anti-inflammatory activity). Thermogravimetric analyses of the samples showed similar profiles, with oil degradation values in the range from 145 to 540 °C, indicating progressive oil decomposition with a mass loss ranging from 93 to 98.7%. In summary, this study demonstrated the flexibility of scCO2 + EtOH as a green technology that can be used to obtain high-value-added products from fermented soybean.

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Pink pepper (Schinus terebinthifolius Raddi) has high potential for commercial use because of its biological activities (anti-inflammatory, antitumor, and antioxidant activities, among others). Herein, the antioxidant activity of a topical formulation containing pink pepper extract obtained by supercritical carbon dioxide extraction is reported. The effects of extraction pressure (100-300 bar) and temperature (40-60 °C) on its antioxidant activity were investigated. The extracts obtained at 50-60 °C showed a higher inhibition percentage in the α,α-diphenyl-ß-picrylhydrazyl (DPPH) assay (80.16-91.27 %), regardless of pressure. The extract obtained under optimized conditions (200 bar and 50 °C) was incorporated into an oil-in-water emulsion containing 2 % (m/m) pink pepper extract. The product presented a creamy texture, light rose color, mild spicy odor, and desirable pH for a topical formulation. Furthermore, the product was stable and remained effective when stored and protected from heat and light, showing 35.38 % inhibition of DPPH.

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Microalgae grow in diverse environments and possess a great biotechnological potential as they contain useful bioactive compounds. These bioactive compounds can be obtained by selective and energy-efficient extraction methods. Various industries are using the supercritical fluid extraction (SFE) method to extract these valuable bioactive compounds. Hence, for the first time, we evaluated the effects of SFE on the recovery of bioactive and antioxidant compounds using Coccomyxa onubensis, a eukaryotic acidophilic microalga of potential relevance which can be used in the field of nutraceutical and functional foods. It was isolated from the Tinto River (Pyritic Belt, Huelva, Spain), a mining region in Spain. Variables such as extraction yield, lutein purity (LP) and recovery (LR), total phenols, and antioxidant capacity (Trolox equivalents antioxidant capacity method) were studied using a Box-Behnken design based on a response surface methodology along with the overall extraction curve fitted to a spline linear model. The effects of temperature (30, 50, and 70 °C), pressure (25, 40, and 55 MPa), and the percentage of co-solvent (0, 25%, and 50% v/v ethanol) on SFE were analyzed, resulting in the co-solvent and temperature as the most significant factors followed by the pressure. Under 70 °C, 40 MPa, and 50% v/v ethanol, C. onubensis reached a maximum of 66.98% of LR. The extracts were richest in total phenols and showed the maximum antioxidant activity (36.08 mg GAEs/g extracts and 2.237 mmol TE/g extracts, respectively) under similar pressure and co-solvent percentage values and different temperatures (30 and 70 °C, respectively). The extracts obtained in this study may have potential applications in the food, nutraceutical, and cosmetic industries. SFE is a highly efficient method to valorize microorganisms living in extreme environments, which are so far unexplored using green extraction methods.

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The study evaluated the techno-economic feasibility of an industrial SFE plant to produce astaxanthin-rich extracts in Chile based on previously published data. A kinetic study comparing two solvent flow rates (3.62 and 7.24 g/min) at a scale production of 2 × 10 L showed the FER period as the more economically feasible with a cost of manufacturing (COM) of US$ 656.31/kg at 7.24 g/min. The study also demonstrated that the extraction times used at a laboratory scale were not industrially feasible due to the flowrate limits of industrial pumps. After adjusting extraction time to real industrial conditions, the results demonstrated that a 5-fold scale increase (2 × 10 L to 2 × 50 L) decreased the COM by 30 % and the process was profitable at all production scales. Finally, the sensitivity study demonstrated that it is possible to reduce the selling price by 25 % at 2 × 50 L scale.

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A widely disseminated native species from Australia, Acacia mearnsii, which is mainly cultivated in Brazil and South Africa, represents a rich source of natural tannins used in the tanning process. Many flowers of the Acacia species are used as sources of compounds of interest for the cosmetic industry, such as phenolic compounds. In this study, supercritical fluid extraction was used to obtain non-volatile compounds from A. mearnsii flowers for the first time. The extract showed antimicrobial activity and the presence of p-anisic acid, a substance with industrial and pharmaceutical applications. The fractionation of the extract was performed using a chromatographic column and the fraction containing p-anisic acid presented better minimum inhibitory concentration (MIC) results than the crude extract. Thus, the extraction process was optimized to maximize the p-anisic acid extraction. The response surface methodology and the Box-Behnken design was used to evaluate the pressure, temperature, the cosolvent, and the influence of the particle size on the extraction process. After the optimization process, the p-anisic acid yield was 2.51% w/w and the extraction curve was plotted as a function of time. The simulation of the extraction process was performed using the three models available in the literature.

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Peppers of the Capsicum genus have a rich nutritional composition and are widely consumed worldwide. Thus, they find numerous applications in the food, pharmaceutical and cosmetic industries. One commercial application is oleoresin production, a nonpolar fraction rich in bioactive compounds, including capsaicinoids and carotenoids. Among the technologies for pepper processing, special attention is given to supercritical fluid technologies, such as supercritical fluid extraction (SFE) with pure solvents and CO2 plus modifiers, and SFE assisted by ultrasound. Supercritical fluid-based processes present advantages over the classical extraction techniques like using less solvents, short extraction times, specificity and scalability. In this review, we present a brief overview of the nutritional aspects of peppers, followed by studies that apply supercritical fluid technologies to produce extracts and concentrate bioactives, besides oleoresin encapsulation. Furthermore, we present related phase equilibrium, cost estimation, and the gaps and needs for the full use of peppers from a sustainable perspective.

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Phaeodactylum tricornutum is the marine diatom best known for high-value compounds that are useful in aquaculture and food area. In this study, fucoxanthin was first extracted from the diatom using supercritical fluid extraction (SFE) and then using the extracted diatom-like substrate to produce bioenergy through anaerobic digestion (AD) processes. Factors such as temperature (30 °C and 50 °C), pressure (20, 30, and 40 MPa), and ethanol (co-solvent concentration from 10% to 50% v/v) were optimized for improving the yield, purity, and recovery of fucoxanthin extracted using SFE. The highest yield (24.41% w/w) was obtained at 30 MPa, 30 °C, and 30% ethanol but the highest fucoxanthin purity and recovery (85.03mg/g extract and 66.60% w/w, respectively) were obtained at 30 MPa, 30 °C, and 40%ethanol. Furthermore, ethanol as a factor had the most significant effect on the overall process of SFE. Subsequently, P.tricornutum biomass and SFE-extracted diatom were used as substrates for biogas production through AD. The effect of fucoxanthin was studied on the yield of AD, which resulted in 77.15 ± 3.85 LSTP CH4/kg volatile solids (VS) and 56.66 ± 1.90 LSTP CH4/kg VS for the whole diatom and the extracted P.tricornutum, respectively. Therefore, P.tricornutuman can be considered a potential source of fucoxanthin and methane and both productions will contribute to the sustainability of the algae-biorefinery processes.

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The goals of this study were to determine the phytochemical profile of Jodina rhombifolia and to evaluate the ability of supercritical fluids (ScFCO2) to selectively extract the metabolites responsible for the bioactivity. This species has simple aromatic compounds and lignan monomers, as well as glycerides containing epoxidized saturated fatty acids. Regarding the extraction by ScFCO2, the extracts showed a higher antimicrobial activity against human pathogenic strains, with respect to the ethanolic extracts obtained from plant residues after extraction by ScFCO2. Furthermore, the bioactive compounds were concentrated in just 1% P/P of the weight of the dry plant material. Extraction by ScFCO2 was carried out under different conditions of pressure and temperature, with the best results being obtained at 30 °C and 30 MPa. The results obtained demonstrate the advantages of ScFCO2 extractions over classical solvent extractions, in terms of improved safety and the ability to selectively extract the compounds of interest.

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Abstract Piper sarmentosum is a herbaceous shrub with numerous pharmacological benefits. However, the presence of two toxic phenylpropanoids (α- and β-asarone) limits the medicinal usage of the plant. In this study, the extraction of three asarone isomers, namely α-, β-, and -asarone was optimised using supercritical carbon dioxide extraction (SC-CO2) combined with Box-Behnken experimental design. Comparison of asarone contents in different conventional solvent extracts of P. sarmentosum leaves prior to and after SC-CO2 extraction was performed. The SC-CO2 method successfully maximised the extraction of α-, β-, and ɣ-asarone at P = 81.16 bar, T = 50.11°C, and t = 80.90 min, yielding 13.91% α-asarone, 3.43% β-asarone, and 14.95% ɣ-asarone. The SC-CO2 residue of the leaves re-extracted with conventional solvents showed a significant decrease of asarone ranging from 45% to 100% (p<0.001) compared to their counterparts without SC-CO2 treatment. α-, β-, and ɣ-asarone were completely removed in the ethanol extract of the residue. These findings suggested that the optimised SC-CO2 extraction parameters may serve as a quick treatment step for the selective removal of asarone from P. sarmentosum to develop safer extracts for the food and nutraceutical industries applications.

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Phenolic compounds from mango (M. indica) seed kernels (MSK) var. Sugar were obtained using supercritical CO2 and EtOH as an extraction solvent. For this purpose, a central composite design was carried out to evaluate the effect of extraction pressure (11-21 MPa), temperature (40-60 °C), and co-solvent contribution (5-15% w/w EtOH) on (i) extraction yield, (ii) oxidative stability (OS) of sunflower edible oil (SEO) with added extract using the Rancimat method, (iii) total phenolics content, (iv) total flavonoids content, and (v) DPPH radical assay. The most influential variable of the supercritical fluid extraction (SFE) process was the concentration of the co-solvent. The best OS of SEO was reached with the extract obtained at 21.0 MPa, 60 °C and 15% EtOH. Under these conditions, the extract increased the OS of SEO by up to 6.1 ± 0.2 h (OS of SEO without antioxidant, Control, was 3.5 h). The composition of the extract influenced the oxidative stability of the sunflower edible oil. By SFE it was possible to obtain extracts from mango seed kernels (MSK) var. Sugar that transfer OS to the SEO. These promissory extracts could be applied to foods and other products.

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The proximal composition, amino acid, carbohydrate, and volatile profiles of caferana (Bunchosia glandulifera) seeds flour were here assessed. Seeds were also subjected to the following extraction processes: one with pressurized ethanol (PLE) and two with ethanol + supercritical CO2 mixture at different temperatures and pressures (SC1 and SC2). Extracts were characterized in terms of caffeine, total phenolic, and δ-lactam. The characterization of caferana seed and its extracts is unprecedented in terms of carbohydrate and volatiles profiles, besides the δ-lactam identification/isolation. SC2 extract exhibited a higher caffeine (9.3 mg/g) and δ-lactam (29.4 mg/g) content, whereas the PLE extract contained a higher total phenolic amount (3.0 mgGAE/g). Caferana is regionally associated to protective effects on mental health. Its byproduct (seed) revealed to be a promising source of bioactive compounds, and a potential raw material of nutritive extracts and flours that can be incorporated into pharmaceutical, nutraceutical, cosmetic, and food products.

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Natural products are a source of a wide range of chemical compounds, from pigments to bioactive compounds, which can be extracted and used in different applications. Due to consumer awareness, the interest in natural compounds significantly increased in the last decades, prompting the search for more efficient and environmentally friendly extraction techniques and methods. Pressurized liquids and fluids (sub and supercritical) are being explored to extract natural compounds within the green process concept. The combination of these techniques with ultrasound has emerged as an alternative to intensify the extraction process efficiently. In this context, this work presents a comprehensive review and current insights into the use of high-pressure systems, specifically supercritical fluid extraction and pressurized liquid extraction assisted by ultrasound, as emerging technologies for extracting bioactive compounds from natural products. The extraction mechanisms, applications, and the influence of operational parameters in the process are addressed, in addition to an analysis of the main challenges to be overcome for widespread application.

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Buritirana (Mauritiella armata Mart.) is a fruit species native to the Amazon and Cerrado region, belonging to the Arecaceae family. It has high nutritional and functional potential, yet little explored. In this study, we evaluated for the first time the overall yield, behavior of total carotenoids in the extraction kinetics, fatty acid profile, bioactive compounds, and the antioxidant capacity of the oil from buritirana fractions obtained by supercritical CO2. The highest extraction yield was found in the pulp and whole without seed at 60 °C (18.06 ± 0.40 and 14.55 ± 1.10 g 100 g-1 of the freeze-dried sample (fdw), respectively), and in the peel at 40 °C (8.31 ± 0.73 g 100 g-1 fdw). During the extraction kinetics, the pulp had the highest yields of oil (41.57%) and total carotenoids (8.34 mg g-1) after 61 min at 40 °C. The antioxidant potential, fatty acid profile, and α-tocopherol content were dependent on both fraction and temperature, with oleic acid being the main fatty acid. The oil from the whole fraction without seed had the largest number (20) of identified phenolic compounds. The extraction at 60 °C reduced the relative intensity of most compounds in the whole without seed and pulp. Moreover, it increased the intensity of the compounds in the peel. These results suggest that buritirana is a good oil source with great bioactive potential to produce new products with functional claims.

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Pollution due to waste generated by the oil industry has led to serious damage to ecosystems and the environment. Therefore, preventive and corrective actions must be taken to mitigate the ecological impact of waste resulting from oil-related activities, to explore and implement environment-friendly approaches, and achieve sustainable development. In this study, an alternative treatment for cuttings generated during the drilling of oil wells was investigated by extracting the hydrocarbons present in such cuttings through the use of carbon dioxide under supercritical conditions. The extractions were performed in a Supercritical Fluid Technologies Inc. Model SFT-150 extractor, under varying pressure (2300-6600 psi) and temperature (52-109 °C), while maintaining constant carbon dioxide flow rate and extraction time, to analyse the effect of these two thermodynamic variables on the extraction efficiency. During supercritical extraction, 21.51 g of total hydrocarbons from drill cuttings (oil/kg) were recovered at 6000 psi and 100 °C. The results indicated that pressure had the strongest effect on the extraction yield, with only a small amount of hydrocarbons recovered at the lowest pressure for all fractions. At <3000 psi pressure, increasing the temperature led to a decrease in the amount of recovered hydrocarbons; at >3000 psi pressure, increasing the temperature led to an increase in the extraction yield.

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The present study evaluated the effect of supercritical fluid extraction (SFE) assisted by cold pressing (SFEAP) on the overall yield, extraction kinetics, composition of baru seed oil and manufacturing cost (COM). The best extraction conditions were determined in extraction assays combining different pressures (150-350 bar) and temperatures (35 and 45 °C). The extraction yield by SFEAP (28.6 g oil/100 g baru seed) was approximately 31% higher than that obtained by SFE (21.9 g oil/100 g baru seed), according to the kinetic study with the best extraction conditions (350 bar and 45 °C). The extraction yield observed under this condition allowed us to obtain a lower COM for both techniques (SFE was US$ 118.32/kg baru oil and SFEAP was US$ 87.03/kg baru oil) compared to lower pressures and temperatures. The oil obtained under all extraction conditions was rich in unsaturated fatty acids and other bioactive compounds. The extraction of baru seed oil by SFEAP resulted in a higher yield and lower manufacturing cost than SFE.