Supercritical Technology Applied to Food, Pharmaceutical and Chemical Industries

A special issue of Processes (ISSN 2227-9717). This special issue belongs to the section "Food Process Engineering".

Deadline for manuscript submissions: closed (30 September 2023) | Viewed by 43972

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School of Food Engineering (FEA), University of Campinas (UNICAMP), Rua Monteiro Lobato, 80, Campinas, SP 13083-862, Brazil
Interests: bioactive compounds; supercritical technology; supercritical extraction; supercritical chromatography; supercritical fluids and particles formation; formulation of functional foods using bioactive extracts obtained using supercritical fluids
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Grain Science and Industry Department, Kansas State University, Manhattan, KS 66506, USA
Interests: supercritical fluid technology; phenolic compounds; analytical chemistry; grain science; glycation; antioxidants; food processing; emerging technologies; agricultural wastes; bioactivity.
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Department of Agriculture and Forestry Engineering, Food Technology, College of Agricultural and Forestry Engineering, University of Valladolid, 34004 Valladolid, Spain
Interests: food science and technology; supercritical technology; natural products; bioactive compounds; solvent extraction; chromatography

Special Issue Information

Dear Colleagues,

Everyday life has made consumers genuinely concerned about the origin of the products they consume. Therefore, green technologies are overly requested in industrial processing for developing more and more products with a high-quality standard. One of these green technologies is the use of supercritical and pressurized fluids, which may be used in one or several stages of industrial processing.

This Special Issue intends to cover various aspects of supercritical technology applied to food, fuel, natural products, pharmaceuticals and materials processing. The manuscripts should focus on (the) extraction, particle formation, hydrolysis, gasification, reactions and catalysis, among other processes that employ high-pressure technologies in an environmentally friendly way. Uses of supercritical chromatography and hyphenated methods with supercritical fluids and pressurized liquids for food and drugs quality assessment are welcome. Modeling, survey papers and reviews are also welcomed.

Prof. Dr. Maria Angela A. Meireles
Dr. Ádina L. Santana
Dr. Grazielle Náthia-Neves
Guest Editors

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Keywords

  • bioactive compounds
  • supercritical technology
  • supercritical extraction
  • supercritical chromatography
  • supercritical fluids and particles formation
  • formulation of functional foods using bioactive extracts obtained using supercritical fluids
  • life cycle analysis of food processing using supercritical or pressurized solvents
  • process intensification with supercritical technology
  • analytical methods hyphenated with supercritical fluids and pressurized liquids
  • accelerated solvent extraction
  • chemical reactions assisted with supercritical fluids
  • characterization and biological activity of products processed with supercritical fluids and pressurized liquids

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Published Papers (16 papers)

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Editorial

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5 pages, 228 KiB  
Editorial
Supercritical Technology Applied to Food, Pharmaceutical, and Chemical Industries
by Ádina L. Santana
Processes 2024, 12(5), 861; https://doi.org/10.3390/pr12050861 - 25 Apr 2024
Viewed by 757
Abstract
Everyday life has caused consumers to feel genuine concern about the origin of the products they consume [...] Full article

Research

Jump to: Editorial, Review

39 pages, 5497 KiB  
Article
Molecular Modeling of Supercritical Processes and the Lattice—Gas Model
by Yuri Konstantinovich Tovbin
Processes 2023, 11(9), 2541; https://doi.org/10.3390/pr11092541 - 24 Aug 2023
Cited by 4 | Viewed by 1038
Abstract
The existing possibilities for modeling the kinetics of supercritical processes at the molecular level are considered from the point of view that the Second Law of thermodynamics must be fulfilled. The only approach that ensures the fulfillment of the Second Law of thermodynamics [...] Read more.
The existing possibilities for modeling the kinetics of supercritical processes at the molecular level are considered from the point of view that the Second Law of thermodynamics must be fulfilled. The only approach that ensures the fulfillment of the Second Law of thermodynamics is the molecular theory based on the discrete–continuous lattice gas model. Expressions for the rates of the elementary stage on its basis give a self-consistent description of the equilibrium states of the mixtures under consideration. The common usage today of ideal kinetic models in SC processes in modeling industrial chemistry contradicts the non-ideal equation of states. The used molecular theory is the theory of absolute reaction rates for non-ideal reaction systems, which takes into account intermolecular interactions that change the effective activation energies of elementary stages. This allows the theory to describe the rates of elementary stages of chemical transformations and molecular transport at arbitrary temperatures and reagent densities in different phases. The application of this theory in a wide range of state parameters (pressure and temperature) is considered when calculating the rates of elementary bimolecular reactions and dissipative coefficients under supercritical conditions. Generalized dependencies are calculated within the framework of the law of the corresponding states for the coefficients of compressibility, shear viscosity, and thermal conductivity of pure substances, and for the coefficients of compressibility, self- and mutual diffusion, and shear viscosity of binary mixtures. The effect of density and temperature on the rates of elementary stages under supercritical conditions has been demonstrated for a reaction’s effective energies of activation, diffusion and share viscosity coefficients, and equilibrium constants of adsorption. Differences between models with effective parameters and the prospects for developing them by allowing for differences in size and contributions from the vibrational motions of components are described. Full article
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18 pages, 2423 KiB  
Article
Post Acid Treatment on Pressurized Liquid Extracts of Sorghum (Sorghum bicolor L. Moench) Grain and Plant Material Improves Quantification and Identification of 3-Deoxyanthocyanidins
by Ádina L. Santana, Jaymi Peterson, Ramasamy Perumal, Changling Hu, Shengmin Sang, Kaliramesh Siliveru and Dmitriy Smolensky
Processes 2023, 11(7), 2079; https://doi.org/10.3390/pr11072079 - 12 Jul 2023
Cited by 2 | Viewed by 1393
Abstract
Sorghum is a unique natural food source of 3-deoxyanthocyanidins (3-DA) polyphenols. This work evaluated the effect of acidification on sorghum extracts post pressurized liquid extraction (PLE) and its ability to increase the identification and quantification of 3-DA. The sorghum genotypes included Sumac and [...] Read more.
Sorghum is a unique natural food source of 3-deoxyanthocyanidins (3-DA) polyphenols. This work evaluated the effect of acidification on sorghum extracts post pressurized liquid extraction (PLE) and its ability to increase the identification and quantification of 3-DA. The sorghum genotypes included Sumac and PI570366 (bran only) and SC991 (leaf and leaf sheath tissue). The acidification of the PLE extracts was carried out with methanol–HCl solutions at various concentrations (0, 0.5, 1, 2, and 4%, v/v). Changes in color were determined using L*a*b*. The overall phenolic composition was estimated with the total phenolic content and the DPPH free radical scavenging assays. Quantitative and qualitative chromatographic methods determined the phenolic profile. Color analysis showed that the redness and color saturation increased after acidification. No statistical difference was found in the total phenolic content of the acidified extracts, except for SC991, which was increased. There were no differences in the antioxidant capacity following acidification in all samples. For chromatographic analysis, luteolinidin was predominant in the extracts and the 3-DA content increased after acid treatment. However, some flavonoid and phenolic acid concentrations decreased following acid treatment, including taxifolin, quercetin, and chlorogenic acid. Interestingly, 0.5% v/v HCl acidification was sufficient to increase the color, allow the detection of 5-methoxyluteolinidin, and to increase luteolinidin and 7-methoxyapigenidin by at least twofold. Full article
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12 pages, 1256 KiB  
Article
Optimization of Supercritical Carbon Dioxide Fluid Extraction of Medicinal Cannabis from Quebec
by Hinane Boumghar, Mathieu Sarrazin, Xavier Banquy, Daria C. Boffito, Gregory S. Patience and Yacine Boumghar
Processes 2023, 11(7), 1953; https://doi.org/10.3390/pr11071953 - 28 Jun 2023
Cited by 6 | Viewed by 2812
Abstract
Research on cannabis oil has evolved to encompass the pharmaceutical industry for the therapeutic potential of the active compounds for pathologies such as Alzheimer, auto-immune disorders, and cancer. These debilitating diseases are best treated with cannabinoids such as tetrahydrocannabinol (∆9-THC), cannabigerol [...] Read more.
Research on cannabis oil has evolved to encompass the pharmaceutical industry for the therapeutic potential of the active compounds for pathologies such as Alzheimer, auto-immune disorders, and cancer. These debilitating diseases are best treated with cannabinoids such as tetrahydrocannabinol (∆9-THC), cannabigerol (CBG), and cannabinol (CBN), which relieve neuropathic pain and stimulate the immune system. We extracted cannabinoids from plants with supercritical CO2 and produced an extract with a total yield close to 26%. The three-level Box–Behnken experimental design considered four factors: Temperature, pressure, CO2 flow rate, and processing time, with predetermined parameters at low, medium, and high levels. The mathematical model was evaluated by regression analysis. The yield of ∆9-THC and CBG reached a maximum after 2 h and 15 g/min of CO2, 235 bar, 55 °C (64.3 g THC/100 g of raw material and 4.6 g CBG/100 g of raw material). After another 2 h of extraction time, the yield of CBN reached 2.4 g/100 g. The regression analysis identified pressure and time as the only significant factors for total yield while pressure was the only significant factor for ∆9-THC and CBG. Time, temperature, pressure, and flow rate were all significant factors for CBN. Full article
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10 pages, 1475 KiB  
Article
Modelling and Scaling-Up of a Supercritical Fluid Extraction of Emulsions Process
by Diego F. Tirado, Albertina Cabañas and Lourdes Calvo
Processes 2023, 11(4), 1063; https://doi.org/10.3390/pr11041063 - 1 Apr 2023
Cited by 7 | Viewed by 3391
Abstract
Supercritical CO2 (scCO2) is utilized in the supercritical fluid extraction of emulsions (SFEE) to swiftly extract the organic phase (O) from an O/W emulsion. The dissolved substances in the organic phase precipitate into small particles and remain suspended in the [...] Read more.
Supercritical CO2 (scCO2) is utilized in the supercritical fluid extraction of emulsions (SFEE) to swiftly extract the organic phase (O) from an O/W emulsion. The dissolved substances in the organic phase precipitate into small particles and remain suspended in the water (W) with the aid of a surfactant. The process can be continuously conducted using a packed column in a counter-current flow of the emulsion and scCO2, at moderate pressure (8–10 MPa) and temperature (37–40 °C). To ensure the commercial viability of this technique, the organic solvent must be separated from the CO2 to facilitate the recirculation of both streams within the process while minimizing environmental impact. Thus, the aim of this work was to design a plant to produce submicron materials using SFEE, integrating the recovery of both solvents. First, experimental equilibrium data of the ternary system involved (CO2/ethyl acetate/water) were fitted with a proper thermodynamic model. Then, simulations of the whole integrated process at different scales were carried out using Aspen Plus®, along with economical evaluations. This work proposes the organic solvent separation with a distillation column. Thus, the two solvents can be recovered and recycled to the process in almost their entirety. Furthermore, the particles in the aqueous raffinate are produced free of solvents and sterilized for further safe use. The costs showed an important economy scale-up. This work could ease the transfer of the SFEE technology to the industry. Full article
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15 pages, 1764 KiB  
Article
Fatty Acid Alkyl Ester Production by One-Step Supercritical Transesterification of Beef Tallow by Using Ethanol, Iso-Butanol, and 1-Butanol
by Ricardo García-Morales, Francisco J. Verónico-Sánchez, Abel Zúñiga-Moreno, Oscar A. González-Vargas, Edgar Ramírez-Jiménez and Octavio Elizalde-Solis
Processes 2023, 11(3), 742; https://doi.org/10.3390/pr11030742 - 2 Mar 2023
Cited by 3 | Viewed by 1892
Abstract
The effect of temperature was studied on the synthesis of fatty acid alkyl esters by means of transesterification of waste beef tallow using ethanol and, iso-butanol and 1-butanol at supercritical conditions. These alcohols are proposed for the synthesis of biodiesel in order to [...] Read more.
The effect of temperature was studied on the synthesis of fatty acid alkyl esters by means of transesterification of waste beef tallow using ethanol and, iso-butanol and 1-butanol at supercritical conditions. These alcohols are proposed for the synthesis of biodiesel in order to improve the cold flow properties of alkyl esters. Alcohol–beef tallow mixtures were fed to a high-pressure high-temperature autoclave at a constant molar ratio of 45:1. Reactions were carried out in the ranges of 310–390 °C and 310–420 °C for ethanol and iso-butanol, respectively; meanwhile, synthesis using 1-butanol was assessed only at 360 °C. After separation of fatty acid alkyl esters, these samples were characterized by nuclear magnetic resonance (NMR) and gas chromatography coupled to mass spectrometry (GC-MS) to quantify yields, chemical composition, and molecular weight. Results indicated that yields enhanced as temperature increased; the maximum yields for fatty acid ethyl esters (FAEEs) were attained at 360 °C, and for fatty acid butyl esters (FABEs) were achieved at 375 °C; beyond these conditions, the alkyl ester yields reached equilibrium. Concerning the physicochemical properties of biodiesel, the predicted cetane number and cloud point were enhanced compared to those of fatty acid methyl esters. Full article
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18 pages, 1643 KiB  
Article
Pilot-Plant-Scale Extraction of Antioxidant Compounds from Lavender: Experimental Data and Methodology for an Economic Assessment
by Encarnación Cruz Sánchez, Jesús Manuel García-Vargas, Ignacio Gracia, Juan Francisco Rodríguez and María Teresa García
Processes 2022, 10(12), 2708; https://doi.org/10.3390/pr10122708 - 15 Dec 2022
Cited by 6 | Viewed by 2432
Abstract
The techno-economic feasibility of lavender essential oil supercritical CO2 extraction was studied. The process was scaled up to a pilot plant, and the extraction yield, composition, and antioxidant potential of the extracts were evaluated at 60 °C and 180 bar or 250 [...] Read more.
The techno-economic feasibility of lavender essential oil supercritical CO2 extraction was studied. The process was scaled up to a pilot plant, and the extraction yield, composition, and antioxidant potential of the extracts were evaluated at 60 °C and 180 bar or 250 bar, achieving a maximum yield of 6.9% and a percentage inhibition of the extracts of more than 80%. These results drove the development of a business plan for three scenarios corresponding to different extraction volumes (20, 50, and 100 L) and annual production. The SWOT matrix showed that this is a promising business idea. The COM was calculated and an investment analysis was performed. The profitability of this process was demonstrated by means of a financial analysis for 8 years, considering a selling price of 1.38 EUR/g for the extract from the 20 L plant and 0.9 EUR/g for industrial-scale plants, supported by the price curve. The sensitivity analysis showed that the price of the equipment was the factor that could most influence the robustness of the project and the business strategy, and the financial ratios evaluation resulted in a ROE value above 57% in all cases, indicating the economic attractiveness of the process. Full article
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19 pages, 11717 KiB  
Article
Carotenoids Recovery Enhancement by Supercritical CO2 Extraction from Tomato Using Seed Oils as Modifiers
by Mihaela Popescu, Petrica Iancu, Valentin Plesu and Costin Sorin Bildea
Processes 2022, 10(12), 2656; https://doi.org/10.3390/pr10122656 - 9 Dec 2022
Cited by 3 | Viewed by 2185
Abstract
The food, cosmetic and pharmaceutical industries have strong demands for lycopene, the carotenoid with the highest antioxidant activity. Usually, this carotenoid is extracted from tomatoes using various extraction methods. This work aims to improve the quantity and quality of extracts from tomato slices [...] Read more.
The food, cosmetic and pharmaceutical industries have strong demands for lycopene, the carotenoid with the highest antioxidant activity. Usually, this carotenoid is extracted from tomatoes using various extraction methods. This work aims to improve the quantity and quality of extracts from tomato slices by enhancing the recovery of the carotenoids from the solid matrix to the solvent using 20 w/w% seeds as modifiers and supercritical CO2 extraction with optimal parameters as the method. Tomato (TSM), camelina (CSM) and hemp (HSM) seeds were used as modifiers due to their quality (polyunsaturated fatty acids content of 53–72%). A solubility of ~10 mg carotenoids/100 g of oil was obtained for CSM and HSM, while, for TSM, the solubility was 28% higher (due to different compositions of long carbon chains). An increase in the extraction yield from 66.00 to 108.65 g extract/kg dried sample was obtained in the following order: TSM < HSM < CSM. Two products, an oil rich in carotenoids (203.59 mg/100 g extract) and ω3-linolenic acid and a solid oleoresin rich in lycopene (1172.32 mg/100 g extract), were obtained using SFE under optimal conditions (450 bar, 70 °C, 13 kg/h and CSM modifier), as assessed by response surface methodology. A recommendation is proposed for the use of these products in the food industry based on their quality. Full article
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12 pages, 13294 KiB  
Article
Efficacy of Supercritical Fluid Decellularized Porcine Acellular Dermal Matrix in the Post-Repair of Full-Thickness Abdominal Wall Defects in the Rabbit Hernia Model
by Yen-Lung Chiu, Yun-Nan Lin, Yun-Ju Chen, Srinivasan Periasamy, Ko-Chung Yen and Dar-Jen Hsieh
Processes 2022, 10(12), 2588; https://doi.org/10.3390/pr10122588 - 4 Dec 2022
Cited by 4 | Viewed by 2511
Abstract
Damage to abdominal wall integrity occurs in accidents, infection and herniation. Repairing the hernia remains to be one of the most recurrent common surgical techniques. Supercritical carbon dioxide (SCCO2) was used to decellularize porcine skin to manufacture acellular dermal matrix (ADM) [...] Read more.
Damage to abdominal wall integrity occurs in accidents, infection and herniation. Repairing the hernia remains to be one of the most recurrent common surgical techniques. Supercritical carbon dioxide (SCCO2) was used to decellularize porcine skin to manufacture acellular dermal matrix (ADM) for the reparation of full-thickness abdominal wall defects and hernia. The ADM produced by SCCO2 is chemically equivalent and biocompatible with human skin. The ADM was characterized by hematoxylin and eosin (H&E) staining, 4,6-Diamidino-2-phenylindole, dihydrochloride (DAPI) staining, residual deoxyribonucleic acid (DNA) contents and alpha-galactosidase (α-gal staining), to ensure the complete decellularization of ADM. The ADM mechanical strength was tested following the repair of full-thickness abdominal wall defects (4 × 4 cm) created on the left and right sides in the anterior abdominal wall of New Zealand White rabbits. The ADM produced by SCCO2 technology revealed complete decellularization, as characterized by H&E, DAPI staining, DNA contents (average of 26.92 ng/mg) and α-gal staining. In addition, ADM exhibited excellent performance in the repair of full-thickness abdominal wall defects. Furthermore, the mechanical strength of the reconstructed abdominal wall after using ADM was significantly (p < 0.05) increased in suture retention strength (30.42 ± 1.23 N), tear strength (63.45 ± 7.64 N and 37.34 ± 11.72 N) and burst strength (153.92 ± 20.39 N) as compared to the suture retention (13.33 ± 5.05 N), tear strength (6.83 ± 0.40 N and 15.27 ± 3.46 N) and burst strength (71.77 ± 18.09 N) when the predicate device materials were concomitantly tested. However, the efficacy in hernia reconstruction of ADM is substantially equivalent to that of predicate material in both macroscopic and microscopic observations. To conclude, ADM manufactured by SCCO2 technology revealed good biocompatibility and excellent mechanical strength in post-repair of full-thickness abdominal wall defects in the rabbit hernia model. Full article
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15 pages, 1372 KiB  
Article
Inactivation of Clostridium Spores in Honey with Supercritical CO2 and in Combination with Essential Oils
by Alejandro Dacal-Gutiérrez, Diego F. Tirado and Lourdes Calvo
Processes 2022, 10(11), 2232; https://doi.org/10.3390/pr10112232 - 31 Oct 2022
Cited by 5 | Viewed by 2815
Abstract
The presence of tens of Clostridium botulinum spores per gram of honey can cause infantile botulism. Thermal treatment is insufficient to inactivate these resistant forms. This study explored the effectiveness of supercritical CO2 (scCO2) on its own and combined with [...] Read more.
The presence of tens of Clostridium botulinum spores per gram of honey can cause infantile botulism. Thermal treatment is insufficient to inactivate these resistant forms. This study explored the effectiveness of supercritical CO2 (scCO2) on its own and combined with lemon (LEO), clove (CLEO), and cinnamon (CEO) essential oils on the inactivation of Clostridium sporogenes (CECT 553) as a surrogate of Clostridium botulinum. In water, the degree of inactivation at 10 MPa after 60 min increased with the increasing temperature, reducing the population by 90% at 40 °C and by 99.7% at 80 °C. In contrast, when applied to honey, scCO2 did not inactivate Clostridium spores satisfactorily at temperatures below 70 °C, which was related to the protective effect of honey. Meanwhile, scCO2 modified with CEO (<0.4% mass) improved the inactivation degree, with a 1.3-log reduction achieved at 60 °C. With this same mixture, a reduction of 3.7 logs was accomplished in a derivative with 70% moisture. Honey was very sensitive to the temperature of the applied CO2. The obtained product could be used as a novel food, food ingredient, cosmetic, or medicine. Full article
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12 pages, 1619 KiB  
Article
Optimization of Subcritical Fluid Extraction for Total Saponins from Hedera nepalensis Leaves Using Response Surface Methodology and Evaluation of Its Potential Antimicrobial Activity
by Hoang Thanh Duong, Ly Hai Trieu, Do Thi Thuy Linh, Le Xuan Duy, Le Quang Thao, Le Van Minh, Nguyen Tuan Hiep and Nguyen Minh Khoi
Processes 2022, 10(7), 1268; https://doi.org/10.3390/pr10071268 - 27 Jun 2022
Cited by 2 | Viewed by 2403
Abstract
(1) Background: Hedera nepalensis (Araliaceae) is a recognized medicinal plant founded in Asia that has been reported to work in antioxidant, antifungal, antimicrobial, and antitumor capacities. (2) Methods: The subcritical fluid extraction of saponin from Hedera nepalensis leaves and the optimum of the [...] Read more.
(1) Background: Hedera nepalensis (Araliaceae) is a recognized medicinal plant founded in Asia that has been reported to work in antioxidant, antifungal, antimicrobial, and antitumor capacities. (2) Methods: The subcritical fluid extraction of saponin from Hedera nepalensis leaves and the optimum of the extraction process based on yield of saponin contents (by calculating the hederacoside C contents in dried Hedera nepalensis leaves) are examined by response surface methodology (RSM). Furthermore, the antimicrobial activity of the extract is tested for potential drug applications in the future. (3) Results: Based upon RSM data, the following parameters are optimal: extraction time of 3 min, extraction temperature of 150 °C, and a sample/solvent ratio of 1:55 g/mL. Under such circumstances, the achieved yield of saponin is 1.879%. Moreover, the extracts inhibit the growth of some bacterial strains (Streptococcus pneumoniae, Streptococcus pyogenes, Haemophilus influenza) at a moderate to strong level with inhibition zone diameter values ranging from 12.63 to 19.50 mm. (4) Conclusions: The development of such a model provides a robust experimental process for optimizing the extraction factors of saponin contents from Hedera nepalensis extract using subcritical fluid extraction and RSM. Moreover, the current work reveals that saponin extracts of Hedera nepalensis leaves exhibit a potential antimicrobial activity, which can be used as scientific evidence for further study. Full article
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16 pages, 2517 KiB  
Article
Production of Oil and Phenolic-Rich Extracts from Mauritia flexuosa L.f. Using Sequential Supercritical and Conventional Solvent Extraction: Experimental and Economic Evaluation
by Ivan Best, Zaina Cartagena-Gonzales, Oscar Arana-Copa, Luis Olivera-Montenegro and Giovani Zabot
Processes 2022, 10(3), 459; https://doi.org/10.3390/pr10030459 - 24 Feb 2022
Cited by 9 | Viewed by 3079
Abstract
Mauritia flexuosa L.f. is a palm from the Amazon. Pulp and oil are extracted from its fruits, with a high content of bioactive compounds. This study presents the economic evaluation of two extraction processes: (a) Conventional solvent extraction (CSE) with 80% ethanol for [...] Read more.
Mauritia flexuosa L.f. is a palm from the Amazon. Pulp and oil are extracted from its fruits, with a high content of bioactive compounds. This study presents the economic evaluation of two extraction processes: (a) Conventional solvent extraction (CSE) with 80% ethanol for the recovery of phenolic-rich extracts; and (b) Supercritical fluid extraction (SFE) followed by CSE to obtain oil and phenolic-rich extracts. The objective of this study was to compare the feasibility of both extraction processes. The economic evaluation and the sensitivity study were evaluated using the SuperPro Designer 9.0® software at an extraction volume of 2000 L. Similar global extraction yields were obtained for both processes; however, 8.4 and 2.4 times more total polyphenol and flavonoid content were extracted, respectively, using SFE+CSE. Cost of manufacturing (COM) was higher in SFE+CSE compared to CSE, USD 193.38/kg and USD 126.47/kg, respectively; however, in the first process, two by-products were obtained. The sensitivity study showed that the cost of the raw material was the factor that had the highest impact on COM in both extraction processes. SFE+CSE was the most economically viable process for obtaining bioactive compounds on an industrial scale from M. flexuosa L.f. Full article
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15 pages, 3776 KiB  
Article
Supercritical Technology-Based Date Sugar Powder Production: Process Modeling and Simulation
by Hooralain Bushnaq, Rambabu Krishnamoorthy, Mohammad Abu-Zahra, Shadi W. Hasan, Hanifa Taher, Suliman Yousef Alomar, Naushad Ahmad and Fawzi Banat
Processes 2022, 10(2), 257; https://doi.org/10.3390/pr10020257 - 27 Jan 2022
Cited by 9 | Viewed by 4043
Abstract
Date palm fruits (Phoenix dactylifera) contain high levels of fructose and glucose sugars. These natural sugar forms are healthy, nutritional and easily assimilate into human metabolism. The successful production of soluble date sugar powder from nutritious date fruits would result in [...] Read more.
Date palm fruits (Phoenix dactylifera) contain high levels of fructose and glucose sugars. These natural sugar forms are healthy, nutritional and easily assimilate into human metabolism. The successful production of soluble date sugar powder from nutritious date fruits would result in a new food product that could replace the commercial refined sugar. In this work, a novel process technology based on the supercritical extraction of sugar components from date pulp was modeled and simulated using Aspen Plus software. The process model consisted of three main steps that were individually simulated for their optimal working conditions as follows: (a) freeze-drying of the date pulp at −42 °C and 0.0001 bar; (b) supercritical extraction of the sugar components using a 6.77 wt.% water mixed CO2 solvent system at a pressure of 308 bar, temperature of 65 °C, and CO2 flow rate of 31,000 kg/h; and (c) spray-drying of the extract using 40 wt.% Gum Arabic as the carrier agent and air as drying medium at 150 °C. The overall production yield of the process showed an extraction efficiency of 99.1% for the recovery of total reducing sugars from the date fruit. The solubility of the as-produced date sugar powder was improved by the process selectivity, elimination of insoluble fiber contents, and the addition of Gum Arabic. The solubility of the final date sugar product was estimated as 0.89 g/g water. Full article
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15 pages, 1387 KiB  
Article
Fractional Factorial Design Study for the Extraction of Cannabinoids from CBD-Dominant Cannabis Flowers by Supercritical Carbon Dioxide
by Sadia Qamar, Yady J. M. Torres, Harendra S. Parekh and James Robert Falconer
Processes 2022, 10(1), 93; https://doi.org/10.3390/pr10010093 - 3 Jan 2022
Cited by 14 | Viewed by 4852
Abstract
The optimization of the supercritical fluid extraction (SFE) of cannabinoids, using supercritical carbon dioxide (scCO2), was investigated in a fractional factorial design study. It is hypothesized that four main parameters (temperature, pressure, dry flower weight, and extraction time) play an important [...] Read more.
The optimization of the supercritical fluid extraction (SFE) of cannabinoids, using supercritical carbon dioxide (scCO2), was investigated in a fractional factorial design study. It is hypothesized that four main parameters (temperature, pressure, dry flower weight, and extraction time) play an important role. Therefore, these parameters were screened at predetermined low, medium, and high relative levels. The density of scCO2 was used as a factor for the extraction of cannabinoids by changing the pressure and temperature. The robustness of the mathematical model was also evaluated by regression analysis. The quantification of major (cannabidiol (CBD), cannabidiolic acid (CBDA), delta 9-tetrahydrocannabinol (Δ9-THC), delta 8-tetrahydrocannabinol (Δ8-THC), and delta 9-tetrahydrocannabinol acid (THCA-A)) and minor (cannabidivann (CBDV), tetrahydrocannabivann (THCV), cannabigerolic acid (CBG), cannabigerol (CBGA), cannabinol (CBN), and cannabichomere (CBC)) cannabinoids in the scCO2 extract was performed by RP-HPLC analysis. From the model response, it was identified that long extraction time is a significant parameter to obtain a high yield of cannabinoids in the scCO2 extract. Higher relative concentrations of CBD(A) (0.78 and 2.41% w/w, respectively) and THC(A) (0.084 and 0.048% w/w, respectively) were found when extraction was performed at high relative pressures and temperatures (250 bar and 45 °C). The higher yield of CBD(A) compared to THC(A) can be attributed to the extract being a CBD-dominant cannabis strain. The study revealed that conventional organic solvent extraction, e.g., ethanol gives a marginally higher yield of cannabinoids from the extract compared to scCO2 extraction. However, scCO2 extraction generates a cleaner (chlorophyll-free) and organic solvent-free extract, which requires less downstream processing, such as purification from waxes and chlorophyll. Full article
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12 pages, 1883 KiB  
Article
Ultrasound-Assisted Extraction of Semi-Defatted Unripe Genipap (Genipa americana L.): Selective Conditions for the Recovery of Natural Colorants
by Grazielle Náthia-Neves, Ádina L. Santana, Juliane Viganó, Julian Martínez and Maria Angela A. Meireles
Processes 2021, 9(8), 1435; https://doi.org/10.3390/pr9081435 - 19 Aug 2021
Cited by 8 | Viewed by 2075
Abstract
Ultrasound-assisted extraction (UAE) of semi-defatted unripe genipap (SDG) using supercritical CO2 was performed to enhance the recovery of natural colorant iridoids genipin and geniposide. There are currently few natural sources of iridoids, and their application as colorants is scarce. The UAE resulted [...] Read more.
Ultrasound-assisted extraction (UAE) of semi-defatted unripe genipap (SDG) using supercritical CO2 was performed to enhance the recovery of natural colorant iridoids genipin and geniposide. There are currently few natural sources of iridoids, and their application as colorants is scarce. The UAE resulted in extracts with blue and green colors using water and ethanol, respectively. The highest global yield and genipin content was recovered with water, and the geniposide was significantly recovered with ethanol. With water at 450 W, the UAE raised the maximum global yield (25.50 g/100 g raw material). At 150 W and 7 min, the maximum content of genipin (121.7 mg/g extract) and geniposide (312 mg/g extract) was recovered. The total phenolic content (TPC) and antioxidant capacity with the oxygen reactive antioxidant capacity (ORAC) assay were also high in aqueous extracts. Ethanolic extracts showed high ferric-reducing ability antioxidant potential (FRAP) values. UAE showed an efficient and fast method to obtain different extracts’ fractions from SDG, which have a wide spectrum of applications, especially as natural food colorants. Full article
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Review

Jump to: Editorial, Research

20 pages, 2186 KiB  
Review
Valorization of Cereal Byproducts with Supercritical Technology: The Case of Corn
by Ádina L. Santana and Maria Angela A. Meireles
Processes 2023, 11(1), 289; https://doi.org/10.3390/pr11010289 - 16 Jan 2023
Cited by 7 | Viewed by 3828
Abstract
Ethanol and starch are the main products generated after the processing of corn via dry grinding and wet milling, respectively. Milling generates byproducts including stover, condensed distillers’ solubles, gluten meal, and the dried distillers’ grains with solubles (DDGS), which are sources of valuable [...] Read more.
Ethanol and starch are the main products generated after the processing of corn via dry grinding and wet milling, respectively. Milling generates byproducts including stover, condensed distillers’ solubles, gluten meal, and the dried distillers’ grains with solubles (DDGS), which are sources of valuable compounds for industry including lignin, oil, protein, carotenoids, and phenolic compounds. This manuscript reviews the current research scenario on the valorization of corn milling byproducts with supercritical technology, as well as the processing strategies and the challenges of reaching economic feasibility. The main products recently studied were biodiesel, biogas, microcapsules, and extracts of enriched nutrients. The pretreatment of solid byproducts for further hydrolysis to produce sugar oligomers and bioactive peptides is another recent strategy offered by supercritical technology to process corn milling byproducts. The patents invented to transform corn milling byproducts include oil fractionation, extraction of undesirable flavors, and synthesis of structured lipids and fermentable sugars. Process intensification via the integration of milling with equipment that operates with supercritical fluids was suggested to reduce processing costs and to generate novel products. Full article
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