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A special issue of Processes (ISSN 2227-9717). This special issue belongs to the section "Chemical Processes and Systems".

Deadline for manuscript submissions: closed (28 February 2021) | Viewed by 57147

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Prof. Dr. Yizhak Marcus

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Guest Editor

Institute of Chemistry, The Hebrew University of Jerusalem, Jerusalem 91904, Israel
Interests: The chemistry of liquids and solutions, dealing with inter alia with solvent properties and applications, including those of supercritical fluids, as well as liquid–liquid solvent extraction

Special Issue Information

Dear Colleagues,

The search for neoteric solvents to replace ecologically unfriendly organic solvents, in addition to room temperature ionic liquids and deep eutectic solvents, also includes supercritical solvents. The latter are used as reaction media and for the extraction of valuable substances from a variety of materials. The term ‘supercritical fluid extraction’ is generally applied to the use of supercritical carbon dioxide, neat or with entrainers (co-solvents). However, this term should also include other fluids, namely supercritical water, methanol, or ethanol, among a few others.

The use of supercritical carbon dioxide for the decaffeination of coffee beans is presently a well-established industry, but decaffeination of other beverages is coming to the forefront. Other uses of supercritical carbon dioxide are for extraction processes in the food industry and in the pharmaceutical and cosmetic industries, and these are maturing. On the other hand, supercritical water has found uses in the fuel production industry for extraction of liquid or gaseous fuels from coal or the conversion of plant biomass to biodiesel oil. Supercritical methanol is useful for transesterification processes during such extractions.

It is the purpose of this Special Issue of Process on “Advances in Supercritical Fluid Extraction” to highlight recent progress and to point out trends, prospects, and areas in which further research will be very beneficial for this area.

Prof. Dr. Yizhak Marcus
Guest Editor

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Keywords

supercritical carbon dioxide
supercritical water
supercritical methanol
supercritical ethanol
food industry
pharmaceutical industry
cosmetic industry
fuel processing
biomass processing
coal

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Published Papers (10 papers)

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18 pages, 3293 KiB

Open AccessFeature PaperArticle

Supercritical Carbon Dioxide + Ethanol Extraction to Improve Organoleptic Attributes of Pea Flour with Applications of Sensory Evaluation, HS-SPME-GC, and GC-Olfactory

by Serap Vatansever, Minwei Xu, Ana Magallanes-López, Bingcan Chen and Clifford Hall

Processes 2021, 9(3), 489; https://doi.org/10.3390/pr9030489 - 9 Mar 2021

Cited by 18 | Viewed by 3278

Abstract

Supercritical carbon dioxide + ethanol (SC-CO₂+EtOH) extraction, was employed as a deflavoring method to improve the sensory properties of pea flours. Furthermore, the impacts of particle size along with extraction on volatile profile and sensory attributes of pea flours were investigated using multiple approaches. These included headspace solid-phase microextraction-gas chromatography (HS-SPME-GC), GC-olfactometry (GC-O), and quantitative descriptive analysis (QDA) using a trained sensory panel. Total volatile contents of non-deflavored and deflavored whole pea flour and its fractions were in the range of 7.1 ± 0.3 to 18.1 ± 1.0 µg/g and 0.4 ± 0.1 to 2.7 ± 0.4 µg/g, respectively. The GC-O system showed that the total volatile intensity was in the range of 14.5 to 22.0 and 0 to 3.5, for non-deflavored and deflavored pea flours, respectively. Volatile analyses indicated that 1-hexanol, 1-octanol, 1-nonanol, nonanal, and 2-alkyl methoxypyrazines were major off-aroma compounds. Most off-aroma compounds were not detected in deflavored pea flours. QDA revealed less pea intensity and bitterness of deflavored pea flours. The larger particle size of flours resulted in less off-aroma compounds based on the GC data but more bitterness based on QDA. The SC-CO₂+EtOH extraction at optimum conditions and particle size modifications can be a potential technology to improve the organoleptic properties of pulse ingredients. Full article

(This article belongs to the Special Issue Advances in Supercritical Fluid Extraction)

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13 pages, 2390 KiB

Open AccessArticle

Effects of Temperature and Extraction Time on Avocado Flesh (Persea americana) Total Phenolic Yields Using Subcritical Water Extraction

by Walid I. Mazyan, Ellen O’Connor, Elia Martin, Anja Vogt, Edward Charter and Ali Ahmadi

Processes 2021, 9(1), 159; https://doi.org/10.3390/pr9010159 - 15 Jan 2021

Cited by 6 | Viewed by 2687

Abstract

This paper investigates the optimum extraction temperature for enhanced total phenolic yields extracted from avocado fruit flesh (Persea americana) using subcritical water extraction, as well as the impact of fruit ripeness on phenol extraction efficiency. Additionally, extraction yield against extraction time was investigated for time intervals of 10 min over an overall extraction time of 30 min. The subcritical water conditions studied were 18 bar, 87 mL/min, and temperatures of 105 °C, 120 °C, and 140 °C. The total phenolic compounds content was compared for week one avocado flesh and ripe (week four) avocado flesh, with a four-week ripening period between the two samples. The results show that extracting with subcritical water at 105 °C provides the highest phenolic compounds yields of 0.11% and 0.26% by dried mass for week one and ripe fruit (week four), respectively. The experimental results also indicate that the implementation of lower extraction temperatures on week four avocado (i.e., following the selection of week one avocados and allowing them to ripen over a period of one month) enhances the phenolic compounds extraction yields by more than four times relative to the first week’s sample extract, specifically during the first 20 min of extraction. Full article

(This article belongs to the Special Issue Advances in Supercritical Fluid Extraction)

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19 pages, 3332 KiB

Open AccessArticle

Extraction of Anthocyanins from Red Raspberry for Natural Food Colorants Development: Processes Optimization and In Vitro Bioactivity

by Rosiane Rocha, José Pinela, Rui M.V. Abreu, Mikel Añibarro-Ortega, Tânia C.S.P. Pires, Ana Luísa Saldanha, Maria José Alves, António Nogueira, Isabel C.F.R. Ferreira and Lillian Barros

Processes 2020, 8(11), 1447; https://doi.org/10.3390/pr8111447 - 11 Nov 2020

Cited by 32 | Viewed by 7505

Abstract

Heat (HAE)- and ultrasound (UAE)-assisted extraction methods were implemented to recover anthocyanins from red raspberry. Processing time, ethanol concentration, and temperature or ultrasonic power were the independent variables combined in five-level rotatable central composite designs coupled with response surface methodology (RSM) for processes optimization. The extraction yield and levels of cyanidin-3-O-sophoroside (C3S) and cyanidin-3-O-glucoside (C3G) were monitored by gravimetric and HPLC-DAD-ESI/MSⁿ methods, respectively, and used as response criteria. The constructed theoretical models were successfully fitted to the experimental data and used to determine the optimal extraction conditions. When maximizing all responses simultaneously, HAE originated slightly higher response values (61% extract weight and 8.7 mg anthocyanins/g extract) but needed 76 min processing at 38 °C, with 21% ethanol (v/v), while the UAE process required 16 min sonication at 466 W, using 38% ethanol (v/v). The predictive models were experimentally validated, and the purple-red extracts obtained under optimal condition showed antioxidant activity through lipid peroxidation and oxidative hemolysis inhibition, and antibacterial effects against food-related microorganisms, such as Escherichia coli and Enterococcus faecalis. These results highlight the potential of red raspberry extracts as natural food colorants with bioactive effects and could be exploited by industries interested in the production of anthocyanin-based products. Full article

(This article belongs to the Special Issue Advances in Supercritical Fluid Extraction)

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14 pages, 2487 KiB

Open AccessArticle

Subcritical Water Extraction of Epigallocatechin Gallate from Camellia sinensis and Optimization Study Using Response Surface Methodology

by Nguyen Tuan Hiep, Hoang Thanh Duong, Dang Tuan Anh, Nguyen Hoai Nguyen, Do Quang Thai, Do Thi Thuy Linh, Vu Thi Huong Anh and Nguyen Minh Khoi

Processes 2020, 8(9), 1028; https://doi.org/10.3390/pr8091028 - 22 Aug 2020

Cited by 7 | Viewed by 4363

Abstract

Background: Camellia sinensis is a plant whose leaves and buds are used to produce tea. With many medicinal activities already found, green tea has been consumed widely in the world. Methods: The subcritical water extraction (SWE) of epigallocatechin gallate (EGCG) from green tea leaves and the effect of the different extraction conditions are investigated by response surface methodology (RSM). Furthermore, the model of the extraction processes is reviewed for application at the industrial scale. Results: Based on the RSM data, the maximum yield of extraction is determined via optimizing different parameters of the extraction processes. Optimal conditions are as follows: extraction time of 6 min, extraction temperature at 120 °C, and a sample/solvent ratio of 1:40 g/mL. Under such conditions, the best yield of EGCG is 4.665%. Moreover, the model of the extraction processes, which can be utilized for industry scale purpose, indicates a good correlation with the experimental data. Conclusions: Overall, SWE is competent and environmental-friendly, and it is also a highly selective and fast method. SWE is a promising method to take the place of organic solvents used in the extraction of weak polar and even non-polar natural compounds. Further studies on the scale-up of the extraction processes are ongoing. Full article

(This article belongs to the Special Issue Advances in Supercritical Fluid Extraction)

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13 pages, 3132 KiB

Open AccessArticle

Mathematical Model for the Removal of Essential Oil Constituents during Steam Distillation Extraction

by Sharad Maharaj and David McGaw

Processes 2020, 8(4), 400; https://doi.org/10.3390/pr8040400 - 29 Mar 2020

Cited by 11 | Viewed by 6960

Abstract

Steam distillation is the conventional means by which oils are extracted in the flavour and fragrance industry. A mathematical model for the steam distillation extraction (SDE) of air-dried Ocimum basilicum (basil) leaves has been developed and tested using a small-scale pilot plant. The model predicts the removal of oil components from the plant matrix and subsequent transfer to the steam. It also accounts for the diffusional transfer of components within the leaf and the simultaneous convective transfer into the vapour phase while also respecting the individual components’ volatilities. It has been applied vertically on an element-by-element basis through the bed for a mixture of major and minor components. The proposed SDE model appears to be a good match between predicted values and the experimental data. The model predicts a faster initial extraction rate for components such as α-pinene and α-terpinene, possibly due to preferential extraction of light, volatile components present in larger quantities. Full article

(This article belongs to the Special Issue Advances in Supercritical Fluid Extraction)

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15 pages, 10148 KiB

Open AccessArticle

Depigmented Centella asiatica Extraction by Pretreated with Supercritical Carbon Dioxide Fluid for Wound Healing Application

by Warintorn Ruksiriwanich, Chiranan Khantham, Korawan Sringarm, Sarana Sommano and Pensak Jantrawut

Processes 2020, 8(3), 277; https://doi.org/10.3390/pr8030277 - 28 Feb 2020

Cited by 22 | Viewed by 7122

Abstract

Centella asiatica has been included in Thai traditional medicinal plants and recipes, as a well-established historical use as a vegetable and tonic. However, when applied in modern formulations, the progressive degradation of the plant pigments occurs, causing color-fading and color variation in the products. Depigmentation of the comminuted sample using supercritical carbon dioxide (scCO₂) fluid extraction with a cosolvent was introduced as a pretreatment to solve the color-fading problem. The contents of compounds with known biological activities and the wound healing activities (antioxidant screening by DPPH and ABTS⁺ scavenging activities; cell migration assay; matrix metallopeptidase [MMP]-2 inhibition on human skin fibroblast; endothelial cell tube formation assay) of the C. asiatica leaf extracts obtained by conventional ethanolic extraction (CV) and pretreatment using scCO₂ extraction, were determined. Total triterpenoids (madecassoside, asiaticoside B, asiaticoside, madecassic acid, terminolic acid and asiatic acid) and total triterpenoid glucosides (madecassoside, asiaticoside B and asiaticoside) were notably more abundant in the extract that had been pretreated using scCO₂ than the extract obtained by CV. Moreover, the scCO₂ pretreatment not only caused greater relative MMP-2 inhibition (58.48 ± 7.50% of the control), but also exhibited a higher cell migration (59.83 ± 1.85% of the initial) and number of vessels (18.25 ± 4.58) of angiogenesis in the wound healing process. Additionally, positive correlations were observed between the DPPH antioxidant activity and madecassoside content (r = 0.914, p < 0.01), as well as between the cell migration activity and asiaticoside content (r = 0.854, p < 0.05). It can be concluded that the scCO₂ pretreatment of C. asiatica can eliminate color pigments from the extract and improve its in vitro wound healing activity. Full article

(This article belongs to the Special Issue Advances in Supercritical Fluid Extraction)

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23 pages, 7768 KiB

Open AccessArticle

Thermodynamic Analysis of Supercritical Carbon Dioxide Cycle for Internal Combustion Engine Waste Heat Recovery

by Wan Yu, Qichao Gong, Dan Gao, Gang Wang, Huashan Su and Xiang Li

Processes 2020, 8(2), 216; https://doi.org/10.3390/pr8020216 - 12 Feb 2020

Cited by 10 | Viewed by 3656

Abstract

Waste heat recovery of the internal combustion engine (ICE) has attracted much attention, and the supercritical carbon dioxide (S-CO₂) cycle was considered as a promising technology. In this paper, a comparison of four S-CO₂ cycles for waste heat recovery from the ICE was presented. Improving the exhaust heat recovery ratio and cycle thermal efficiency were significant to the net output power. A discussion about four different cycles with different design parameters was conducted, along with a thermodynamic performance. The results showed that choosing an appropriate inlet pressure of the compressor could achieve the maximum exhaust heat recovery ratio, and the pressure increased with the rising of the turbine inlet pressure and compressor inlet temperature. The maximum exhaust heat recovery ratio for recuperation and pre-compression of the S-CO₂ cycle were achieved at 7.65 Mpa and 5.8 MPa, respectively. For the split-flow recompression cycle, thermal efficiency first increased with the increasing of the split ratio (SR), then decreased with a further increase of the SR, but the exhaust heat recovery ratio showed a sustained downward trend with the increase of the SR. For the split-flow expansion cycle, the optimal SR was 0.43 when the thermal efficiency and exhaust heat recovery ratio achieved the maximum. The highest recovery ratio was 24.75% for the split-flow expansion cycle when the total output power, which is the sum of the ICE power output and turbine mechanical power output, increased 15.3%. The thermal performance of the split-flow expansion cycle was the best compared to the other three cycles. Full article

(This article belongs to the Special Issue Advances in Supercritical Fluid Extraction)

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10 pages, 1934 KiB

Open AccessArticle

Extraction of Oil and Minor Compounds from Oil Palm Fruit with Supercritical Carbon Dioxide

by Huan Phan Tai and Gerd Brunner

Processes 2019, 7(2), 107; https://doi.org/10.3390/pr7020107 - 18 Feb 2019

Cited by 15 | Viewed by 7629

Abstract

A significant quantity of tocochromanols and carotenoids remains in the residual from palm oil production by traditional screw pressing. Supercritical carbon dioxide extraction was used as alternative method with the purpose to recover better these valuable minor compounds. Total oil yield and co-extracted water were investigated in the course of extraction. Tocochromanols and carotenoids were evaluated, not only in the extraction oil, but also in the oil of residual fibre. Modelling of extraction process was also performed for a further up-scaling. The results showed that oil yield up to 90% could be observed within 120 min. Supercritical carbon dioxide (SCCO₂) could extract tocochromanols and carotenoids with concentration in the same range of normal commercial processing palm oil, while co-extracted water remained rather low at a level of 2–4%. Moreover, recovery efficiencies of these minor compounds were much higher in case of extraction processed with supercritical carbon dioxide than those with screw pressing method. Full article

(This article belongs to the Special Issue Advances in Supercritical Fluid Extraction)

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10 pages, 1967 KiB

Open AccessArticle

Energy Analysis of the S-CO₂ Brayton Cycle with Improved Heat Regeneration

by Muhammad Ehtisham Siddiqui and Khalid H. Almitani

Processes 2019, 7(1), 3; https://doi.org/10.3390/pr7010003 - 20 Dec 2018

Cited by 24 | Viewed by 5123

Abstract

Supercritical carbon dioxide (S-CO₂) Brayton cycles (BC) are promising alternatives for power generation. Many variants of S-CO₂ BC have already been studied to make this technology economically more viable and efficient. In comparison to other BC and Rankine cycles, S-CO₂ BC is less complex and more compact, which may reduce the overall plant size, maintenance, and the cost of operation and installation. In this paper, we consider one of the configurations of S-CO₂ BC called the recompression Brayton cycle with partial cooling (RBC-PC) to which some modifications are suggested with an aim to improve the overall cycle’s thermal efficiency. The type of heat source is not considered in this study; thus, any heat source may be considered that is capable of supplying temperature to the S-CO₂ in the range from 500 °C to 850 °C, like solar heaters, or nuclear and gas turbine waste heat. The commercial software Aspen HYSYS V9 (Aspen Technology, Inc., Bedford, MA, USA) is used for simulations. RBC-PC serves as a base cycle in this study; thus, the simulation results for RBC-PC are compared with the already published data in the literature. Energy analysis is done for both layouts and an efficiency comparison is made for a range of turbine operating temperatures (from 500 °C to 850 °C). The heat exchanger effectiveness and its influence on both layouts are also discussed. Full article

(This article belongs to the Special Issue Advances in Supercritical Fluid Extraction)

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14 pages, 296 KiB

Open AccessFeature PaperReview

Some Advances in Supercritical Fluid Extraction for Fuels, Bio-Materials and Purification

by Yizhak Marcus

Processes 2019, 7(3), 156; https://doi.org/10.3390/pr7030156 - 13 Mar 2019

Cited by 15 | Viewed by 6537

Abstract

Supercritical fluids are used for the extraction of desired ingredients from natural materials, but also for the removal of undesired and harmful ingredients. In this paper, the pertinent physical and chemical properties of supercritical water, methanol, ethanol, carbon dioxide, and their mixtures are provided. The methodologies used with supercritical fluid extraction are briefly dealt with. Advances in the application of supercritical extraction to fuels, the gaining of antioxidants and other useful items from biomass, the removal of undesired ingredients or contaminants, and the preparation of nanosized particles of drugs are described. Full article

(This article belongs to the Special Issue Advances in Supercritical Fluid Extraction)

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