Supercritical Carbon Dioxide Extraction Research Articles

1H NMR and chemical analysis to characterize camellia oil obtained by different extraction methods: A comparative study using chemometrics

Camellia oil has become one of the most popular edible vegetable oils especially in China. It can be obtained by cold-pressing (CPE), soxhlet extraction (SE), aqueous enzymatic extraction (AEE), and supercritical carbon dioxide extraction (SC-CO2), while research on their efficient identification is limited. Thus, in this study, proton nuclear magnetic resonance (1H NMR) and conventional chemical analysis, respectively coupled to chemometrics, were employed to compare the camellia oils, produced by CPE, SE, AEE, and SC-CO2. The results showed an obviously overlapping among those four different extracted camellia oils, in both principal component analysis (PCA) and hierarchical clustering analysis (HCA), when using fatty acids as input variables. While two obtained PCA models showed good discrimination, according to the minor component compositions (α-tocopherol, squalene, stigmasterol, β-sitosterol, β-amyrin and lanosterol) and 1H NMR spectra, respectively. Additionally, by means of variable importance for the projection (VIP) scores, less 10 dominant 1H NMR spectra signals were screened out as detailed markers for different camellia oils classification. Therefore, 1H NMR combined with chemometrics may be applied as an efficient technique to classify different extracted camellia oils and potentially other vegetable oils.

Antibacterial activity of Savory (Satureja hortensis) extract against pure culture strains of

The paper presents the results of a study of the antibacterial activity of supercritical carbon dioxide extract of the aboveground part of Savory (Satureja hortensis) against Escherichia coli, Salmonella spp. and Staphylococcus aureus bacteria.To study the antibacterial properties of Savory extract (Satureja hortensis) against infections caused by Staphylococcus aureus, Escherichia coli and Salmonella spp.In the course of the experiment, Savory extract obtained by supercritical carbon dioxide extraction was studied for antimicrobial activity against these bacteria. The component composition of the extract was determined by chromatography–mass spectrometry. To determine the antibacterial activity, we used the method of dilution in a liquid medium with subsequent measurement of the growth of the suspension culture biomass. The activity of the extract was compared with certified drugs included in the protocols for the treatment of bacterial infections. DMSO and potassium phosphate buffer were used as a negative control.The studies showed that the extract exhibits high antibacterial activity against all the studied bacterial strains and has a direct positive correlation with its concentration. Chromatographic mass‐spectrometry analysis showed that the extract of garden Savory contains 28 substances, the main ones being thymol (30.51 %), gamma‐terpinene (15.27 %), para‐ cymene (14.25 %) and Carvacrol (9.18 %), which both individually and in combination could exhibit antibacterial activity.Supercritical carbon dioxide extract exhibits pronounced antimicrobial activity against reference strains of S. aureus, Escherichia coli and Salmonella spp.

Revealing the Potential of Star Anise Essential Oil: Comparative Analysis and Optimization of Innovative Extraction Methods for Enhanced Yield, Aroma Characteristics, Chemical Composition, and Biological Activities

ABSTRACTStar anise has been used for a long time in improving human health and curing diseases, owing to its unlimited components with complex chemical structures and a wide range of bioactivities. This study is aimed to investigate the influence of extraction methods (steam distillation, ethanol Soxhlet extraction, supercritical carbon dioxide extraction, subcritical n‐butane extraction) on the yield, aroma properties, chemical composition, and bioactivity of star anise essential oils. Electronic nose detection revealed the essential oils from subcritical extraction exhibited the most intense aroma, while the essential oils from ethanol Soxhlet extraction had a more complex aroma profile. Fourier‐transform infrared analysis showed the presence of benzene rings, carbonyl groups, C=C, and aromatic ether bonds in the essential oils extracted through different methods. The major components were heterocyclic olefins, heterocyclic oxygenates, and aromatic oxygenates, as well as certain amounts of flavonoids and polyphenols. Correlation analysis revealed the relative contents of volatile trans‐anethole, wormwood, d‐limonene, cineole, and trans‐α‐citronelene were strongly associated with the antibacterial activity of the essential oils. Similarly, the contents of volatile components (d‐limonene, cineole) and non‐volatile components (total flavonoids and total polyphenols) were strongly correlated with the DPPH scavenging activity of the essential oils. These results confirm the effectiveness of the ethanol Soxhlet extraction method in retaining the bioactivity of the essential oils. Finally, with a Box–Behnken central composite design of response surface and single‐factor experiments, the optimal extraction conditions for the ethanol Soxhlet method were determined: ultrasonic frequency of 80 kHz, crushing particle size of 60 meshes, liquid–material ratio of 8:1 (mL:g), and ultrasonic time of 35 min. Under these conditions, the essential oil yield was 25.51% ± 0.21%. Overall, these findings highlight the significance of extraction methods in obtaining high‐quality star anise essential oils with desirable aroma properties and potent bioactivities.

Supercritical CO2 as a green technology for carotenoids-rich virgin palm oil production: Process optimization, kinetics and thermodynamics modeling

The experimental conditions of supercritical carbon dioxide (scCO2) extraction of virgin palm oil (VPO) from oil palm mesocarp fiber (OPMF) were optimized using the Response Surface Methodology (RSM). Results showed that a maximum of 28.68% of VPO extraction was obtained at the optimal experimental conditions of scCO2 extraction: pressure of 31MPa, temperature of 340K, and extraction time of 80min. The second-order rate equation, Arrhenius equation and Eyring theory were employed to assess the kinetics behaviour, activation energy and thermodynamics behaviour of scCO2 extraction of VPO from oil palm mesocarp fiber. The lower activation energy value (12.17kJ/mol) of scCO2 for the extraction of VPO from OPMF indicates that the scCO2 extraction technology is less dependent on temperature during the extraction of VPO from OPMF. The physicochemical properties and fatty acids compositions analyses reveal that the scCO2 extracted VPO contains high carotenoids content (982μg/g), low free fatty acids content (0.31wt.%), higher oxidative stability and higher unsaturated fatty acids content.

Preparation of decellularized bone graft material with supercritical carbon dioxide extraction technique.

To evaluate the immunogenicity and osteogenic ability of animal-derived bone graft material decellularized with supercritical carbon dioxide. Porcine femurs were randomly divided into two groups after preliminary treatment, and decellularized with conventional method (conventional control group) or supercritical carbon dioxide (experimental group). Clearance rate of galactose-α-1, 3-galactose (α-Gal) and residual DNA of the two groups were analyzed to assess the immunogenicity of the xenogenic materials. Clearance rate of α-Gal was determined by enzyme-linked immunosorbent assay and residual DNA was detected by fluorescence method. Nine SPF-grade male athymic nude mice of 6 weeks old were randomly divided into experimental group, conventional control group and positive control group. Samples were implanted over biceps femoris muscle of athymic nude mice, the explants were collected 4 weeks post implantation, hematoxylin and eosin (HE) staining and immunohistochemistry were applied to determine the osteogenic ability and bone tissue-associated protein expressions of the implants. The clearance rates of α-Gal antigen in the experimental group and the conventional control group were (99.09±0.26)% and (30.18±2.02)%, respectively (t=58.67, P<0.01). The residual DNA of the experimental group, the conventional control group and the positive control group were (13.49±0.07) ng/mg, (15.20±0.21) ng/mg and (14.70±0.17) ng/mg, the residual DNA in the experimental group was significantly lower than that in the conventional control group (t=－13.41, P<0.01) and the positive control group (t=－11.30, P<0.01). HE staining showed that multiple bone formation centers with active osteogenesis and rich bone marrow were observed in experimental group 4 weeks after implantation, only a small number of bone formation centers were observed in the conventional control group and the positive control group, with no obvious osteoblasts present. Immunohistochemistry results indicated that the expressions of alkaline phosphatase, Runt-related transcription factor 2, typeⅠcollagen and osteocalcin in the experimental group showed an increasing trend compared with those in the conventional control group and the positive control group. Compared with clinically used demineralized bone matrix and bone graft material decellularized with conventional method, bone graft material decellularized with supercritical carbon dioxide exhibits lower immunogenicity and better osteogenic ability.

VOC removal from automotive waste by supercritical CO2 extraction

This study investigated the reduction of volatile organic compounds (VOCs) from waste polypropylene (PP) from automobile bumpers by supercritical carbon dioxide (scCO2) extraction. The scCO2 extraction was performed with varying temperatures, pressures, and times in the range of 313–353 K, 10–25 MPa, and 1–6 h, respectively. At 333 K, 25 MPa, and 6 h, highly efficient removal of xylene, styrene, and total VOCs were observed, with removal percentages of >98 %. Optimal condition for VOC removal using scCO2 based on response surface methodology was determined to be 313 K, 10 MPa, and 2.17 h. No differences in size and color were observed in the scCO2-treated PP pellets. Moreover, VOC removal using scCO2 did not induce noticeable changes in the chemical and thermal properties of the treated PP samples. This result demonstrated that scCO2 extraction is a promising method for the VOC removal from automobile plastic waste.

Response surface optimization for supercritical carbon dioxide extraction of Korarima (Aframomum corrorima) seed oil and its antibacterial activity evaluation

Oils extracted from natural plants are valuable resources because of their diverse biocidal activity against microorganisms. This paper reports, for the first time, supercritical CO2 extraction of oil from Korarima (Aframomum corrorima) seeds and its antibacterial activity evaluation. The influences of pressure, temperature, and extraction time on the yield of supercritical CO2-extracted oil (scCO2-extracted oil) were optimized using the Response Surface Methodology. Under the optimal extraction conditions of 46 °C, 15.5 MPa, and 147 min, the extraction yield reached 1.60±0.04 %, consistent with the theoretical value of 1.58 %. The compositions of the scCO2-extracted oil were identified by GC-MS, primarily consisting of nerolidol (33.97–41.20 %), geraniol (23.08–24.50 %), and α-terpinene (8.90–9.06 %). The oil exhibited significant antibacterial activity against Staphylococcus. aureus with a minimum inhibitory concentration of 1 mg·mL−1. This study highlights the potential applications of supercritical CO2 extraction technology for extracting Korarima seed oil and its use as an antibacterial ingredient in cosmetics and pharmaceuticals.

Evaluating Supercritical Carbon Dioxide Extraction vs. Conventional Aqueous Extraction of Natural Dyes from Hypericum triquetrifolium for Textile Fibers Dyeing

Evaluating Supercritical Carbon Dioxide Extraction vs. Conventional Aqueous Extraction of Natural Dyes from Hypericum triquetrifolium for Textile Fibers Dyeing

Advances and challenges in the fractionation of edible oils and fats through supercritical fluid processing.

Petrochemical solvents are widely used for the extraction and fractionation of biomolecules from edible oils and fats at an industrial scale. However, owing to its safety concerns, toxicity, price fluctuations, and sustainability, alternative solvents and technologies have been actively explored in recent years. Technologies, such as ultrasound and microwave-assisted extraction, supercritical carbon dioxide extraction, supercritical fluid fractionation, and sub-critical water extraction, and solvents, like ionic liquids and deep eutectic solvents, are reported for extraction and fractionation of biomolecules. Among them, supercritical carbon dioxide extraction and fractionation are some of the most promising green technologies with the potential to replace petrochemical-based conventional techniques. The addition of cosolvents, such as water, ethanol, and acetone, improves the extraction of amphiphilic and polar compounds from edible oils and fats. Supercritical fluid processing has diverse applications, including concentration of solutes, selective separation of desired molecules, and separation of undesirable compounds from the feed material. Temperature, pressure, particle size, porosity, flow rate, solvent-to-feed ratio, density, viscosity, diffusivity, solubility, partition coefficient, and separation factor are the fundamental factors governing the extraction and fractionation of desired biomolecules from lipids. Supercritical fluids stand alone compared to conventional fluids, because of their tunable solvent properties. Overall, it is to be noted that supercritical fluid-based methods have lots of scope to replace conventional solvent-based methods and progress toward the creation of sustainable food-processing techniques. This review critically evaluates the parameters responsible for the extraction and fractionation of biomolecules from edible oils and fats under supercritical conditions.

Supercritical carbon dioxide extracts of Schinus terebinthifolia fruits and their utilization against microbial illness, lipase, and butyrylcholinesterase activities in vitro

Supercritical carbon dioxide extracts of Schinus terebinthifolia fruits and their utilization against microbial illness, lipase, and butyrylcholinesterase activities in vitro

Green extraction of marine phospholipids from Conger eel by-product using SC-CO2: Lipidomic profiles and biological activities

This paper presents an eco-friendly approach to recovering phospholipids (PLs) from the Conger myriaster head (CMH) via supercritical carbon dioxide (SC–CO2) extraction using ethanol as a cosolvent. The lipidomic profile and biological activities of the extracted PLs were investigated. Purity assessments, PL composition analysis, and fatty acid profiling were performed to characterize the PLs. Biological activity was determined through antioxidant, antimicrobial, antihypertensive, anti-inflammatory, and anticancer evaluations. The results showed that the yields of the SC–CO2 extracted CMH PLs (SCHP) and organic solvent extracted CMH PLs (OCHP) were 3.26% ± 0.20 % (76.18% ± 0.09% purity) and 9.02% ± 0.21% (purity = 18.29% ± 0.04%), respectively. The 31P NMR analysis revealed a diverse PL composition in both extracts, with the SCHP showing higher PC content and selective extraction characteristics. The SCHP exhibited significantly superior antioxidant, antimicrobial, antihypertensive, and anti-dementia activities compared to the OCHP. Both extracts inhibited nitric oxide production in RAW 264.7 cells, suggesting anti-inflammatory activity. Selective anticancer activity was observed, with high toxicity in SK-N-SH cells but no cytotoxicity in RAW 264.7 and HaCaT cells. The findings highlight the potential of SC-CO2 extraction using ethanol to obtain bioactive PLs from marine by-products, with promising applications in the pharmaceutical, cosmetic, and food industries.

Application of green SC-CO2 oil extraction method with a new green catalyst from luffa fruit for biodiesel production from Persian Lilac-Melia Azedarach fruits

Considering the importance of finding new suitable and environmentally friend resources and methods for biodiesel production, the present work has investigated Supercritical Carbon dioxide (SC-CO2) extraction as a new highly efficient and green oil extraction method for oil production from Persian Lilac-Melia Azedarach (PLMA) fruits and its conversion into biodiesel using a new green catalyst. The effects of pressure (22–30 MPa), temperature (40–80 °C) and extraction time (0–240 min) on supercritical carbon dioxide extraction were investigated and the results were compared with ultrasonic probe and Soxhlet extraction methods. The findings indicated that the total oil production rose with higher pressure and temperature, but a decrease was noticed at elevated temperatures. The most effective parameters for extracting PLMA oil were determined to be a pressure of 30 MPa, a temperature of 40 °C, and an extraction time of 180 min. The oil yield obtained by SC-CO2 extraction method was 32 % while it was 30 % and 28 % for Ultrasonic probe and Soxhlet extraction methods, respectively. Finally, a new green catalyst was synthesized from sponge of luffa plant to convert the extracted oil into a green biodiesel. In the future outlook, the efficient oil extraction method including modified SC-CO2 will be proposed for oil extraction from Melia azedarach fruits and the using of the modified catalyst for converting the oil to biodiesel.

Recovery of Fennel Non-Polar Bioactives via Supercritical Carbon Dioxide Extraction

Recovery of Fennel Non-Polar Bioactives via Supercritical Carbon Dioxide Extraction

Extraction of Omega-3 Fatty Acids from Atlantic Sea Cucumber (Cucumaria frondosa) Viscera Using Supercritical Carbon Dioxide.

This study explores the potential of Cucumaria frondosa (C. frondosa) viscera as a natural source of omega-3 FAs using supercritical carbon dioxide (scCO2) extraction. The extraction conditions were optimized using a response surface design, and the optimal parameters were identified as 75 °C and 45 MPa, with a 20 min static and a 30 min dynamic extraction, and a 2:1 ethanol to feedstock mass ratio. Under these conditions, the scCO2 extraction yielded higher FAs than the solvent-based Bligh and Dyer method. The comparative analysis demonstrated that scCO2 extraction (16.30 g of FAs/100 g of dried samples) yielded more fatty acids than the conventional Bligh and Dyer method (9.02 g, or 13.59 g of FAs/100 g of dried samples with ultrasonic assistance), indicating that scCO2 extraction is a viable, green alternative to traditional solvent-based techniques for recovering fatty acids. The pre-treatment effects, including drying methods and ethanol-soaking, were investigated. Freeze-drying significantly enhanced FA yields to almost 100% recovery, while ethanol-soaked viscera tripled the FA yields compared to fresh samples, achieving similar EPA and DHA levels to hot-air-dried samples. These findings highlight the potential of sea cucumber viscera as an efficient source of omega-3 FA extraction and offer an alternative to traditional extraction procedures.

Correction to “Reduction of lauric acid in coconut copra by supercritical carbon dioxide extraction: Process optimization and design of functional cookies using the lauric acid‐lean copra meal”

Correction to “Reduction of lauric acid in coconut copra by supercritical carbon dioxide extraction: Process optimization and design of functional cookies using the lauric acid‐lean copra meal”

Prevention of supercritical carbon dioxide fluid extract from Chrysanthemum indicum Linnén on cutaneous squamous cell carcinomas progression following UV irradiation in mice.

Chrysanthemum indicum Linnén (C. indicum), a medicinal and food herb with various bioactive components, may be of beneficial use in cosmetics and the treatment of skin-related diseases. However, to date, few studies have been reported on its potential preventive and therapeutic effects on skin cancer. Therefore, the present study aimed to investigate the effect and potential mechanism of action of supercritical carbon dioxide extract from C. indicum (CISCFE) on UV-induced skin cancer in a mouse model. Kunming mice were allocated randomly to five treatment groups: Sham, model, low concentration CISCFE, high concentration CISCFE and positive control nicotinamide groups. The dorsal skin of mice was irradiated with UV light for 31 weeks. Histopathological changes, ELISA assays, immunohistochemical analysis and western blotting were performed to investigate the potential therapeutic effects of CISCFE. The results showed that CISCFE alleviated skin oxidative and inflammatory damage in a UV-induced mouse model of skin cancer. Moreover, CISCFE suppressed abnormal activation of proto-oncogene c-Myc and the overexpression of Ki-67 and VEGF, and increased expression of the anti-oncogene PTEN, thereby reducing abnormal proliferation of the epidermis and blood vessels. Additionally, CISCFE increased the protein expression levels of NAD-dependent protein deacetylase sirtuin-1 (SIRT1), Kelch-like ECH associated protein 1 (Keap1) and inhibited the expression of nuclear factor 2 erythroid 2-related factor 2 (Nrf2), phosphorylated (p)-p62 (Ser 349), p-p65 and acetyl-p65 proteins in a UV-induced skin cancer mouse model. In summary, CISCFE exhibited potent anti-skin cancer activity, which may be attributed its potential effects on the p62/Keap1-Nrf2 and SIRT1/NF-κB pathways.

Diffusion coefficients of polycyclic aromatic hydrocarbons in supercritical carbon dioxide: A molecular dynamics simulation study

Supercritical carbon dioxide (SC-CO2) extraction technology is an effective way to deal with soil contamination problems. Among them, polycyclic aromatic hydrocarbons (PAHs) are one of the main pollutants in soil. Studying the diffusion coefficients of PAHs in SC-CO2 can help us better understand the mass transfer characteristics during the SC-CO2 extraction process. Molecular dynamics simulation was applied in this work to study the diffusion behavior of PAHs in the SC-CO2 environment. Under different SC-CO2 thermodynamic states (temperature: 313–373 K, pressure: 10–30 MPa) and molecule sizes, the diffusion coefficients of PAHs were calculated. The trend of the interaction energy between PAHs and SC-CO2 molecules as temperature, pressure, and molecule size changed was also investigated. The findings demonstrated that compared to heavy PAHs, light PAHs had a higher diffusion coefficient in SC-CO2. Changes in the system’s temperature and pressure have an important effect on the diffusion coefficients of PAHs in SC-CO2. The high-temperature and low-pressure conditions had a promoting effect on the diffusion behavior of PAHs molecules. The van der Waals energy accounts for the largest proportion of the intermolecular interaction energy, which was about 80 %. It can be concluded that the van der Waals interaction energy played an important impact on the diffusion process of PAHs molecules in SC-CO2.

Evaluation of the Anti-MRSA Activity of Supercritical Carbon Dioxide and Macerated Crude Extracts of Padina spp. Collected from the Coastal Waters of Tacloban City, the Philippines

The World Health Organization classifies methicillin-resistant Staphylococcus aureus (MRSA) as a high priority in the pathogens list for research and development of new antibiotics. Natural compounds from brown algae are being studied for their potential as alternative sources of antibiotics, including Padina spp. This study aims to evaluate the anti-MRSA activity of the crude extracts obtained through supercritical carbon dioxide extraction (SCCO2) and maceration (MAC) of Padina spp. seaweeds from the coastal waters of Tacloban City, the Philippines. The evaluation of extracts for their anti-MRSA and anti-MSSA (methicillin-susceptible Staphylococcus aureus) activities was done via the resazurin microplate assay, and the Mann-Whitney U test was used to compare these activities. Results show that MAC exhibited minimum inhibitory concentrations (MIC) of 2,048–4,096 μg/mL and 512–4,096 μg/mL for SCCO2 for the MRSA and MSSA control and clinical isolates, respectively. While the MICs for the SCCO2 extracts were lower than those for the MAC extracts, no significant difference was found between the MICs of the extracts from the two extraction methods. No significant difference was observed between the MICs of the extracts against the MRSA (43300) and MSSA (25923) ATCC strains and clinical isolates. Finally, significant differences were observed between the MICs of the control antibiotics and both extraction methods.

Effects of temperature and pressure on volatile compounds of black cumin seeds (Nigella sativa L.) oil extracted by supercritical carbon dioxide

AbstractThis study investigated the effects of temperature and pressure on the yield and volatile compound contents of black cumin seed oil (BCO) extracted from black cumin seeds using supercritical carbon dioxide (SCCO2). The solubility of BCO in SCCO2 increased 2.5‐fold as the pressure increased by 10 MPa. Major volatile compounds in BCO were identified using a static headspace gas chromatography–mass spectrometry (SH–GC–MS). Evidence indicated the main volatile components in SCCO2‐extracted BCO to be hexanal, p‐cymene, and thymoquinone. BCO extracted from China‐cultivated black cumin seed contained similar amounts of p‐cymene and thymoquinone. This black cumin seed is classified as the cymene/thymoquinone chemotype and is also found in Indian, Iranian, and Algerian black cumin seeds. Thymoquinone contents in BCO were more sensitive to the extraction temperature than hexanal and p‐cymene contents. The maximum oil yield of 36.28 ± 1.38 wt%, with approximately 2.0 mg of thymoquinone per milliliter of oil, was obtained at extraction temperatures of 50°C and pressures of 30 MPa. A SH–GC–MS could detect small molecules in black cumin seed oil such as hexanal. The results of this work reveal that temperature has more impact on the selectivity of volatile compounds than pressure in supercritical carbon dioxide extraction.

Optimization of Antifungal Properties of Hop Cone Carbon Dioxide Extracts Based on Response Surface Methodology.

Response surface methodology (RSM) was employed to optimize the process parameters of the supercritical carbon dioxide extraction of hop cones in terms of their antifungal properties against Fusarium culmorum and Aspergillus niger. The effects of temperature (40-50 °C), pressure (200-300 bar), and CO2 consumption (25-75 kgCO2/kg) on the extraction yield, content of α- and β-acids, as well as pathogens' growth inhibition were investigated. Both pressure and CO2 consumption had a significant effect on antifungal properties. It was observed that the best results for antifungal properties were obtained when hop cones were extracted with pure carbon dioxide at the temperature of 50 °C, under the pressure of 300 bar with CO2 consumption at the level of 75 kgCO2/kg of feed for extraction. The highest antifungal properties of hop cone supercritical carbon dioxide extracts were analyzed as 100% for Fusarium culmorum and 68% for Aspergillus niger, calculated as the growth inhibition of tested pathogens. The aim of the study was to determine the optimum values of extraction parameters to achieve the maximum response and enable us to investigate the interaction of these parameters on the antifungal properties of hop cone extracts.