Supercritical CO2 extraction optimization of pomegranate (Punica granatum L.) seed oil using response surface methodology

This study examined extraction of pomegranate seed oil by using supercritical carbon dioxide. Response surface methodology was used to evaluate the effects of the process parameters, namely extraction pressure, temperature and CO₂ flow rate on the yield of pomegranate seed oil. The extraction parameters were optimized with a central composite design experiment. The linear term of pressure, followed by the linear term of CO₂ flow rate, the quadratic terms of pressure, temperature and CO₂ flow rate and the interactions between pressure and temperature, as well as CO₂ flow rate and temperature, had significant effects on the oil yield (p < 0.05). Maximum yield of pomegranate seed oil from the mathematical model was predicted to be 156.3 g/kg dry basis under the condition of pressure 37.9 MPa and temperature 47.0 °C with CO₂ flow rate of 21.3 L/h. The fatty acid composition and the tocopherols' content of pomegranate seed oil extracted using supercritical CO₂ were compared with those obtained by Soxhlet method. Minor difference was found in the fatty acid composition of the oils extracted by the two methods. The content of total tocopherols was about 14% higher in the oil extracted with supercritical CO₂ than that obtained by Soxhlet extraction.     

Characteristics of Prunus serotina seed oil

Oils from Prunus serotina raw and toasted seeds extracted with hexane and supercritical CO₂ were evaluated for their physicochemical characteristics. Supercritical CO₂ extracted the least oil (21.3%), with high absorbing carotenoid pigments. P. serotina oil had characteristically high refractive index and density with three typical absorbance peaks in the UVC (100–290 nm) range centred at 260, 270 and 280 nm. The oil was highly polyunsaturated and abundant in oleic (35%), α-elostearic (27%), linoleic (27%), palmitic (4%), stearic (4%) and β-elostearic (1%) acids. P. serotina seed oil exhibited at least three distinct thermal structural transitions between −35 and −13 °C with two reversing transitions between −19 and −12 °C. Thermal oxidation by differential scanning calorimetry (DSC) revealed a three step oxidation of P. serotina seed oil with the mean onset and oxidation temperatures at 121 and 130–273 °C, respectively, depending on processing. Supercritical CO₂ extraction and toasting significantly affected the thermal and oxidation characteristics, fluorescence, and fatty acids of oils.     

Extraction of tocopherol-enriched oils from Kalahari melon and roselle seeds by supercritical fluid extraction (SFE-CO2)

Tocopherol-enriched oil was extracted by supercritical fluid extraction of carbon dioxide (SFE-CO₂) from Kalahari melon and roselle seeds. The SFE-CO₂ process was optimised using response surface methodology (RSM) with central composite design (CCD). Three SFE-CO₂ parameters namely extracting pressure, extracting temperature, and flow rate of carbon dioxide were examined. The optimal SFE-CO₂ conditions were determined and the quadratic response surfaces were drawn from the mathematical models. The optimal SFE-CO₂ conditions for the extraction tocopherol-enriched oil from Kalahari melon seeds were: extracting pressure 290 bar, extracting temperature 58 °C, and flow rate of carbon dioxide 20 ml/min. The optimum conditions for roselle seeds were extracting pressure 200 bar, extracting temperature 80 °C, and flow rate of carbon dioxide 20 ml/min. These optimum conditions yielded tocopherol concentration of 274.74 and 89.75 mg/100 g oil from Kalahari seed and roselle seed, respectively. No significant (P > 0.05) differences were obtained between the experimental and predicted values.     

Application of response surface methodology to optimise supercritical carbon dioxide extraction of essential oil from Cyperus rotundus Linn.

Supercritical fluid extraction with carbon dioxide (SC-CO₂ extraction) was performed to isolate essential oils from the rhizomes of Cyperus rotundus Linn. Effects of temperature, pressure, extraction time, and CO₂ flow rate on the yield of essential oils were investigated by response surface methodology (RSM). The oil yield was represented by a second-order polynomial model using central composite rotatable design (CCRD). The oil yield increased significantly with pressure (p < 0.0001) and CO₂ flow rate (p < 0.01). The maximum oil yield from the response surface equation was predicted to be 1.82% using an extraction temperature of 37.6 °C, pressure of 294.4 bar, extraction time of 119.8 min, and CO₂ flow rate of 20.9 L/h.     

Functional food oil coloured by pigments extracted from microalgae with supercritical CO2

A functional food oil, rich in fatty acids and antioxidants, coloured with pigments (carotenoids) extracted with supercritical CO₂ from the microalga Chlorella vulgaris, was produced, having in view its use in food industry (namely for derived seafood). The supercritical fluid extraction (SFE) was carried out in order to study the effect of several modifiers (oil mixed with the microalga and ethanol with the supercritical CO₂), the degree of crushing of the microalga and the supercritical fluid flow rate, at a pressure of 300 bar and temperature of 40 °C. Moreover, the microalga pigments were also extracted with acetone and with vegetable oil at room and high temperature. The recovery of carotenoids was 100% with oil at room temperature for 17 h, 70% with oil at 100 °C for 30 min, 69% with supercritical CO₂ at 40 °C and 300 bar. In SFE the degree of crushing strongly influenced the extraction recovery and higher pigment recoveries were obtained with well crushed biomass.     

Extraction of canola seed (Brassica napus) oil using compressed propane and supercritical carbon dioxide

This study aimed to investigate the extraction of canola seed (Brassica napus) oil using supercritical carbon dioxide and compressed propane as solvents. The extractions were performed in a laboratory scale unit at temperatures and pressures of 40, 50 and 60 °C and 20, 22.5 and 25 MPa for carbon dioxide and 30, 45 and 60 °C and 8, 10 and 12 MPa for propane extractions, respectively. The results indicated that pressure and temperature were important variables for the CO₂ extraction, while temperature is the most important variable for the extraction yield with propane. The extraction with propane was much faster than that with carbon dioxide. The characteristics of the extracted oil, that is, the oxidative stability determined by DSC and the chemical profile of fatty acids determined by gas chromatography, were similar for the two solvents. The overall extraction curves were well described by the Sovová model.     

Supercritical carbon dioxide extraction of seed oil from Opuntia dillenii Haw. and its antioxidant activity

Supercritical carbon dioxide extraction of seed oil from Opuntia dillenii Haw. and its antioxidant activity were investigated in this study. The effects of main operating parameters including extraction pressure, temperature, time and CO₂ flow rate on the extraction yield of seed oil were studied. The maximum extraction yield of 6.65% was achieved at a pressure of 46.96 MPa, a temperature of 46.51 °C, a time of 2.79 h and a CO₂ flow rate of 10 kg/h. The chemical composition of the seed oil was analysed by GC–MS. The main fatty acids were linolenic acid (66.56%), palmitic acid (19.78%), stearic acid (9.01%) and linoleic acid (2.65%). The antioxidant activity of seed oil was assessed by means of 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical-scavenging assay and β-carotene bleaching test. Both methods demonstrated notable antioxidant activity of seed oil, which is nearly comparable to the references ascorbic acid and butylated hydroxytoluene (BHT). The antioxidant activity of the seed oil was also found to be concentration-dependent.     

Supercritical fluid extraction of oil from potato chips: Two scale comparison and mathematical modeling

Oil was extracted from fried chipped potatoes using supercritical carbon dioxide. The goals of the study were to determine the effect of process parameters on the extraction, explore the scalability of the process, and determine useful kinetic parameters. Extraction conditions range 27.6–41.4 MPa (4000–6000 PSI), 35–80 °C and solvent flow rate of 0.5–5.0 g CO₂/min. Up to 100% of the oil was recovered from the potato chips at the highest pressure and temperature conditions. Two process conditions were chosen for comparison of performance with a larger scale (1:5) system, maintaining the same CO₂ flow rate to feed mass ratio. Good agreement between scales was seen at the higher pressure and temperature settings. Kinetic parameters, calculated using a literature model, indicated that, as expected, the extraction is limited by internal diffusion.     

Extraction of fish oil from the skin of Indian mackerel using supercritical fluids

The total oil was extracted from the ground skin of Indian mackerel (Rastrelliger kanagurta) using various techniques of supercritical fluid extraction (SFE) at 20–35 MPa and 45–75 °C and by the Soxhlet method for comparison. The oil yield increased with pressure and temperature and the highest yields were 24.7, 53.2, 52.8, and 52.3/100 g sample (dry basis) for the continuous, cosolvent, soaking, and pressure swing techniques, respectively, at 35 MPa and 75 °C. The yield from the Soxhlet extraction was 53.6/100 g sample (dry basis). The CO₂ consumption was 581.8, 493.6, 484.9 and 290.9 g for the continuous, cosolvent, soaking and pressure swing techniques, respectively, at 35 MPa and 75 °C. The largest recoveries of PUFA, especially the ω-3 family, were achieved from the soaking and pressure swing techniques at 35 MPa and 75 °C. Thus, the pressure swing and soaking techniques are the most effective at extracting the oil from fish skin.     

Extraction of β-carotenes from palm oil mesocarp using sub-critical R134a

Sub-critical extraction of palm oil from palm mesocarp using R134a solvent was conducted via the dynamic mode to investigate the ability of R134a to extract β-carotene. The yield of palm oil and the solubility of β-carotene were investigated at 40, 60 and 80 °C and pressure range from 45–100 bar. The extracted oil was analysed for β-carotene content using UV–Vis spectrophotometry. The results showed that palm oil yield increased with pressure and temperature. The maximum solubility of β-carotene was obtained at 100 bar and 60 °C while the lowest solubility occurred at 80 bar and 40 °C. The higher concentration of extracted β-carotene ranging from 330–780 ppm as compared to that achieved through conventional palm oil processing indicates that extraction of β-carotene using R134a is viable.     

Effect of various salts and pH condition on rheological properties of Salvia macrosiphon hydrocolloid solutions

The extraction of Salvia macrosiphon seed hydrocolloid was performed successfully and the optimum hydration time and temperature were found to be 30 min and 25 °C for 12% extraction yield. The effect of solution pH (3–9) and addition of NaCl (0.5–3%), CaCl₂ (0.5–3%) and Na₂HPO₄ (0.2–0.6%) on rheological properties of the hydrocolloid solutions were investigated. Rheologcal data were fitted with the Power law model with regression coefficient of greater than 0.95. Strong shear thinning behavior with the n value of less than 0.53 was recorded. All variables had significant impacts on rheological parameters. The minimum and maximum consistencies were found at pH 3 and the 9, respectively. This was explained with the presence of carboxylic groups on the biopolymer backbone as indicated by FTIR. NaCl, CaCl₂ and Na₂HPO₄ had significant effects on rheological properties. Moreover, at similar salt concentration of 0.5%, Na₂HPO₄ had the greatest and NaCl had the lowest effect.     

Breaking the spores of the fungus Ganoderma lucidum by supercritical CO2

The hard sporoderm of Ganoderma lucidum spores prevents the release of bioactive components such as polysaccharides which have significant anti-tumour activity. In the present study, supercritical carbon dioxide (SC–CO₂) was used for the sporoderm breaking of G. lucidum spores, and polysaccharides were subsequently extracted and determined for evaluating the performances of SC–CO₂. The operating parameters were optimized by orthogonal array design (OAD), and the morphological status of sporoderm was observed by scanning electron microscope (SEM). The optimum operating conditions for SC–CO₂ breaking of sporoderm were as follows: pressure 35 MPa, temperature 25 °C, time 4 h, and CO₂ flow rate 10 kg/h. After SC–CO₂ processing, the extraction yield of polysaccharides reached 2.98%, which was 3-fold to that of the intact ones (0.94%). This method is fast, efficient and advanced enough to break the hard sporoderm of G. lucidum, which may provide a scientific reference for the large-scale processing of spores in the pharmaceutical and food industries.     

Supercritical CO2 cell breaking extraction of Lycium barbarum seed oil and determination of its chemical composition by HPLC/APCI/MS and antioxidant activity

The extraction parameters for oil extraction from Lycium barbarum seed including extraction pressure, temperature and time were optimized using an orthogonal test design. The optimum conditions for supercritical CO₂ extraction were as follows: extraction pressure, 30 MPa; extraction temperature, 45 °C; dynamic extraction time, 60 min; CO₂ flow, 25 kg/h. The oil yield under the conditions proposed was 19.28 g/100 g. The effect of cell wall breakage pretreatment was investigated by supercritical CO₂ rapid depressurization, and results indicated this pretreatment could result in a rapid and efficient extraction. A sensitive fluorescent reagent 2-(11H-benzo[a]carbazol-11-yl) ethyl 4-methylbenzenesulfonate (BCETS) was utilized as pre-column labeling regent to determine fatty acids (FA) from Lycium barbarum seed oils obtained by different extraction methods. The main FA were: C18:2, C18:1, C16, C20:6, C18:3, and C20. The oil from L. barbarum seed exhibited excellent antioxidant activity in 2,2-diphenyl-1-picrylhydrazyl（DPPH）radical scavenging assay and β-carotene bleaching test, and its antioxidant activity compared well with the references ascorbic acid and α- tocopherol.     

Extraction and characterisation of lipids from Antarctic krill (Euphausia superba)

There is significant commercial interest in oil extraction from krill because it is rich in omega-3 polyunsaturated fatty acids (n-3 PUFA) such as eicosapentaenoic (EPA, 20:5n3) and docosahexaenoic (DHA, 22:6n3) acids. The objectives were to determine oil extraction efficiency using different solvent systems and the composition of extracted oil and spent krill following extraction. Extraction efficiency was the highest (P < 0.05) for one-step extraction using freeze-dried krill with 1:12 or 1:30 krill:solvent ratio (w:v) compared to Folch, Soxhlet, and conventional two-step extraction. Extracted oils contained predominantly phospholipids (20–33%), polar non-phospholipids (64–77%), and minor triglycerides (1–3%). Triglycerides contained much less (P < 0.05) total n-3 (4.0%), DHA (1.1%), and EPA (2.3%), but more (P < 0.05) saturated FA (38.7%) than phospholipids (total n-3-47.4%, DHA-18.0%, EPA-28.2%, saturated FA-23.5%). Antioxidant capacity of krill oil extracted by one-step extraction (9.4–14.2 μmol Trolox Equivalents/ml oil) was generally similar to antioxidant capacity of krill oil extracted by ethanol (22.9), but greater (P < 0.05) than antioxidant capacity of krill oil extracted by acetone (1.2) and Folch method (1.5). The spent krill following oil extraction contained protein (72.9–75.8%, dry basis). Based on the extraction efficiency and composition of the extracted oil, the one-step extraction using 1:12 krill:solvent ratio is recommended.     

Supercritical carbon dioxide extraction of volatile oil from Italian coriander seeds

Supercritical CO₂ fluid extraction of the volatile oil from Italian coriander seeds was carried out under different conditions of temperature (40 and 50 °C), pressure (90, 100 and 150 bar), mean particle size (0.4, 0.6 and 0.8 mm) and CO₂ flow rate (0.79, 1.10 and 1.56kg/h) in order to evaluate their influence on the yield and composition of the volatile oil. Hydrodistillation with the same mean particle sizes was performed and used as a comparative method. The best supercritical fluid extraction conditions were found to be 90 bar, 40 °C, 1.10 kg/h and 0.6 mm. The chemical composition of each supercritical fluid extraction sample was analysed by GC and GC–MS and the global composition was compared with that obtained by hydrodistillation. The dominant components were linalool (65–79%), γ-terpinene (4–7%), camphor (3%), geranyl acetate (2–4%), α-pinene (1–3%), geraniol (1–3%) and limonene (1–2%). Moreover, supercritical fluid extraction samples were collected at specific intervals of amount of CO₂ consumed, during each extraction, and the contribution of the main volatile components from each sample, for the global volatile compositions, was evaluated. In general, the first sample of each extraction contained up to 50% of the mass of each component.     

Characteristics of flaxseed hull oil

Oils from two commercial flaxseed hulls extracted by six procedures were evaluated for physicochemical characteristics. Oil yield ranged from 9% to 28% depending on solvent and extraction. Lipid fractionation of crude flaxseed hull oil yielded 92.5% neutral lipids, 3.1% phospholipids, 2.4% acidic lipids and 2.1% free fatty acids. Flaxseed hull oil exhibited three thermal transitions between −35 and −13 °C with solvent dependent polymorphism. Thermal oxidation by differential scanning calorimetry (DSC) revealed three step oxidation of flaxseed hull oil with mean onset and oxidation temperatures at 121 and 150–253 °C, respectively depending on the extraction procedure. Flaxseed hull oil exhibited two-fold difference (0.6–1.2 μm Trolox equivalent/g) in antioxidant activity measured by a photochemiluminescence (PCL) assay. Supercritical CO₂ extracted the most oil with the highest antioxidant capacity of all evaluated procedures resulting in a defatted flaxseed hull containing the highest (53 mg/g) secoisolariciresinol diglucoside (SDG) level.     

Supercritical fluid extraction of daidzein and genistein isoflavones from soybean hypocotyl after hydrolysis with endogenous β-glucosidases

An optimal condition of supercritical fluid extraction (SFE) for isoflavone aglycones (daidzein and genistein) in soybean hypocotyls previously subjected to thermohydration at pH 5.0 and a temperature of 50 °C for 6, 12 and 18 h was developed. Different temperatures, pressures and cosolvents (methanol, ethanol, and acetonitrile) was tested and compared with solid–liquid extraction using aqueous methanol solution (80% v v⁻¹) conducted in parallel for comparison. The extraction conditions were 50–70 °C, 176–380 bar, adding 0, 5, 10 mol% of cosolvents 80% in water as a modifier. The results from SC–CO₂ showed that the cosolvent and pressure have significant effects in the extraction efficiency. It was found that the extraction conditions promoting the highest extraction of daidzein and genistein were at the temperature of 60 °C, pressure of 380 bar and both static and dynamic extraction of 15 min with the addition of 10% acetonitrile (80% v v⁻¹). The maximum amounts of daidzein and genistein extracted by each method were solid–liquid extraction (70.07 mg 100 g⁻¹) and carbon dioxide–acetonitrile (17.97 mg 100 g⁻¹). The yield of daidzein and genistein achieved by a 30 min SC–CO₂ extraction on soybean hypocotyls after 12 h soaking time was markedly improved by the addition of a modifier (acetonitrile) to the CO₂ fluid. HPLC analysis of the obtained extracts revealed that extraction of isoflavone aglycones by SC–CO₂ was 4.78 and 13.19 mg 100 g⁻¹ for daidzein and genistein, respectively. The contents of daidzein and genistein obtained in the solid–liquid extraction were superior to 86% and 63%, respectively, compared to supercritical extraction.     

Analysis of ginsenosides in Panax ginseng in high pressure microwave-assisted extraction

High pressure microwave assisted extraction (HPMAE) was applied to extract the ginsenosides from Panax ginseng root. The influences of extraction solvent, extraction pressure and extraction time were individually investigated. HPMAE has been compared with other extraction methods, including Soxhlet extraction, ultrasound-assisted extraction and heat reflux extraction. The determination of ginsenosides was performed by HPLC–ESI-MS. The results indicated that the HPMAE not only took a shorter time but also afforded higher extraction yields of ginsenosides, especially ginsenoside Rb₁, Rc, Rb₂ and Rd. Furthermore, the neutral ginsenosides and malonyl ginsenosides in Panax ginseng root extracts by HPMAE were investigated. The malonyl ginsenoside m-Rb₁, m-Rc, m-Rb₂ and m-Rd degraded in HPMAE at 400 kPa (109–112 °C) in 70% (v/v) ethanol–water and at 600 kPa (112–115 °C) in methanol, and transformed into corresponding neutral ginsenoside Rb₁, Rc, Rb₂ and Rd. Using water as extraction solution, the neutral ginsenosides degraded under HPMAE at 400 kPa (135–140 °C), and transformed into less polarity rare ginsenosides.     

Optimization of supercritical carbon dioxide extraction of sea buckthorn (Hippophaë thamnoides L.) oil using response surface methodology

Response surface methodology (RSM) was employed to optimize the conditions of supercritical CO₂ extraction of the whole berry oil from sea buckthorn. The effects of pressure, temperature, CO₂ flow rate and extraction time on the yield of oil, vitamin E and carotenoids were investigated. Results showed that the data were adequately fitted into three second-order polynomial models. The independent variables, the quadratics of pressure and extraction time, the interactions between pressure and temperature, pressure and extraction time, temperature and extraction time, as well as flow rate and extraction time had a significant effect on the yield of the oil, vitamin E or carotenoids. It was predicted that the optimum extraction conditions within the experimental ranges would be the extraction pressure of 27.6 MPa and temperature of 34.5 °C with flow rate of 17.0 L/h and extraction time of 82.0 min. Under such parameters, the yields of oil, vitamin E and carotenoids were predicted to be 208.0 g/kg, 288.7 mg/kg and 620.0 mg/kg dry sea buckthorn berry, respectively. Monounsaturated fatty acids were predominant in the whole berry oil, accounting for over 62% of the total fatty acids.     

Determination of lutein and zeaxanthin and antioxidant capacity of supercritical carbon dioxide extract from daylily (Hemerocallis disticha)

Lutein and zeaxanthin were extracted from daylily (Hemerocallis disticha) flowers using supercritical fluid extraction-carbon dioxide (SFE-CO₂) at a temperature range of 50–95 °C and pressure range of 300–600 bar. The extracts were analysed by HPLC with a C30 column and an isocratic solvent system: methanol/methyl-tert-butyl ether = 86/14 (v/v). Moreover, the antioxidant capacities of the extracts were evaluated by a 2,2-diphenyl-2-picrylhydrazyl radical scavenging assay and a chemiluminescence assay to measure the scavenging activity of hydrogen peroxide, superoxide anion and hydroxyl radical. The optimal lutein and zeaxanthin extraction could be achieved at 80 °C and 600 bar, and the extraction pressure was the most important parameter for SFE-CO₂. In addition, the extracts had significantly higher antioxidant activities in all antioxidant assays.