Effects of supercritical CO2 fluid parameters on chemical composition and yield of carotenoids extracted from pumpkin

Pumpkin is a traditional food that is grown extensively worldwide and is believed to be beneficial to human health due to its high contents of carotenoids. The carotenoids in pumpkin were extracted by organic solvents and by supercritical carbon dioxide (SC-CO₂), and then they were identified, quantified, and compared. β-carotene (31 to 40 g per 100 g of total carotenoids) was the predominate carotenoid in pumpkin. Lutein and lycopene contents were much higher in SC-CO₂ extracts than those in organic solvent extract. Cis-β-carotene increased by more than two times in the SC-CO₂ extracts, even at a relatively low temperature of 40 °C, over those in the solvent extracts, indicating both enhanced solubility and isomerization from trans- to cis-β-carotene. The influences of modifier (10 mL/100 mL), temperature (40-70 °C), and pressure (25-35 MPa) of SC-CO₂ extraction on the change of carotenoid yields were also investigated. The highest yield (109.6 μg/g) was obtained at 70 °C and 35 MPa, with a 73.7% recovery. Selective extraction could be achieved by adjusting the temperature and pressure. Higher proportions of all-trans-β-carotene extracts were achieved at 40 °C under both 25 MPa and 35 MPa conditions. In order to extract more cis-isomers, a higher temperature of 70 °C was preferred.     

Extraction of lignans, proteins and carbohydrates from flaxseed meal with pressurized low polarity water

This study examined the application of pressurized low polarity water (PLPW) extraction of lignans, proteins and carbohydrates from defatted flaxseed meal. Key processing conditions included temperature (130, 160, 190 °C), solvent pH (4, 6.5 and 9), solvent to solid ratio (90, 150 and 210 mL/g) and introduction of co-packing material (0 and 3 g glass beads). The addition of 3 g glass beads increased the yields for all target compounds. The maximum yield of lignans (21 mg/g meal) was obtained at 170 °C with solvent to solid ratio of 100 mL/g meal at pH 9. Optimal conditions for protein extraction were pH 9, solvent to solid ratio of 210 mL/g meal and 160 °C. Total carbohydrates recovery was maximized at 215 mg/g meal (50% recovery) at pH 4 and 150 °C with solvent to solid ratio of 210 mL/g meal. The increase of temperature accelerated extraction, thus reducing solvent volume and time to reach equilibrium. For the extraction of proteins and carbohydrates, however, a temperature of 130-160 °C is recommended, as proteins and carbohydrates are vulnerable to thermal degradation.     

Effects of supercritical fluid extraction parameters on lycopene yield and antioxidant activity

The effects of various parameters of supercritical carbon dioxide (SC-CO₂) fluid extractions of tomato skins on the extraction yields and antioxidant activities of lycopene-rich extracts were investigated. A Box–Behnken design was applied to study the effects of three independent variables (temperature ranging from 40 to 100 °C, pressure ranging from 20 to 40 MPa, and flow rate ranging from 1.0 to 2.0 mL/min) on lycopene yield. The model showed good agreement with the experimental results, by the coefficient of determination (r² = 0.9834). Temperature, pressure, and the quadratic term for the temperature of SC-CO₂ extraction were large significantly positive factors affecting lycopene yield (P < 0.05). The maximum total lycopene content of 31.25 μg/g of raw tomato was extracted at the highest temperature of 100 °C, 40 MPa and 1.5 mL/min. TEAC assay was applied to assess the antioxidant activity of lycopene-rich extracts from SC-CO₂ fluid extraction. The effects of SC-CO₂ fluid extraction parameters on the antioxidant activities of the extracts differed with the yield. For each unit of lycopene extract, the antioxidant activity level was constant below 70 °C, but then gradually decreased above 70 °C due to isomerization occurring as a result of the higher temperature. The ratio of all-trans-lycopene to the cis-isomers changed from 1.70 to 1.32 when the operating temperature was adjusted from 40 to 100 °C, indicating an increased bioavailability due to the generation of the cis-isomers. No significant effects of pressure or flow rate of SC-CO₂ fluid extraction on the antioxidant activity were observed.     

Optimization of SC-CO2 extraction of oil from almond pretreated with autoclaving

Supercritical carbon dioxide (SC-CO₂) extraction parameters affecting oil recovery from almond were optimized through response surface methodology (RSM). The optimum extraction conditions were as follows: extraction pressure, 44.1 MPa; extraction temperature, 43.8 °C; dynamic extraction time, 93.6 min; and CO₂ flow rate, 10.1 mL/min. Under these conditions, a mean value of 86.54 ± 0.66 g/100 g (n = 3) was observed, which is well matched with the predicted value of 87.32 g/100 g. Furthermore, the effects of autoclaving pretreatment for the almond particles on the oil recovery, fatty acids' composition, and almond particles' microstructure were also investigated by calculating the percentages of the oil yield, gas chromatograph fitted with a mass spectrometer (GC-MS), and scanning electron microscopy (SEM) analysis, respectively. The results showed that autoclaving pretreatment had minor modifications of the fatty acids' profile of the extracted oil, but greatly promoted the disturbing of almond cell walls, and increased the oil recovery by 6.44%.     

Optimisation of aqueous extraction of gum from durian (Durio zibethinus) seed: A potential, low cost source of hydrocolloid

The main goal of the present study was to investigate the effect of aqueous extraction conditions on the extraction yield and physicochemical properties of the durian seed gum. The studied aqueous extraction variables were water/seed (W/S) ratio (20:1-60:1, w/w), temperature (25.0-85.0 °C), and pH (4.0-10.0). The results indicated that the aqueous extraction variables exhibited the least significant (p < 0.05) effect on oil-holding capacity (OHC). Conversely, they had the most significant (p < 0.05) effect on the span and extraction yield. The current study revealed that the interaction effect of aqueous extraction variables showed the least significant (p < 0.05) effect on the solubility and OHC of durian seed gum. The optimum extraction condition led to the production of durian seed gum with a relatively high extraction yield (56.4%), solubility (27.9%), volume-weighted mean (98.7 μm), span (3.8), water-holding capacity (WHC) (270.6 g water/100 g gum), and OHC (146.5 g oil/100 g gum).     

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 optimization of watermelon seed protein using response surface methodology

Extraction conditions for maximum protein recovery from watermelon (Citrullus vulgaris Cv Sugar baby) seed meal were investigated using response surface methodology. A central composite design with four independent variables: temperature (40, 45, 50, 55 and 60 °C); NaOH concentration (0.03, 0.06, 0.09, 0.12 and 0.15 g/L); extraction time (5, 10, 15, 20 and 25 min) and solvent/meal ratio (30:1, 40:1, 50:1, 60:1 and 70:1, v/w) was used to study the response variable (protein yield). The experimental values of protein yield ranged between 72.03 and 81.52 g/100 g seed meal. A second-degree equation for independent and response variables was computed and used to create the contour plots graphs. The predicted values obtained for protein yield revealed that coefficient of determination and standard error was 0.80 and 0.906, respectively. Optimum protein extraction was obtained with 0.12 g/L alkali concentration, 15 min extraction time and 70:1 (v/w) solvent/meal ratio at 50 °C. Confirmatory studies revealed that the protein yield under optimum conditions was 80.71 g/100 g seed meal.     

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.     

Subcritical water extraction of flavonol quercetin from onion skin

Subcritical water could be an excellent alternative to organic solvent as a medium for extracting flavonol quercetin, due to its temperature-dependent selectivity, safety, efficiency of recovery, and lower cost. This study investigated the application of subcritical water extraction (SWE) of quercetin from onion skin and evaluated the effect of key operation conditions by varying the temperature (100-190 °C), extraction time (5-30 min), and mixture ratio of onion skin and diatomaceous earth (DE) (0.5:3.5-2:2) under high pressure (90-131 bar). The maximum yield of quercetin (16.29 ± 0.75 mg/g onion skin) was obtained at extraction temperature of 165 °C, extraction time of 15 min, mixture ratio of 1.5:2.5 for onion skin and DE. The SWE was compared with three conventional extraction methods in terms of the efficiency. The quercetin yield by SWE was over eight-, six-, and fourfold greater than those obtained using the ethanol, methanol, and water-at-boiling-point extraction methods, respectively.     

Supercritical carbon dioxide extraction of the residual oil from palm kernel cake

Palm kernel cake contains residual oil that has never been retrieved and it is treated as wastes. In this study, supercritical carbon dioxide was used to separate the oil from the palm kernel matrix. The studied extraction parameters were at the set pressures 27.57, 34.47 and 41.36 MPa, temperatures 40-70 °C and carbon dioxide flow rate between 1 and 3 ml/min. The effect of the particle size on the oil yield was examined using different particle size that separated by sieving from ?106, ?150, ?180, ?250 and ?450 μm. The results showed that the highest oil removed was 9.26 g oil/100 g sample (p < 0.05) for the particle ?150 μm, and under extraction temperature of 70 °C, pressure 41.36 MPa, and carbon dioxide flow rate of 2 ml/min. The experimental results indicate that supercritical carbon dioxide extraction could be a viable technique to remove the remaining oil and to produce defatted palm kernel cake.     

Supercritical fluid extraction of grape seed: Process scale-up, extract chemical composition and economic evaluation

The scale-up of the supercritical fluid extraction (SFE) process for grape (Vitis vinifera L.) seed was studied from the laboratory (0.29 L) to the pilot scale (5.15 L) at 35 MPa and 313 K. The scale-up criterion adopted consisted of maintaining a constant solvent to feed ratio (S/F), and the criterion was successfully used to predict the approximate behavior of the SFE process from the laboratory at the pilot scale for a 17-fold scale-up. Linoleic acid was the major component of the extract; palmitic, stearic and oleic acids were also detected. The economic evaluation showed that it is viable to establish a SFE plant in Brazil for SFE processing of grape seed. From the technical-economic evaluation, for SFE of grape seed at 313 K/35 MPa, an extraction time of 240 min and S/F of 6.6 produced the best relationship between yield and cost.     

Isolation of hesperidin from peels of thinned Citrus unshiu fruits by microwave-assisted extraction

Simultaneous extraction by microwave-irradiation and crystallisation were performed in the same pot of solvent of 70% (v/v) aqueous ethanol for isolation of hesperidin from thinned immature fruit peels of Citrus unshiu as refining of Citrus waste biomass. The hesperidin content in immature fruits peels was about 3.2-fold higher than that of mature fruit. After microwave-assisted extraction (MAE), the yield of hesperidin reached 58.6 mg/g, which was comparable to the amount obtained after extraction using DMSO:methanol (1:1, v/v) as a solvent for 30 min at room temperature. Heating temperature and time for isolation of hesperidin crystallites were optimised as 140 °C and 8 min by using response surface methodology. Under this optimal condition, 86.8% (47.7 mg/g) of total hesperidin was isolable by MAE and low-temperature storage (5 °C, 24 h).     

微波-超声协同辅助提取燕麦麸油的研究

本研究采用微波-超声协同辅助提取技术从燕麦麸皮中提取燕麦麸油,考察了溶剂配比、微波功率、液料比和作用时间对燕麦麸油得率和抗氧化活性的影响。试验结果表明,燕麦麸油的最佳微波-超声协同辅助提取工艺条件为正己烷∶乙醇=1∶1(V/V)、功率300 W、液料比12∶1(m L/g)、作用时间60 s,在此条件下,燕麦麸油的得率为6.88%;与溶剂浸提相比,微波-超声协同辅助提取的燕麦麸油具有更强的抗氧化活性,对DPPH自由基清除的IC50值1.064 mg/m L,其中主要的抗氧化活性物质总酚、生育酚(VE)、甾醇的含量分别为(1 531.04±10.28)、(84.15±2.47)mg/kg和(578.23±7.04)mg/100 g;GCMS结果显示微波-超声协同辅助提取燕麦麸油的主要脂肪酸组成为棕榈酸、油酸、亚油酸,与溶剂浸提的无明显差异。     

Phenolic and antioxidant potential of olive oil mill wastes

Olive oil mill waste was subjected to conventional liquid solvent extraction and supercritical fluid extraction using different solvents and carbon dioxide, respectively. The optimum solvent extraction conditions of phenols were 180 min using ethanol, at a solvent to sample ratio 5:1 v/w, and at pH 2. Solvent and SFE extracts were tested for their antioxidant activity by the DPPH radical scavenging method and by determination of peroxide value on virgin olive oil and sunflower oil. The ethanol extract exhibited the highest antiradical activity, and no correlation was found between antiradical activity and phenol content. The SFE extract exerted good antioxidant capacity although its phenolic yield was not quite high. Moreover, the ethanol extract appeared to be a stronger antioxidant than BHT, ascorbyl palmitate and vitamin E by the Rancimat method on sunflower oil. HPLC analysis of the extracts showed that the predominant phenolic compound was hydroxytyrosol. Various phenolic acids and flavonoids were also identified.     

Ultrasound-assisted extraction of polyphenols (flavanone glycosides) from orange (Citrus sinensis L.) peel

The present study reports on the extraction of polyphenols especially flavanones from orange (Citrus sinensis L.) peel by using ethanol as a food grade solvent. After a preliminary study showing that the best yield of extraction was reached for a particle size of 2 cm², a response surface methodology (RSM) was launched to investigate the influence of process variables on the ultrasound-assisted extraction (UAE) followed by a central composite design (CCD) approach. The statistical analysis revealed that the optimised conditions were a temperature of 40 °C, a sonication power of 150 W and a 4:1 (v/v) ethanol:water ratio. The high total phenolic content (275.8 mg of gallic acid equivalent/100 g FW), flavanone concentrations (70.3 mg of naringin and 205.2 mg of hesperidin/100 g FW) and extraction yield (10.9 %) obtained from optimised UAE proved its efficiency when compared with the conventional method. Furthermore, the antioxidant activity determined by the DPPH and ORAC tests confirmed the suitability of UAE for the preparation of antioxidant-rich plant extracts.     

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.     

Recovery and characterization of proteins precipitated from surimi wash-water

The objectives of this study were testing the methodology involved in the recovery of water-soluble proteins from surimi wash-water (SWW) by shifting the pH and organic solvent use, and characterization of the recovered proteins. Water-soluble proteins were recovered from three successive washes in a surimi process; these were: 1.23 ± 0.08, 0.64 ± 0.06 and 0.54 ± 0.05 mg/mL for wash stages I (WS-I), II (WS-II) and III (WS-III), respectively. For WS-I, most of the recovered proteins had a molecular weight (MW) between 23.2 and 71.6 kDa with some traces having less than 23.2 kDa. WS-II and III also had MW between 23.2 and 71.6 kDa; however, at a lower amount. Maximum precipitation from surimi wash-water was obtained at pH 3.5 (66.3 g protein/100 ml SWW). Percentage of precipitation was directly related to temperature. Increasing the organic solvent concentration (10-60 g ethanol/100 g SWW) yielded greater precipitation. The highest precipitation (65.0 g protein/100 mL SWW) was obtained with ethanol concentration of 60 g/100 g SWW. Reaction time for pH shift and organic solvent had little or no significant effect (p > 0.05) on percentage of precipitation. Minimum solubility of recovered proteins occurred around pH 3.5 and 60 g/100 g of ethanol, an increase in temperature decreased protein solubility.     

Response surface optimisation of aqueous enzymatic oil extraction from bayberry (Myrica rubra) kernels

Aqueous enzymatic extraction (AEE) of oil from Myrica rubra kernels was performed. The four AEE parameters namely mixed enzyme (cellulose/neutral protease = 1/2, w/w) amount, liquid/solid ratio, extraction time, and temperature, were optimised by response surface methodology. The statistical analysis indicated that the enzyme amount, liquid/solid ratio, time, and the quadratics of liquid/solid ratio, and enzyme amount, as well as the interactions between time and temperature, showed significant effects on oil yield. The optimal extraction conditions for oil yield were mixed enzyme amount, liquid/solid ratio, time, temperature as 3.17% (w/w), 4.91 ml/g, 4 h and 51.6 °C. Under the optimum conditions, the experimental oil extraction yield was 31.15%. The GC–MS analysis showed that the oil was abundant in the unsaturated fatty acids (9-octadecenoic acid and 9,12-octadecadienoic acid accounting for more than 80%), and the AEE was more efficient method to extract polyunsaturated fatty acid than the organic solvent process.     

Supercritical carbon dioxide fluid extraction of Hibiscus cannabinus L. seed oil: A potential solvent-free and high antioxidative edible oil

The supercritical fluid extraction (SFE) trends and antioxidant activities of Hibiscus cannabinus seed oils were studied. SFE results indicate that extraction pressure is the major factor determining the oil yield. In comparison, classic Soxhlet extraction (SOX/L) yielded higher oil content than SFE (P < 0.05). However, no significant differences in oil content were observed in SFE at 600 bars/80 °C, rapid Soxhlet extraction (SOX/S) and conventional ultra-sonic assisted solvent extraction (SONIC) (P > 0.05). Antioxidant activities of H. cannabinus seed oils were compared with 7 types of commercial edible oils. DPPH scavenging activity test indicated that H. cannabinus seed oil extracted by SFE at 200 bars/80 °C possessed the highest antiradical activity whereas beta-carotene bleaching (BCB) assay revealed that all H. cannabinus seed oils (except for SFE at 400 bars/80 °C and 600 bars/80 °C) exhibited higher antioxidant activity than all commercial edible oils (P < 0.05). Thus, SFE – H. cannabinus seed oil may serve as an excellent source of solvent-free edible oil with high antioxidant properties.     

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.