Supercritical fluid extraction of oils from apple seeds: Process optimization,chemical characterization and comparison with a conventional solvent extraction

Oils from apple seeds were extracted with the application of supercritical fluid (SFE) and Soxhlet techniques. The effect of SFE experimental variables such as pressure (10–30 MPa), temperature (40–60 °C) and carbon dioxide flow rate (1–8 L/h) on the yield, antioxidant activity and total phenolic content was investigated using a central composite design. The experimental data were fitted with a second-order polynomial equation using regression analysis. The maximum yield, obtained at the optimum processing conditions (24 MPa, 40 °C, 1 L/h of carbon dioxide flow rate, 140 min) was 20.5 ± 1.5% (w/w). For comparison, the yield from Soxhlet extraction was 22.5 ± 2.5% (w/w). Both techniques produced an oil with a fatty acids profile rich in linoleic acid. However, the extract from SFE was higher in linoleic acid (63.76 ± 4.96 g/100 g_oil) than that achieved by Soxhlet (49.03 ± 3.85 g/100 g_oil). Despite the higher unsaturated fatty acids content, SFE extracts reported a higher oxidative stability (21.4 ± 1.2 h) compared to that one extracted by Soxhlet (12.1 ± 1.1 h). This result was expport addressing the extraction of apple seed oil by supercritical fluid at pressures lower tha The most abundant phenolic compound found in the extract was phloridzin (2.96 ± 0.046 μg/gs_eed in SFE oil and 1.56 ± 0.026 μg/g_seed in Soxhlet). Instead, amygdalin, one of the antinutrients present in seeds, was not detected in the SFE oil.Industrial relevanceThe present study provided results addressing the extraction of apple seed oil by supercritical fluid at pressures lower than 30 MPa. The process allowed extracting an oil that was rich in unsaturated fatty acids, oxidative stable thanks to the high antioxidant activity, and free from anti-nutritional compounds.     

Comparison of yields and quality of nutmeg butter obtained by extraction of nutmeg rind by soxhlet and supercritical carbon dioxide (SC-CO2)

Nutmeg is a native South East Asian plant which has medicinal properties. In this work, supercritical extraction was studied in order to obtain experimental data of the influence of pressure, temperature and particle size and in comparison to soxhlet extraction. Supercritical extraction was conducted at operating temperatures of 40, 50 and 60 °C, operating pressures of 20.7, 27.6, 34.5 and 41.4 MPa and dynamic extraction time was 90 min. The effect of three different sieved particle sizes ?0.500, ?1 mm and ?2 mm on the extraction yield was examined. The results show that the highest yield was 38.8 g oil/100 g sample obtained under extraction temperature of 60 °C, pressure 41.4 MPa using particle size of ?0.5 mm. Soxhlet extraction yields 34 g oil/100 g sample for 6 h of extraction time. The GCTOFMS shows that the supercritical extracts exhibited significantly higher aromatic ether group comparable to those obtained by soxhlet.     

Effects of Particle Size,Applied Pressure and Pressing Time on the Yield of Oil Expressed from Almond Seed

An investigation of the effects of particle size, applied pressure and pressing time on the yield of oil expressed from almond seeds was undertaken. The oil was expressed mechanically using a mini laboratory oil press. The fixed processing parameters were: moisture content of 17% wet basis, heating temperature of 65 – 70°C and heating time of 15 min. The pressing pressures used were 60.6 kPa, 101.3 kPa and 116.6 kPa. Pressing times used were 2, 4, 8 and 12 min, and particle size of Φ < 0.5 mm (fine sample) and Φ > 0.5 mm (coarse sample) were used. The result shows that oil yield increased with increase in applied pressure and pressing time, however result obtained from fine and coarse sample sizes are similar. Pressing time and applied pressure had significant (p < 0.05) difference on oil yield; particle size had no significant (p > 0.05) difference on oil yield. Regression and correlation analysis gave a reasonable experimental prediction between oil yield and applied pressure with correlation coefficient r = 0.952 and also with pressing time with r = 0.7342. Higher oil yields were obtained from samples with fine particles size (Φ < 0.5 mm) and coarse particles size (Φ > 0.5 mm) samples pressed at 116.6 kPa pressure for 12 min. Maximum oil yields of 48.44% and 48.40% were obtained from coarse and fine samples respectively. The results obtained can be used in the design of a suitable process and machine for the expression of oil from almond seed.     

Optimization of the enzymatic treatment during aqueous oil extraction from sunflower seeds

Partially dehulled sunflower seeds were subjected to a hydrolytic treatment with cellulases during aqueous processing for oil and protein extraction. Sub-optimal extraction conditions (particle size and separation technology) were established in order to appreciate the potential improvement caused by the enzymatic treatment and to select the best operational conditions. The effects of three operational variables (extraction–treatment time, water/seeds ratio and enzyme/seed ratio) were studied on three objective functions (the extent of hydrolysis reaction, the oil extraction yield and the percent polyphenolics removal). After 2 h of enzymatic treatment–extraction a practical optimum in the range 7.5–8 g water g⁻¹ seeds and 1.25–1.4 g enzyme 100 g⁻¹ seeds could be defined. Under these conditions the oil extractability and the polyphenolics removal are improved by more than 30 and 80%, respectively.     

Extraction of oil from tiger nut (Cyperus esculentus L.) with supercritical carbon dioxide (SC-CO2)

Supercritical carbon dioxide (SC-CO₂) was used to extract oil from tiger nuts and the physicochemical properties and the impact of extraction conditions [i.e., temperature (40 °C–80 °C), pressure (20–40 MPa) and time (60–360 min)] on the oil yield were studied. The response surface analysis results revealed that the oil yield was significantly (P < 0.05) influenced by the main effect of the extraction pressure, extraction time and their quadratic effects respectively. However, the interaction between the extraction temperature and time had no significant (P > 0.05) effect on the oil yield. The highest oil yield was 26.28 g/100 g sample after 210 min of extraction time at 30.25 MPa and 60 °C respectively. The fatty acid composition of oils obtained by SC-CO₂ and Soxhlet showed marked variation. Also, the fatty acid composition varied depending on the operating conditions. The viscosity of the oil decreased with the increase in temperature.     

Extraction of sesame seed oil using supercritical CO2 and mathematical modeling

In this work, extraction of sesame oil from sesame seeds using supercritical CO₂ was carried out. The effect of operating parameters such as pressure, temperature, and supercritical CO₂ flow rate and particle size on extraction yield were investigated. An increase in the pressure and the supercritical CO₂ flow rate improved the extraction yield and also shortened the extraction time. The extraction yield increased as the particle size decreased depending on decreasing intraparticle diffusion resistance. The maximum extraction yield obtained was about 85% (relative to Soxhlet extraction by hexane) at 50 °C, 350 bar, 2 mL CO₂/min, 300–600 μm of particle size. Some extraction curves were modeled with two mathematical approaches as shrinking core model and broken and intact core model. The evaluation of model parameters showed that shrinking core model, however, is better than broken and intact cell model.     

Supercritical fluid extraction and microencapsulation of bioactive compounds from red pepper (Capsicum annum L.) by-products

The objective of this work was to obtain and stabilize natural vitamins from red pepper by-products. The method of obtainment was supercritical carbon dioxide extraction, studying different parameters that affect the yield. The highest extraction yield was found at 60 °C, 24 MPa extraction, with no modifier added and 0.2–0.5 mm particle size. The recovered extract was a red-coloured oil. The extract was subsequently microencapsulated by spray-drying using gum arabic as wall material to avoid the degradation of vitamin over the storage time. The thermal stability of microcapsules was analysed by thermal gravimetric analysis (TGA), while size, shape and morphology of microcapsules were studied by scanning electron microscopy (SEM). The microcapsules containing pepper extract were particles of spherical shape with dents on the surface, the average size of these particles was 5.46 μm.     

Ultrasound-assisted extraction of pomegranate seed oil – Kinetic modeling

In this work, ultrasound-assisted extraction was employed to extract oil from pomegranate seeds. Seed particle size, extraction temperature, solvent/solid ratio, amplitude level, and pulse duration/pulse interval ratio were the factors investigated with respect to extraction yield using a central composite design. The optimum operating conditions were found to be: seed particle size, 0.2 mm; extraction temperature, 20 ^oC; solvent/solid ratio, 20/1; amplitude level, 60%; pulse duration/pulse interval ratio, 5/15. Under these optimized conditions, the predicted value for extraction yield was 59.8%. A second-order kinetic model was successfully developed for describing the mechanism of ultrasound extraction under different processing parameters.     

Optimization of subcritical fluid extraction of seed oil from Nitraria tangutorum using response surface methodology

Subcritical fluid extraction (SFE) technology was used to extract oil from Nitraria tangutorum seed. The best possible combination of extraction parameters was found using response surface methodology (RSM) in a three-variable, three-level Box-Behnken experimental design (BBD). The optimum extraction parameters were an extraction time of 40 min, an extraction pressure of 0.60 MPa, an extraction temperature of 44 °C and a raw material particle size of 0.45 mm. Conventional solvent extraction and supercritical CO₂ fluid extraction were comparatively used. The yield of seed oil obtained using SFE was 12.92%, which was similar to or higher than the other methods. The chemical compositions of the seed oil, determined by GC–MS, indicate that its unsaturated fatty acids content was 97%. SFE proved to be an effective technique for extracting oil from N. tangutorum.     

Texturing and Instant Cooling of Rapeseed as Pretreatment Prior to Pressing and Solvent Extraction of Oil

Instant controlled pressure drop process (DIC) was used to texture rapeseeds in order to intensify oil extraction performances of both pressing and solvent extraction processes. Solvent extraction from both DIC-textured and non-treated raw material RM seeds was achieved with n-hexane using separately accelerated solvent extraction (ASE) and dynamic maceration (DM). ASE allowed quantifying the extraction yields while the extraction kinetics issued from DM experimental data was studied through coupled washing/diffusion CWD phenomenological model. ASE oil contents were 622.5?±?0.5 and 664.4?±?0.5 g oil/kg dry dry basis ddb for untreated and DIC-textured seeds, respectively. In terms of kinetics, 45-min DM of DIC-treated seeds implied higher yields than 8-h DM of RM (467.8?±?0.5 against 435.6?±?0.5 g oil/kg ddb). Moreover, pressing oil yields reached 553.5?±?0.5 against 490?±?0.5 g oil/kg ddb for DIC and RM seeds, respectively. Besides, optimized DIC treatment allowed obtaining preservation of lipid fatty acid profiles.     

Tocotrienol levels in sieving fraction extracts of brewer’s spent grain

Dried brewer’s spent grain (DBSG) is rich in tocotrienols (T3) and tocopherols (T) and can be used to produce a valuable oil with the serum cholesterol–lowering functions of lipid-soluble T3. The economic feasibility of extracting oil from DBSG (fat: 3.9–10.6% dry weight, dw) increases with increasing fat content of the feedstock. The objective of this research was to determine whether DBSG can be separated into fractions enriched in fat and T3 by milling and sieving and to characterize the fractions from sieves of different mesh sizes: 500, 800, 850, and 1,000 μm. Six different charges of DBSG were milled and sieved with different techniques ranging in scale from laboratory to industrial. The oil yield of DBSG sieving fractions >500 μm was consistently low (6.6–12.67% dw after Soxhlet extraction with 96% ethanol), as were the levels of T (77.4–185.6 mg/kg of extracted oil), T3 (181.9–538.8 mg/kg of extracted oil), and protein (14.38–25.73% dw). In contrast, oil yields of DBSG sieving fractions <500 μm were higher (12.98–18.09% dw after Soxhlet extraction with 96% ethanol), as were the concentrations of T (188.6–318.0 mg/kg of extracted oil), T3 (516.8–850.2 mg/kg of extracted oil), and protein (26.05–33.30% dw). Furthermore, oil yields were lower (8.24–12.39% dw) after Soxhlet extraction with n-hexane. Milled DBSG sieving fractions <500 μm thus appear to be a suitable feedstock for economical extraction of T3-rich oil and may be useful in developing markets for value-added brewing by-products.     

Supercritical carbon dioxide extraction of oil and α‐tocopherol from almond seeds

The objective of this study was to extract oil and tocopherols from almond seeds using supercritical carbon dioxide and to compare this extraction with a traditional solvent method. Oil and tocopherol extraction rates were determined as functions of the pressure (350–550 bar), temperature (35–50 °C) and CO₂ flow rate (10–30 kg h⁻¹), using a 10‐l vessel. The effects of matrix particle size on extraction yield were also studied and it was demonstrated that extraction yield is greatly influenced by particle size. Maximum recovery was obtained in the first 2–3 h of extraction at a pressure of 420 bar, a temperature of 50 °C and a flow rate of 30 kg h⁻¹ CO₂. These results suggest that the elevated initial oil and tochopherol solubility is related to the increased proportion of fatty acids in the initial extract. The results were compared with those obtained when hexane/methanol was used as a solvent. Copyright © 2005 Society of Chemical Industry     

Enzyme‐assisted aqueous extraction of safflower oil: optimisation by response surface methodology

Aqueous enzymatic oil extraction of safflower seeds was assisted by Alcalase 2.5L and Celluclast 1.5L. Enzyme type and amount, pH, time, temperature, churning rate, dilution ratios and particle size were varied to determine their influence on the oil amount. The amount of oil recovered was higher using seeds ground to a particle size of <0.6 mm. Response surface methodology was employed for the optimisation of aqueous enzymatic oil extraction conducted with Celluclast 1.5L. When the extraction was assisted by Celluclast 1.5L, the maximum oil amount and yield were 33.3 (% w/w) and 79.7 (% w/w), respectively. The optimum conditions were 48.3 °C; 0.25 mL enzyme g^?1 substance; pH, 4.84; resulting oil amount and yield were 28.2 (% w/w) 65 (% w/w), respectively. The predicted critical values were experimentally verified, and an oil amount of 27.1 (% w/w) was achieved. The enzyme treatment did not have any determining effect on the physicochemical properties of extracted oil.     

金银花种子中脂溶性成分分析

以金银花种子为原料,在索氏提取仪中用乙醚提取脂溶性成分, 测定其含量,并将其分成极性和非极性两类,用GC-MS 进行分析。结果表明,忍冬种子中油脂含量为25%,极性成分有21 种化合物,非极性成分有45 种化合物。     

Extraction of Cuminum cyminum essential oil by combination technology of organic solvent with low boiling point and steam distillation

Extraction of essential oil from Cuminum cyminum seeds using a combination of organic solvent with low boiling point and steam distillation was explored. The effect of different parameters, such as particle size (40, 60, 80 mesh), temperature (°C) 10, 15, 20 and extraction time (3, 5, 8 h), on the extraction yield was investigated using three-level orthogonal array design. The experimental results showed that the temperature had the largest effect on the yield of the extract (oleoresin), followed by extraction time and particle size. The optimum parameters, such as temperature, particle size, and extraction time were in turn 20 °C, 80 mesh, and 8 h. Essential oil of C. cyminum seeds obtained by supercritical fluid extraction (SFE), hydrodistillation (HD), combination technology of organic solvent with low boiling point and steam distillation (OS-SD) were further analysed by gas chromatographic/mass spectrometric detection to compare the extraction methods. Forty-five compounds in the C. cyminum essential oil were identified, showing that the composition of the extraction by different methods was mostly similar, whereas relative concentration of the identified compounds was apparently different. General characteristics of the C. cyminum essential oil obtained by different methods were further compared, and OS-SD was considered as the optimum process among the three processes to obtain C. cyminum essential oil for high quality, simple technology and low cost.     

EXTRACTION OF VOLATILE OIL FROM CUMIN (CUMINUM CYMINUM L.) WITH SUPERHEATED WATER

A comparative study of superheated water extraction (SWE) with two conventional methods including hydrodistillation and Soxhlet extraction was performed on cumin (Cuminum cyminum L.). The effect of some superheated water parameters at 20 bar pressure on the essential oil extraction from 4 g cumin seeds such as temperatures from 100 to 175C, particle size at 0.25 and 0.50 mm, and flow rates at 2 and 4 mL/min were investigated. Separation and identification of the components were carried out by gas chromatography‐flame ionization detector and gas chromatography‐mass spectrometry. The best operating conditions for the SWE of C. cyminum L. were determined to be 150C temperature, 0.50 mm mean particle size and 4 mL/min flow rate for 3‐h extraction time. The SWE method resulted in a more valuable essential oil with respect to the oxygenated components.     

Subcritical fluid extraction of Lycium ruthenicum seeds oil and its antioxidant activity

The effective, energy-saving and green subcritical fluid extraction (SFE) technology was applied to obtain the oil from Lycium ruthenicum seeds (LRSO). The optimal conditions of extraction parameters were found using response surface methodology with Box-Behnken experimental design. The maximum extraction yield of 21.20% was achieved at raw material particle size of 0.60 mm, extraction pressure of 0.63 MPa, temperature of 50 °C and time of 48 min. Other traditional extraction technologies were comparatively used. The physicochemical property of LRSO was analysed and the chemical compositions indicated that they were rich in unsaturated fatty acid, β-carotene, tocopherols and total phenolics. Furthermore, the antioxidant activity of LRSO was evaluated by scavenging activity of three kinds of radicals (DPPH·, ·OH and O₂^-·) and lipid peroxidation in vitro. And its results showed the oil had the potential to be a novel antioxidant agent for using in the field of food, pharmaceuticals and cosmetics.     

Supercritical Carbon Dioxide Extraction of Squalene from <Emphasis Type="Italic">Amaranthus paniculatus</Emphasis>: Experiments and Process Characterization

Separation of squalene from Amaranthus paniculatus using supercritical carbon dioxide extraction (SC-CO₂) technology and optimization of its process parameters such as temperature, pressure, time of extraction, flow rate of carbon dioxide, and batch size have been conducted. The optimized conditions that provided the best yield of squalene were a sample size of 40 g of amaranth grains of particle diameter of 0.75 mm at a temperature of 100°C and pressure of 550 bar for 1.5 h extracting time at a flow rate of 0.2 L min⁻¹ of carbon dioxide. Solubility of squalene in SC-CO₂ under different operating conditions has also been evaluated using Chrastil equation which showed good agreement with the experimentally obtained yields. Various statistical analyses (regression equations, t test, and analysis of variance) conducted on the extraction parameters concluded that extraction pressure, time and sample batch size have significant effect on the yield of the squalene whereas extraction temperature and particle diameter do not. The results obtained are in accordance to the basic principle of supercritical fluid-phase equilibrium behavior and the solubility isobar and isotherm obtained showed similar trends with those reported for squalene. Using dimensionless numbers, an empirical correlation was also deduced for characterization of the extraction process of squalene in SC-CO₂.     

Effect of chlorophyll removal and particle size upon the nutritional and technological properties of powdered by‐products from artichoke (Cynara scolymus,L.) industrial canning

In this study, the effect of the particle‐size fractionation (Ø < 0.212 mm and 0.212 mm < Ø < 0.991 mm) and chlorophyll extraction on the nutritional and technological properties of the powdered artichoke ingredient was evaluated. The contents of minerals, protein, fat, carbohydrates and dietary fibre together with the content in bioactive compounds such as inulin and phenolics were determined. Other properties such as water‐ and oil‐holding capacities, water activity and antioxidant capacity were measured. The ingredient with chlorophyll and the lowest particle size presented the highest phenolic content and antioxidant capacity (8.4 mg of vitamin C equivalents per 100 g of dry matter) and water‐ and oil‐holding capacities. The removal of chlorophyll increased the oil‐holding capacity (from 59.7% to 94.6%), which was much higher than in the coarse ingredient (34%), but has a deleterious effect reducing the antioxidant capacity and the inulin content. The ingredients also showed high dietary fibre (22.5–33%), inulin (9–16%) and mineral (7.5–7.8%) contents. Although the ingredient with chlorophyll and smaller particle size had the higher antioxidant capacity, the removal of chlorophyll improved the technological properties to be used as food ingredient without affecting significantly to the nutritional value.     

A supercritical tuneable process for the selective extraction of fats and essential oil from coriander seeds

A selective supercritical CO₂ extraction process has been developed in order to extract selectively the vegetal oil and the essential oil from coriander seeds in a consecutive way by tuning experimental conditions. A 4-step process has been set up: (i) seeds preparation by grinding and sieving, (ii) extraction by supercritical CO₂ and (iii; iv) selective separation in two separators with different pressure levels. The first part of this study consisted in studying the effects of the operating conditions (T, P, CO₂ density, flow rate and particle size distribution of ground seeds) on the yield of extraction. The results showed that the global performance of the process depends mainly on the pressure level of extraction, on the CO₂ flow rate and on the size of the ground seeds. An optimization of the parameters led to an extraction ratio of 90%. The second part of this study dealt with the effects of the operating conditions on the quality of extracts, and more precisely on their composition in vegetal oil and essential oil. It was observed that the supercritical extraction had no major effect on the fatty acid composition of the vegetal oil compared to classical extraction techniques, while essential oil is enriched in components such as linalool and that a previous drying of the seeds is deleterious. Finally, we propose a procedure in order to extract separately each oil by adjusting CO₂ density and separation conditions.