Extraction of palm oil using propane,ethanol and its mixtures as compressed solvent

This work is aimed to investigate the extraction of palm oil using pressurized ethanol and propane as solvents. The effects of temperature (293⿿333 K), pressure (from 10 to 20 MPa), solvent flow rate (from 1 to 5 mL/min), and composition of the solvent mixture were evaluated on the oil extraction yield, and chemical profile of the extracted oils. The experiments were conducted in a 100 mL extractor coupled to a HPLC pump for ethanol and a syringe pump for the propane displacement. Global yields up to 75 wt% were obtained in the experiments. The kinetic profiles of the extractions were described by the Sovová⿿s model, which presented good agreement with the experimental observations. The palm oils extracted with distinct solvents were characterized regarding its density and viscosity in a temperature range from 293 to 343 K, its chemical profile determined by GC/MS, and carotenoid content.     

Extraction of curcuminoids from deflavored turmeric (Curcuma longa L.) using pressurized liquids: Process integration and economic evaluation

Pressurized liquid extraction (PLE) of curcuminoids from deflavored turmeric rhizomes was optimized. The rhizomes were initially deflavored by extraction with supercritical CO₂. Immediately after SFE, PLE process was performed using ethanol as the solvent and a static extraction time of 20 min, and the independent variables were the temperature (333–353 K) and pressure (10–35 MPa). The results indicate that the optimum extraction temperature and pressure were 333 K and 10 MPa, respectively. PLE required three and six times less extraction time than low-pressure solvent extraction and Soxhlet extraction, respectively, to produce similar extraction yields. The cost of manufacturing (COM) decreased from US$ 94.92 kg⁻¹ to US$ 88.26 kg⁻¹ when the capacity of the two-extractor system increased from 0.05 m³ to 0.5 m³ and from US$ 94.92 kg⁻¹ to US$ 17.86 kg⁻¹ when the cost of the raw materials decreased from US$ 7.91 kg⁻¹ to US$ 0.85 kg⁻¹ for a two 0.05 m³ extractor system.     

Lycopene solubility in mixtures of carbon dioxide and ethyl acetate

In order to improve the efficiency of processes using supercritical (sc) carbon dioxide (CO₂) to micronize the carotenoid “lycopene”, it is important to know the solubility of lycopene in mixtures of the organic solvent ethyl acetate (EA) and the antisolvent CO₂ at elevated pressures. The solubility of lycopene has been determined for different temperatures (313–333 K), pressures (12–16 MPa) and CO₂ molar fractions (0.58–1). The obtained data show that CO₂ acts as an antisolvent in the system lycopene/EA/CO₂ in the range of CO₂/EA ratios studied. The solubility of lycopene is rather small with lycopene molar fractions ranging from 0.1 × 10⁻⁶ to 46 × 10⁻⁶. The solubility of lycopene increases with temperature, pressure and EA concentration.     

Phenolic and flavonoid content and antioxidants capacity of pressurized liquid extraction and perculation method from roots of Scutellaria pinnatifida A. Hamilt. subsp alpina (Bornm) Rech. f.

The extract was separated from roots of Scutellaria pinnatifida using perculation and pressurized liquid extraction (PLE). A circumscribed central composite (CCC) was used to optimize the effective extraction variables. For achieving maximum extraction yield via PLE the temperature, pressure, static time, dynamic time, and the solvent flow rate were adjusted 65.8 °C, 39.2 bar, 12.9 min, 18.9 min, and 0.76 mL/min, respectively. Ferric reducing antioxidant power (FRAP) (mmol/g) and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activity (mg/mL) were evaluated and the highest antioxidant activity was observed from the PLE extract. The total phenolic and flavonoid content was calculated and a good correlation founded between phenolic content and antioxidant activity. The results indicated the root of this plant is a potential source of natural antioxidants and flavonoids. The PLE method is quicker and it has more extraction yield than perculation.     

Application of response surface methodology for the optimization of supercritical carbon dioxide extraction and ultrasound-assisted extraction of Capparis spinosa seed oil

Caper (Capparis spinosa) seed oil growing wild in Iran was extracted using supercritical CO₂ and ultrasound-assisted extraction methods. The experimental parameters of SFE and UAE were optimized using a rotatable central composite design. The highest yield for SFE was obtained at a pressure of 355 bar, temperature of 65 °C, modifier volume of 140 μL, static and dynamic extraction time of 10 and 35 min, respectively, and for UAE was gained at solvent volume of 23 mL, sonication time of 45 min and temperature of 40 °C. This resulted in a maximum oil recovery of 25.1% and 27.9% for SFE and UAE, respectively. The extracts with higher yield from both methods were subjected to transesterification and GC–MS analysis. SFE and UAE processes selectively extracted the fatty oils with high percentage of omega-6 and omega-9-fatty acids. The major components of the extracted oils from both methods were linoleic, oleic, its positional isomer cis-vaccenic and Palmitic acid.     

Effect of different parameters on enzyme-assisted extraction of lycopene from tomato processing waste

The present study aims to optimize extraction process of lycopene by using solvents and examine the effect of enzyme treatment on the recovery if any. Different parts of tomato fruits like whole tomato, peel, pulp and industrial waste were screened for lycopene content. The extraction of lycopene was carried out with four different solvents to know their extraction efficiency. Two step extraction processes was followed for enzyme-assisted extraction of lycopene. In the first step waste samples were treated with enzymes i.e. cellulase and pectinase, whereas in second step extraction of lycopene was carried out by solvent. The optimization study with respect to concentrations and incubation time were carried out for both the enzymes. Also the effect of particle size and cooking methods on recovery of lycopene were studied. The results revealed that the tomato peel (417.97 μg/g) contains highest amount of lycopene followed by industry waste (195.74 μg/g), whole tomato (83.85 μg/g) and pulp (47.6 μg/g). When extraction was carried out by tri-mixture (i.e. acetone, ethanol and hexane) got higher recovery of lycopene than the other solvents. Maximum recovery of lycopene was obtained at 1.5% cellulase and 2% pectinase respectively at 4 h of incubation period. The results also indicated that finer the particle size, higher the recovery of lycopene, whereas all cooking methods reduced the recovery of lycopene. The above extraction process will be beneficial to the small scale entrepreneur to improve their socio-economical status.     

Pressurized liquid extraction and low-pressure solvent extraction of carotenoids from pressed palm fiber: Experimental and economical evaluation

In this work, a comparison of Soxhlet extraction (LPSE–SOX), percolation (LPSE–PE) and pressurized liquid extraction (PLE) for the recovery of carotenoid-rich extracts from pressed palm fiber (PPF) was carried out in terms of yield, carotenoid profile and economic viability to evaluate the methods’ industrial applicability. An optimization study was performed for each extraction technique with ethanol at a solvent/feed ratio of 20. The independent variables were temperature (35–55 °C), pressure (0.1–8 MPa) and flow rate (1.6, 2.4 g/min). The results showed that the global extraction yield obtained using LPSE–SOX (96 ± 4 mg extract/g PPF d.b.) after 6 h was higher than that obtained using LPSE–PE (74 ± 5 mg extract/g PPF d.b., 35 °C, 2.4 g/min) or PLE (44 ± 3 mg extract/g PPF d.b., 55 °C, 4 MPa, 2.4 g/min) after dynamic extraction time of 17 min under optimized conditions. On the other hand, the carotenoid yield obtained using PLE (305 ± 18 μg α-carotene/g extract and 713 ± 46 μg β-carotene/g extract) was higher than the obtained by LPSE–SOX (142 ± 13 μg α-carotene/g extract and 317 ± 46 μg β-carotene/g extract). PLE technique showed the highest selectivity for carotenoids than LPSE techniques. The lowest cost of manufacturing (COM) were obtained for LPSE–PE and PLE with values of US$13.4 and US$29.2/kg extract for a 0.5 m³ vessel capacity.     

Extraction of glycyrrhizic acid from licorice root using ultrasound: Process intensification studies

This work deals with the intensification of extraction process of glycyrrhizic acid (GA) from licorice using ultrasound. Various process parameters such as extraction time, solvent to solute ratio, extraction temperature and ultrasound frequency which affect the extraction yield are optimized. The maximum yield of 36.4 mg of GA/g of licorice is obtained at optimized parameters of 10 min time, 30:1 solvent to solute ratio, 40 °C temperature and 25 kHz frequency. The yield obtained with ultrasound assisted extraction (UAE) is compared with that of Soxhlet and batch extraction of GA. It is observed that the ultrasound assisted extraction not only gives higher yield but also reduces the extraction time as compared to conventional method. Temperature has no effect on ultrasound assisted extraction while higher frequency of ultrasound gives slightly better extraction yield. Further the kinetics of this extraction process is also investigated based on the second order rate equation available in the literature. Extraction rate constant, initial extraction rate and equilibrium concentration for different solvent to solute ratio and temperatures are predicted. Model validation is done successfully by plotting experimental and predicted values of concentration of GA in extract.     

Determination of sulfonylurea herbicides in soil samples via supercritical fluid extraction followed by nanostructured supramolecular solvent microextraction

The present work describes a sensitive procedure for extraction and determination of three sulfonylurea herbicides (metsulfuron-methyl, bensulfuron-methyl and chlorsulfuron) in water samples using supramolecular solvent microextraction. A supramolecular solvent with a nano structure made up of decanoic acid assemblies dispersed in tetrahydrofuran and water was proposed. Also, a supercritical fluid extraction coupled with supramolecular solvent microextraction was applied for extraction and determination of ultra-trace amounts of sulfonylurea herbicides in soil samples. A Taguchi orthogonal array experimental design with an OA₁₆ (4⁵) matrix was employed to optimize the supercritical fluid extraction conditions. In supercritical fluid extraction–supramolecular solvent microextraction procedure, a mixture of decanoic acid and the SFE collecting solvent (tetrahydrofuran) was added to water for supramolecular solvent formation. The effective parameters on the supramolecular solvent microextraction efficiency were studied and optimized using two different optimization methods: one variable at a time and face centered design. Under the optimum conditions, linear dynamic ranges varied within 0.1–5 mg kg⁻¹ (0.9978 ≤ R² ≤ 0.9987) and 0.5–100 μg L⁻¹ (0.9973 ≤ R² ≤ 0.9995) for all of the sulfonylurea herbicides in the supercritical fluid extraction–supramolecular solvent microextraction and supramolecular solvent microextraction, respectively. The intraday (n = 5) and interday standard deviations were calculated by extracting the SUHs from water and soil samples through supramolecular solvent microextraction and supercritical fluid extraction–supramolecular solvent microextraction. Interday RSDs% lower than 7.1% and intraday RSDs% lower than 3.8% were obtained. Limits of detection, based on a S/N ratio of 3, were 0.5 μg L⁻¹ and 0.7 mg kg⁻¹ for supramolecular solvent microextraction and supercritical fluid extraction–supramolecular solvent microextraction, respectively.     

Optimization of supercritical CO2 extraction of different anatomical parts of lovage (Levisticum officinale Koch.) using response surface methodology and evaluation of extracts composition

Supercritical carbon dioxide extraction (SFE-CO₂) parameters were optimized using response surface methodology and central composite design for lovage (Levisticum officinale Koch.) roots and leaves containing valuable phytoconstituents. Mathematical model predicted the highest yields of extracts from roots and leaves 2.26 and 2.29%, respectively, at 45 MPa pressure, 60 °C temperature, 90 min (roots) and 30 min (leaves) extraction time, whereas the yield of hydrodistilled essential oil was 0.24 and 0.74%, respectively. The highest relative content of the most valuable constituent Z-ligustilide in roots and leaves extracts was 77 and 50% at 10 MPa; however, the highest yields of this compound from 100 g of dry material were obtained at the highest applied pressure and constituted 1188 mg (roots) and 540 mg (leaves). This study showed that lovage is a good source of Z-ligustilide and SFE-CO₂ is a preferable technique for its isolation.     

Digestive enzymes characterization of krill (Euphausia superba) residues deoiled by supercritical carbon dioxide and organic solvents

In this study, Enzyme activities of krill were characterized before and after lipid extraction by supercritical carbon dioxide (SC-CO₂) and organic solvent, n-hexane and acetone. Krill SC-CO₂ extraction was performed under the conditions of temperature range from 35 to 45 °C and pressure, 150–250 bar for 2.5 h with a constant flow rate of 22 g/min. Extraction yields of lipids increased with pressure and temperature. The digestive enzyme activities of protease, lipase and amylase of SC-CO₂ treated krill residues were slightly decreased comparing to organic solvent, n-hexane and acetone treated residues. In SC-CO₂ treated samples, all of the digestive enzymes showed slightly higher temperature stability. In the other hand the crude extracts of SC-CO₂ and n-hexane treated krill samples showed almost same optimum pH and pH stability for each of the digestive enzymes. It was also found in SDS-PAGE that there are no significant differences in protein patterns of the crude extracts of untreated, SC-CO₂, n-hexane and acetone treated krill indicating no denaturation of proteins.     

A shrinking core model and empirical kinetic approaches in supercritical CO2 extraction of safflower seed oil

Utilization of supercritical CO₂ in safflower seed extraction was performed using a semi-batch extractor. Different extraction parameters, such as 40–60 MPa pressure, 323–347 K temperature, 20–76 min time, and 1–3 mL/min CO₂ flow rate were applied. A two-stage experimental design application was performed in order to maximize the oil yield. First of all, a 3² factorial design was applied to estimate the effect of the main factors and their interactions. The second part of the experimental design was improved and accelerated using the steepest ascent method. Optimum extraction parameters were determined to be 50 MPa pressure, 347 K temperature and 76 min time at a constant CO₂ flow rate (3 mL/min) according to the 2² design. Under these conditions, the oil yield obtained was 39.42%, comparable with Soxhlet extraction (40%) for 8 h. Shrinking core and empirical kinetic models were applied in order to generalize the extraction process. The predicted data was compatible with the experimental data.     

Subcritical water extraction of steviol glycosides from Stevia rebaudiana leaves and characterization of the raffinate phase

The objectives of this work were to obtain steviol glycosides of S. rebaudiana leaves, possessing natural and noncaloric sweetener properties, using subcritical water extraction; to assess optimum extraction conditions; to determine biological activities of Stevia extracts and to characterize the raffinate phase. A Box–“Bhenken” statistical design was used to evaluate the effects of various values of temperature (100–150 °C), time (30–60 min) and flow rate (2–6 ml/min) at a pressure of 230 bar applying a solid/liquid ratio of 1:10 (m:v). The most effective parameter was temperature (p < 0.005). Optimum extraction conditions were elicited as 125 °C, 45 min, 4 ml/min flow rate which yielded 38.67 mg/g stevioside and 35.68 mg/g rebaudioside A. The total phenolic, flavonoid contents and DPPH free radical scavenging activity were found as 48.63 mg gallic acid/g extract, 29.81 mg quercetin/g extract and 92.50%, respectively. After extraction, total chlorophyll, carotenoid contents and dietary fibers were quantified as 31.91 mg/100 g, 5.71 mg/100 g and 4.98% in the raffinate phase. Hence, both extract and raffinate phases of S. rebaudiana leaves can be utilized as sources of natural sweeteners, fibers and coloring agents in the industry.     

Extraction of protocatechuic acid from Scutellaria barbata D. Don using supercritical carbon dioxide

The use of supercritical carbon dioxide (SC⿿CO₂), with water as a modifier, was evaluated in this study as a method to extract protocatechuic acid (PA) from Scutellaria barbata D. Don. The highest extraction yield of PA, 64.094 ± 2.756 μg/g of dry plant, was achieved at 75 °C and 27.5 MPa, with the addition of 15.6% (v/v) water as a modifier. The mean particle size was 0.355 mm, the CO₂ flow rate was 2.2 mL/min (STP) and the dynamic extraction time was 100 min. At pressures of 16.2⿿30.0 MPa and temperatures of 45⿿75 °C, the mole fraction solubilities of PA in SC⿿CO₂ ranged from 2.829 ÿ 10^⿿7 to 9.631 ÿ 10^⿿7. The solubility data for PA fit well in the Chrastil model. It is evident that the SC⿿CO₂ extraction uses less solvent, saves both energy and time and is an environmentally friendly extract technology that can be used in the food, cosmetic and pharmaceutical industries.     

Integrated supercritical fluid extraction and subcritical water hydrolysis for the recovery of bioactive compounds from pressed palm fiber

Pressed palm fiber (PPF), a residue obtained from palm oil industry, is a source of bioactive compounds, such as carotenoids, which are used as food additives. It also has cellulose and hemicellulose that can be used to yield fermentable sugars for the production of second generation ethanol. Supercritical fluid extraction (SFE) of pressed palm fiber provides an oil rich in carotenoids while subcritical water hydrolysis (SubWH) produces hydrolysates with high amounts of fermentable sugars. In this work, the effects of pressure (15–30 MPa) and temperature (318 and 328 K) on SFE of carotenoids were investigated. The SFE extract with highest carotenoid content was obtained at 318 K and 15 MPa (2.3% d.b., 0.81 mg β-carotene/g extract). After the extraction, the influence of process temperature (423–633 K), pressure (15 and 25 MPa), solvent:feed ratio (120 and 240), and residence time (1.25–5 min) on SubWH of the extraction residue was studied. At the temperature of 523 K, the highest total reducing sugar yield (11–23 g glucose/100 g carbohydrate) and the highest biomass conversion (40–97%) were obtained for any pressure and solvent:feed ratio. The highest selectivity for saccharide formation was found at 423 K (20–59 mol glucose/mol furfural equivalent). Optimal conditions for high saccharide formation and low sugar degradation product in subcritical hydrolysis were obtained at 523 K, 15 MPa, solvent:feed ratio of 120, residence time of 2.5 min with a total reducing sugar yield of 22.9 g glucose/100 g carbohydrate and a conversion of 84.9%.     

Extraction of bioactive components from Centella asiatica using subcritical water

Bioactive components, asiatic acid and asiaticoside, were extracted from Centella asiatica using subcritical water as an extraction solvent. Extraction yields of asiatic acid and asiaticoside were measured using high-performance liquid chromatography (HPLC) at temperatures from 100 to 250 °C and pressures from 10 to 40 MPa. As temperature or pressure increased, the extraction yield of asiatic acid and asiaticoside increased. At the optimal extraction conditions of 40 MPa and 250 °C, the extraction yield of asiatic acid was 7.8 mg/g and the extraction yield of asiaticoside was 10.0 mg/g. Extracted asiatic acid and asiaticoside could be collected from water as particles with a simple filtering process. Dynamic light scattering (DLS) was used to characterize particle size. Particles containing asiatic acid were larger (1.21 μm) than particles containing asiaticoside (0.76 μm). The extraction yields of asiatic acid and asiaticoside using subcritical water at 40 MPa and 250 °C were higher than extraction yields using conventional liquid solvent extraction with methanol or ethanol at room temperature while the subcritical water extraction yields were lower than extraction yields with methanol or ethanol at its boiling point temperature.     

Optimization of multi-stage countercurrent extraction of antioxidants from Ginkgo biloba L. leaves

Multi-stage countercurrent extraction (MCE) as a novel extraction technique was used to extract antioxidants from Ginkgo biloba leaves. Orthogonal array design (OAD) was employed to optimize the ratio of 60% ethanol to raw material (8–16 mL/g), extraction time (30–60 min) and extraction temperature (60–80 °C) to obtain a high yield of antioxidants from G. biloba leaves by MCE. The optimum conditions were a ratio of 60% ethanol to raw material of 16 mL/g and extraction time of 30 min at 80 °C. Under these conditions, the yields of flavonoids and total phenolics were 1.74% and 2.42%, respectively, and DPPH radicals scavenging activity of the extract was 89.97%. Compared with heat-reflux extraction, MCE had obvious advantages of less extraction time and lower solvent and energy consumption. It may be used as a promising technique for the extraction of bioactive compounds from plant materials.     

Extraction of phenolic compounds from pitanga (Eugenia uniflora L.) leaves by sequential extraction in fixed bed extractor using supercritical CO2, ethanol and water as solvents

With the goal of maximizing the extraction yield of phenolic compounds from pitanga leaves (Eugenia uniflora L.), a sequential extraction in fixed bed was carried out in three steps at 60 °C and 400 bar, using supercritical CO₂ (non-polar) as solvent in a first step, followed by ethanol (polarity: 5.2) and water (polarity: 9.0) in a second and third steps, respectively. All extracts were evaluated for global extraction yield, concentration and yield of both polyphenols and total flavonoids and antioxidant activity by DPPH method (in terms of EC₅₀). The nature of the solvent significantly influenced the process, since the extraction yield increased with solvent polarity. The aqueous extracts presented higher global extraction yield (22%), followed by ethanolic (16%) and supercritical extracts (5%). The study pointed out that the sequential extraction process is the most effective in terms of global extraction yield and yield of polyphenols and total flavonoids, because it produced the more concentrated extracts on phenolic compounds, since the supercritical ethanolic extract presented the highest phenolics content (240.5 mg GAE/g extract) and antioxidant capacity (EC₅₀ = 9.15 μg/mL). The most volatile fraction from the supercritical extract, which is similar to the essential oils obtained by steam distillation or hydrodistillation, presented as major compounds the germacrenos D and B + bicyclogermacrene (40.75%), selina-1,3,7(11)-trien-8-one + selina-1,3,7(11)-trien-8-one epoxide (27.7%) and trans-caryophyllene (14.18%).     

Supercritical fluid extraction of Prunus persica leaves and utilization possibilities as a source of phenolic compounds

Mediterranean countries contribute highly on world peach production and tonnes of waste leaves are released due to pruning. The aim of this study was to investigate the utilization possibilities of the leaves by supercritical fluid extraction. A statistical design was used to evaluate the effect of temperature (40–80 °C), pressure (150–300 bar) and concentration of ethanol as co-solvent (6–20%) at a flow rate of 15 g/min and for a duration of 60 min. The most effective variables were found as pressure and co-solvent ratio (p < 0.005). Optimum extraction conditions were elicited as 60 °C, 150 bar and 6% co-solvent yielding a total phenol content of 79.92 mg GAE/g extract, EC₅₀ value of 232.20 μg/ml and a radical scavenging activity of 53.25% which was higher than the value obtained by conventional solvent extraction method (32.23%). Consequently, Prunus persica L. leaves were found as a potential phenolic source for industrial applications.     

Production of a lycopene-enriched fraction from tomato pomace using supercritical carbon dioxide

In recent years there has been a growing interest in functional foods because they may provide beneficial effects on human health. Moreover, the increasing interest of consumers in functional foods has brought about a rise in demand for ingredients obtained using technologies perceived to be natural and safe. In this study, supercritical fluid technology was used in order to obtain lycopene from an extract of dried tomato pomace using sunflower oil and ethanol. After the supercritical fluid fractionation, four fractions were collected, three separated fraction (SF) from the separator (after 30, 60 and 120 min of fractionation) and one residual fraction (RF) from the bottom of column (after 120 min). The concentration of lycopene was studied in the different fractions obtained under different pressures (10 and 30 MPa), CO₂ flow rates (5 and 15 kg h⁻¹), and heights of loading (top and bottom). The quantitative determination of lycopene was performed by HPLC coupled with a diode array detector. The effects of the different extraction parameters, as well as their interactions, were investigated using a full factorial design with three factors and two levels; the optimal conditions were calculated through response surface methodology. A statistically significant difference in lycopene content in the four fractions was obtained.