The objective of this research is recovery of squalene from palm fatty acid distillate (PFAD) using supercritical fluid extraction (SFE). The extraction process was performed by using the SFE and recovered squalene was analyzed from total lipid extracts using HPLC. A central composite design was used to study the effect of SFE variables namely pressure (X₁) from 200 to 400 bar and temperature (X₂) from 40 to 60⁰C on the total lipid extracts (Y₁) and squalene concentration (Y₂) and optimize the SFE conditions. The nonlinear regression equations were significantly (p < 0.05) fitted for both responses with high R₂ (> 0.965), which had no indication of lack of fit. The results indicated that a combined pressure (200 bar) and temperature (50⁰C) was predicted to provide the optimum region in terms of total lipid extracts (13.84 ± 0.52%) and squalene concentration (418.31 ± 18.40 ppm) studied.
This study aims to optimise the operating conditions for the supercritical fluid extraction (SFE) of toxic elements from fish oil. The SFE operating parameters of pressure, temperature, CO2 flow rate and extraction time were optimised using a central composite design (CCD) of response surface methodology (RSM). High coefficients of determination (R²) (0.897-0.988) for the predicted response surface models confirmed a satisfactory adjustment of the polynomial regression models with the operation conditions. The results showed that the linear and quadratic terms of pressure and temperature were the most significant (p < 0.05) variables affecting the overall responses. The optimum conditions for the simultaneous elimination of toxic elements comprised a pressure of 61 MPa, a temperature of 39.8ºC, a CO₂ flow rate of 3.7 ml min⁻¹ and an extraction time of 4 h. These optimised SFE conditions were able to produce fish oil with the contents of lead, cadmium, arsenic and mercury reduced by up to 98.3%, 96.1%, 94.9% and 93.7%, respectively. The fish oil extracted under the optimised SFE operating conditions was of good quality in terms of its fatty acid constituents.
The reported work demonstrates and discusses the effect of supercritical fluid density (pressure and temperature of supercritical fluid carbon dioxide) on particle size and distribution using the supercritical antisolvent (SAS) method in the purpose of drug encapsulation. In this study, paracetamol was encapsulated inside L-polylactic acid, a semicrystalline polymer, with different process parameters, including pressure and temperature, using the SAS process. The morphology and particle size of the prepared nanoparticles were determined by scanning electron microscopy and transmission electron microscopy. The results revealed that increasing temperature enhanced mean particle size due to the plasticizing effect. Furthermore, increasing pressure enhanced molecular interaction and solubility; thus, particle size was reduced. Transmission electron microscopy images defined the internal structure of nanoparticles. Thermal characteristics of nanoparticles were also investigated via differential scanning calorimetry. Furthermore, X-ray diffraction pattern revealed the changes in crystallinity structure during the SAS process. In vitro drug release analysis determined the sustained release of paracetamol in over 4 weeks.
Artemisia arborescens, Artemisia abyssinica, Pulicaria jaubertii, and Pulicaria petiolaris are fragrant herbs traditionally used in medication and as a food seasoning. To date, there are no studies on the use of supercritical fluids extraction with carbon dioxide (SFE-CO2) on these plants. This study evaluates and compares total phenolic content (TPC), antioxidant activity by DPPH• and ABTS•+, antibacterial, and anti-biofilm activities of SFE-CO2 extracts. Extraction was done by SFE-CO2 with 10% ethanol as a co-solvent. A. abyssinica extract had the highest extraction yield (8.9% ± 0.41). The GC/MS analysis of volatile compounds identified 307, 265, 213, and 201compounds in A. abyssinica, A. arborescens, P. jaubertii, and P. petiolaris, respectively. The P. jaubertii extract had the highest TPC (662.46 ± 50.93 mg gallic acid equivalent/g dry extract), antioxidant activity (58.98% ± 0.20), and antioxidant capacity (71.78 ± 1.84 mg Trolox equivalent/g dry extract). The A. abyssinica and P. jaubertii extracts had significantly higher antimicrobial activity and were more effective against Gram-positive bacteria. B. subtilis was the most sensitive bacterium. P. aeruginosa was the most resistant bacterium. P. jaubertii extract had the optimum MIC and MBC (0.4 mg/ml) against B. subtilis. All SFE-CO2 extracts were effective as an anti-biofilm formation for all tested bacteria at 1/2 MIC. Meanwhile, P. jaubertii and P. petiolaris extracts were effective anti-biofilm for most tested bacteria at 1/16 MIC. Overall, the results indicated that the SFE-CO2 extracts of these plants are good sources of TPC, antioxidants, and antibacterial, and they have promising applications in the industrial fields.
Recently natural polyphenol compounds (PCs) of plants, gained wide consideration of
scientists, companies and public people because of its unique pharmaceutical and
preservative benefits in the physiological system. They can prevent mortal and serious
diseases such as cancer, cardiovascular and Alzheimer. However, defining a suitable
source of PCs and their proper, economic and efficient extraction method are still a
challenge. The aim of this study was to review PCs as an important antioxidant, the
significance of pomegranate as a source of natural PCs and its application in meat and
meat product. This study also covers different types of PCs extraction methods such as
solid-liquid extraction (SLE) method as a conventional extraction which using Soxhlet
apparatus and several solvents and advanced methods such as microwave-assisted
extraction (MAE), supercritical fluid extraction (SFE), accelerated solvent extraction
(ASE), ultrasound-assisted extraction (UAE) and high hydrostatic pressure extraction
(HHPE). Simple and developed analytical method of PCs is also reviewed in the study.
SLE method is an easy and simple method but, it uses lots of chemicals and is not
suitable for all kinds of PCs extraction. UAE is using for quick extraction PCs, SFE is green
extraction method uses less solvent and have a good result but it needs high
technology. ASE method is a proper alternative for Soxhlet extraction method for its
quick result. MAE method has high extraction result but is not suitable for some
thermolabile PCs. Several parts of pomegranate showed antioxidant and antimicrobial
traits for shelf life extension of meat and meat product. Pomegranate peel is the
strongest antioxidant followed by pomegranate juice and seed. Pomegranate peel
prolonged chilled chicken meat shelf live up to three weeks.
In the present work, supercritical fluid extraction (SFE) with CO2 as solvent and EtOH/water (v/v) as co-solvent was optimised by applying 23 factorial experimental design for the extraction of betacyanins from red pitaya fruit (Hylocereus polyrhizus) peel. Three independent variables of pressure (20-30 MPa), temperature (40-60°C) and co-solvent concentration (10-20%) were chosen for response variables. With the 2 mL/min flow rate of CO2, the dynamic time of extraction was found to be 90 min. The linear effects of main factors and interactions were evaluated. The calculated response surface model for the pressure/temperature was found to be significant for all the dependent variables. At optimal condition of SFE, the response variables were assessed as maximum extraction yield of 4.09 ± 0.69%, total betacyanins content of 25.49 ± 1.54 mg/100 mL, redness (a*) of 58.18 ± 0.82, and IC50 (antioxidant activity) of 1.34 ± 0.12 mg/mL for the experimental peel extracts. The optimal levels of independent variables were validated for the experimental responses as predicted by the mathematical model. The reliability of this method was confirmed as there was no significant difference between experimental and predicted values. The HPLC-MS profile of betacyanins extract comprised of both acylated and non-acylated betacyanins constituents.
In order to improve the encapsulation process, a newly supercritical antisolvent process was developed to encapsulate fish oil using hydroxypropyl methyl cellulose as a polymer. Three factors, namely, temperature, pressure, and feed emulsion rate were optimized using response surface methodology. The suitability of the model for predicting the optimum response value was evaluated at the conditions of temperature at 60°C, pressure at 150 bar, and feed rate at 1.36 mL/min. At the optimum conditions, particle size of 58.35 μm was obtained. The surface morphology of the micronized fish oil was also evaluated using field emission scanning electron microscopy where it showed that particles formed spherical structures with no internal voids. Moreover, in vitro release of oil showed that there are significant differences of release percentage of oil between the formulations and the results proved that there was a significant decrease in the in vitro release of oil from the powder when the polymer concentration was high.
High-quality fish oil for human consumption requires low levels of toxic elements. The aim of this study was to compare different oil extraction methods to identify the most efficient method for extracting fish oil of high quality with the least contamination. The methods used in this study were Soxhlet extraction, enzymatic extraction, wet reduction, and supercritical fluid extraction. The results showed that toxic elements in fish oil could be reduced using supercritical CO2 at a modest temperature (60°C) and pressure (35 MPa) with little reduction in the oil yield. There were significant reductions in mercury (85 to 100%), cadmium (97 to 100%), and lead (100%) content of the fish oil extracted using the supercritical fluid extraction method. The fish oil extracted using conventional methods contained toxic elements at levels much higher than the accepted limits of 0.1 μg/g.
A preliminary study was conducted to study the effects of different types and concentrations of co-solvents based on yield, composition and antioxidants capacity of extract prior to optimization studies of supercritical fluid extraction (SFE) of Labisia pumila (locally referred to as 'kacip fatimah'). The following co-solvents were studied prior to the optimization of supercritical carbon dioxide (SC-CO2) technique: ethanol, water, methanol, as well as aqueous solutions of ethanol-water and methanol-water (50% and 70% v/v). By using the selected co-solvents, identification of phenolic acids (gallic acid, methyl gallate and caffeic acid) was determined by using High-Performance Liquid Chromatography (HPLC). Then, the antioxidant capacity was evaluated by using three different assays: total phenolic content (TPC), ferric reducing/antioxidant power (FRAP) and free radical-scavenging capacity of 2,2-diphenyl-1-picrylhydrazyl (DPPH). SC-CO2 with 70% ethanol-water co-solvent was superior in terms of a higher combination of phenolic compounds extracted and antioxidants capacity. Overall, SC-CO2 with co-solvent 70% ethanol-water technique was efficient in extracting phenolic compounds from L. pumila, and thus the usage of this solvent system should be considered for further optimization studies.
In recent years, astaxanthin is claimed to have a 10 times higher antioxidant activity than that of other carotenoids such as lutein, zeaxanthin, canthaxanthin, and β-carotene; the antioxidant activity of astaxanthin is 100 times higher than that of α-tocopherol. Penaeus monodon (tiger shrimp) is the largest commercially available shrimp species and its waste is a rich source of carotenoids such as astaxanthin and its esters. The efficient and environment-friendly recovery of astaxanthins was accomplished by using a supercritical fluid extraction (SFE) technique. The effects of different co-solvents and their concentrations on the yield and composition of the extract were investigated. The following co-solvents were studied prior to the optimization of the SFE technique: ethanol, water, methanol, 50% (v/v) ethanol in water, 50% (v/v) methanol in water, 70% (v/v) ethanol in water, and 70% (v/v) methanol in water. The ethanol extract produced the highest carotenoid yield (84.02 ± 0.8 μg/g) dry weight (DW) with 97.1% recovery. The ethanol extract also produced the highest amount of the extracted astaxanthin complex (58.03 ± 0.1 μg/g DW) and the free astaxanthin content (12.25 ± 0.9 μg/g DW) in the extract. Lutein and β-carotene were the other carotenoids identified. Therefore, ethanol was chosen for further optimization studies.
The Nigella sativa L. popularly referred to as black seeds are widely used as a form of traditional nutrition and medicine. N. sativa seeds were used for the extraction of their oil by way of supercritical fluid extraction (SFE) and cold press (CP) to determine the physicochemical properties, antioxidant activity, and thermal behavior. The GC-MS results showed the primary constituents in the Nigella sativa oil (NSO) were Caryophyllene (17.47%) followed by thymoquinone (TQ) (11.80%), 1,4-Cyclohexadiene (7.17%), longifolene (3.5%), and carvacrol (1.82%). The concentration of TQ was found to be 6.63 mg/mL for oil extracted using SFE and 1.56 mg/mL for oil extracted by CP method. The antioxidant activity measured by DPPH and the IC50 was 1.58 mg/mL and 2.30 mg/mL for SFE oil and cold pressed oil, respectively. The ferric reducing/antioxidant power (FRAP) activity for SFE oil and CP oil was 538.67 mmol/100 mL and 329.00 mmol/100 mL, respectively. The total phenolic content (TPC) of SFE oil was 160.51 mg/100 mL and 94.40 mg/100 mL for CP oil presented as gallic acid equivalents (GAE). This research showed that a high level of natural antioxidants could be derived from NSO extracted by SFE.
The extraction of phenolics from Citrus hystrix leaf was carried out using supercritical fluid extraction and was optimized using response surface methodology (RSM). The effects of CO2 flow rate, extraction pressure and extraction temperature on yield, total phenolic content and diphenyl-picrylhydrazyl-IC50 were evaluated and compared with ethanol extraction. The extraction pressure was the most significant factor affecting the yield, TPC and DPPH-IC50 of the extracts, followed by CO2 flow rate and the extraction temperature. The optimum conditions of pressure, CO2 flow rate and temperature were at 267 bars, 18 g/min and 50°C, respectively. The yield, TPC and DPPH-IC50 obtained were 5.06%, 116.53 mg GAE/g extract and IC50 of 0.063 mg/ml, respectively. These values were not significantly different (p
Kenaf (Hibiscus cannabinus) from the family Malvaceae, is a valuable fiber plant native to India and Africa and is currently planted as the fourth commercial crop in Malaysia. Kenaf seed oil contains alpha-linolenic acid, phytosterol such as β -sitosterol, vitamin E, and other antioxidants with chemopreventive properties. Kenaf seeds oil (KSO) was from supercritical carbon dioxide extraction fluid (SFE) at 9 different permutations of parameters based on range of pressures from 200 to 600 bars and temperature from 40 to 80°C. They were 200/40, 200/60, 200/80, 400/40, 400/60, 400/80, 600/40, 600/60, and 600/80. Extraction from 9 parameters of KSO-SFE was screened for cytotoxicity towards human colorectal cancer cell lines (HT29) and mouse embryonic fibroblast (NIH/3T3) cell lines using MTS assay. KSO-SFE at 600/40 showed the strongest cytotoxicity towards HT29 with IC50 of 200 µg/mL. The IC50 for NIH/3T3 was not detected even at highest concentration employed. Cell cycle analysis showed a significant increase in the accumulation of KSO-SFE-treated cells at sub-G1 phase, indicating the induction of apoptosis by KSO-SFE. Further apoptosis induction was confirmed by Annexin V/PI and AO/PI staining.
Syzygium campanulatum Korth is a plant, which is a rich source of secondary metabolites (especially flavanones, chalcone, and triterpenoids). In our present study, three conventional solvent extraction (CSE) techniques and supercritical fluid extraction (SFE) techniques were performed to achieve a maximum recovery of two flavanones, chalcone, and two triterpenoids from S. campanulatum leaves. Furthermore, a Box-Behnken design was constructed for the SFE technique using pressure, temperature, and particle size as independent variables, and yields of crude extract, individual and total secondary metabolites as the dependent variables. In the CSE procedure, twenty extracts were produced using ten different solvents and three techniques (maceration, soxhletion, and reflux). An enriched extract of five secondary metabolites was collected using n-hexane:methanol (1:1) soxhletion. Using food-grade ethanol as a modifier, the SFE methods produced a higher recovery (25.5%‒84.9%) of selected secondary metabolites as compared to the CSE techniques (0.92%‒66.00%).
This study was conducted to investigate and compare the fatty acids and tocopherols of lipid extracted from marine microalgae, Nannochloropsis oculata (NO) and Tetraselmis suecica (TS) using solvent extraction and supercritical fluid extraction (SFE). Fatty acids and tocopherols were determined in the extracted lipid as functions of the temperature (40, 80oC) and pressure (3000, 5000, 7000, 9000psi). Dichloromethane/methanol and hexane were the chosen conventional solvent for fatty acids and tocopherols extraction respectively. The results obtained showed that there were differences in the fatty acid composition of various lipid extracts of NO and TS. Extracts of NO were high in myristic acid (C14:0) (17-35%), palmitic acid (C16:0) (14-47%) and palmitoleic acid (C16:1) (11-42%) whereas extracts of TS were high in C14:0 (21-34%) and C16:0 (29-49%). Eicosapentaenoic acid (EPA) was detected only under certain SFE conditions in NO but was not detected in TS. α-, β- and γ-tocopherol were detected in various SFE extracts of NO but only α- and β-tocopherol were detected in TS. Hexane extraction of both NO and TS resulted in the detection of only α-tocopherol. In conclusion, the use of different extraction methods resulted in different compositions and concentrations of fatty acids and tocopherols in the microalgae studied.
In this study, optimization of supercritical reactive extraction directly from Jatropha seeds in a high pressure batch reactor using Response Surface Methodology (RSM) coupled with Central Composite Rotatable Design (CCRD) was performed. Four primary variables (methanol to solid ratio (SSR), reaction temperature, time and CO2 initial pressure) were investigated under the proposed constraints. It was found that all variables had significant effects towards fatty acid methyl esters (FAME) yield. Moreover, three interaction effects between the variables also played a major role in influencing the final FAME yield. Optimum FAME yield at 92.0 wt.% was achieved under the following conditions: 5.9 SSR, 300°C, 12.3 min and 20 bar CO2. Final FAME product was discovered to fulfil existing international standard. Preliminary characterization analysis proved that the solid residue can be burnt as solid fuel in the form of biochar while the liquid product can be separated as specialty chemicals or burned as bio-oil for energy production.
There are six tocol analogs present in palm oil, namely α-tocopherol (α-T), α-tocomonoenol (α-T₁), α-tocotrienol (α-T₃), γ-tocotrienol (γ-T₃), β-tocotrioenol (β-T₃) and δ-tocotrienol (δ-T₃). These analogs were difficult to separate chromatographically due to their similar structures, physical and chemical properties. This paper reports on the effect of pressure and injection solvent on the separation of the tocol analogs in palm oil. Supercritical CO₂ modified with ethanol was used as the mobile phase. Both total elution time and resolution of the tocol analogs decreased with increased pressure. Ethanol as an injection solvent resulted in peak broadening of the analogs within the entire pressure range studied. Solvents with an eluent strength of 3.4 or less were more suitable for use as injecting solvents.
Different extraction processes were employed to extract bioactive metabolites from Salacca zalacca flesh by a range of aqueous and organic solvents. The highest extraction yield was obtained by 50% ethanol extract of SE (73.18 ± 4.35%), whereas SFE_1 showed the lowest yield (0.42 ± 0.08%). All extracts were evaluated for in vitro α-glucosidase inhibitory activity, measured by their IC50 values in comparison to that of quercetin, the positive control (IC50 = 2.7 ± 0.7 μg/mL). The lowest α-glucosidase inhibitory activity was indicated by water extract of SE (IC50 = 724.3 ± 42.9 μg/mL) and the highest activity was demonstrated by 60% ethanol extract by UAE (IC50 = 16.2 ± 2.4 μg/mL). All extracts were analysed by GC-MS and identified metabolites like carbohydrates, fatty acids, organic acids, phenolic acids, sterols and alkane-based compounds etcetera that may possess the potential as α-glucosidase inhibitor and may attribute to the α-glucosidase inhibitory activity.
Candlenut oil was extracted using supercritical CO(2) (SC-CO(2)) with an optimization of parameters, by the response surface methodology. The ground candlenut samples were treated in 2 different ways, that is, dried in either a heat oven (sample moisture content of 2.91%) or dried in a vacuum oven (sample moisture content of 1.98%), before extraction. An untreated sample (moisture content of 4.87%) was used as a control. The maximum percentage of oil was extracted from the heat-oven-dried sample (77.27%), followed by the vacuum-oven-dried sample (74.32%), and the untreated sample (70.12%). At an SC-CO(2) pressure of 48.26 Mpa and 60 min of extraction time, the optimal temperatures for extraction were found to be 76.4 °C, 73.9 °C, and 70.6 °C for the untreated, heat-oven-dried, and vacuum-oven-dried samples, respectively. The heat-oven-dried sample contains the highest percentage of linoleic acid, followed by the untreated and vacuum-oven-dried samples. The antiradical activity of candlenut oil corresponded to an IC(50) value of 30.37 mg/mL.
Fish oil was extracted from the viscera of African Catfish using supercritical carbon dioxide (SC-CO(2)). A Central Composite Design of Response Surface methodology (RSM) was employed to optimize the SC-CO(2) extraction parameters. The oil yield (Y) as response variable was executed against the four independent variables, namely pressure, temperature, flow rate and soaking time. The oil yield varied with the linear, quadratic and interaction of pressure, temperature, flow rate and soaking time. Optimum points were observed within the variables of temperature from 35 °C to 80 °C, pressure from 10 MPa to 40 MPa, flow rate from 1 mL/min to 3 mL/min and soaking time from 1 h to 4 h. However, the extraction parameters were found to be optimized at temperature 57.5 °C, pressure 40 MPa, flow rate 2.0 mL/min and soaking time 2.5 h. At this optimized condition, the highest oil yields were found to be 67.0% (g oil/100 g sample on dry basis) in the viscera of catfish which was reasonable to the yields of 78.0% extracted using the Soxhlet method.