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1.
Supercritical carbon dioxide (SC-CO2) extraction of lipid from Scenedesmus sp. for biodiesel production was investigated and compared to conventional extraction methods. The effect of biomass pre-treatment prior to extraction and extracting conditions, namely pressure in the range of 200–500 bar, temperatures in the range of 35–65 °C and CO2 flow rate in the range of 1.38–4.02 g min−1, on SC-CO2 extraction yield and quality of lipid were investigated. Three levels full factorial design of experiments and response surface methodology was used to model the system. A second order polynomial model was developed and used to predict the optimum conditions. Scaling up to a laboratory larger scale was also tested. The results indicated that SC-CO2 extraction was superior to other extraction techniques, but exhibited significant variations in yield with changes in operating parameters. In the developed model, it was found that the linear and quadratic terms of the temperature, as well as the interaction with pressure had a significant effect on lipid yield; whereas, their effect on lipid quality was insignificant. The best operating conditions, in the tested range, were 53 °C, 500 bar and 1.9 g min−1, in which lipid extraction yield of 7.41% (dry weight basis) was obtained. Negligible differences were observed when the fatty acid composition of SC-CO2 extracted lipid was compared to that extracted by the conventional methods. At the optimum conditions, SC-CO2 extraction was successfully scaled-up by eight-folds and the extracted lipid yield dropped by 16%. 相似文献
2.
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. 相似文献
3.
《The Journal of Supercritical Fluids》2009,50(3):345-350
As a novel technique, supercritical CO2 (SC-CO2) extraction enhanced by ultrasound was applied to the extraction of lutein esters from marigold and the extraction curves were described by Sovová model. The mass transfer coefficient in the solid phase (ks) increased from 3.1 × 10−9 to 4.3 × 10−9 m/s due to ultrasound. The effect of extraction parameters including particle size of matrix, temperature, pressure, flow rate of CO2, and ultrasonic conditions consisting of power, frequency and irradiation time/interval on the yield of lutein esters were investigated with single factor experiments. The results showed that the yield of lutein esters increased significantly with the presence of ultrasound (p < 0.05). The maximal yield of lutein esters (690 mg/100 g) was obtained for a particle size fraction of 0.245–0.350 mm, extraction pressure of 32.5 MPa, temperature of 55 °C and CO2 flow rate of 10 kg/h with ultrasonic power of 400 W, ultrasonic frequency of 25 kHz and ultrasonic irradiation time/interval of 6/9 s. 相似文献
4.
The objective of this work was to determine the economic feasibility of large-scale operations of supercritical fluid extraction (SFE) for the recovery of phenolics using grape bagasse from Pisco residues. Experimental data were used to estimate the extraction kinetic parameters, as well as the cost of manufacturing the extracts. Experimental data were obtained using supercritical CO2 containing 10% ethanol (w/w) at 313 K and 20–35 MPa. The supercritical CO2/ethanol extraction process produced extracts with higher concentrations of phenolics than extracts produced using conventional techniques. The compounds identified in the extracts were syringic, vanillic, gallic, p-hydroxybenzoic, protocatechuic and p-coumaric acids, as well as quercetin. An evaluation of the economics of the process indicated the feasibility of an industrial SFE plant with a capacity of 0.5 m3 for producing an extract with an expected phenolics concentration of approximately 23 g/kg of extract at an estimated cost of manufacturing of US$ 133.16/kg. 相似文献
5.
《The Journal of Supercritical Fluids》2007,40(3):330-337
In this study, the extraction of jojoba seed oil obtained from jojoba seed using both supercritical CO2 and supercritical CO2+ethanol mixtures was investigated. The recovery of jojoba seed oil was performed in a green and high-tech separation process. The extraction operating was carried out at operating pressures of 25, 35 and 45 MPa, operating temperatures of 343 and 363 K, supercritical fluid flow rates of 3.33 × 10−8, 6.67 × 10−8 and 13.33 × 10−8 m3 s−1, entrainer concentrations of 2, 4 and 8 vol.%, and average particle diameters of 4.1 × 10−4, 6.1 × 10−4, 8.6 × 10−4 and 1.2 × 10−3 m. It was found that a green chemical modifier such as ethanol could enhance the solubilities, initial extraction rate and extraction yield of jojoba seed oil from the seed matrix as compared to supercritical CO2. In addition, it was found that the solubility, the initial extraction rate and the extraction yield depended on operating pressure and operating temperature, entrainer concentration, average particle size and supercritical solvent flow rate. The solubility of jojoba seed oil and initial extraction rate increased with temperature at the operating pressures of 35 and 45 MPa and decreased with increasing temperature at the operating pressure of 25 MPa. Furthermore, supercritical fluid extraction involved short extraction time and minimal usage of small amounts entrainer to the CO2. About 80% of the total jojoba seed oil was extracted during the constant rate period at the pressure of 35 and 45 MPa. 相似文献
6.
Ethanol modified supercritical carbon dioxide (SC-CO2) extraction of flavonoids from Momordica charantia L. fruits and its antioxidant activity were performed. The influences of parameters such as temperature, extraction time and pressure on the yield of flavonoids were investigated. The antioxidant activities of flavonoids were assessed by means of 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical-scavenging assay and β-carotene bleaching test. The experimental data obtained indicated that pressure, temperature and time had significant effect on the extraction yield. The optimum extraction conditions, determined by the 3D response surface and contour plots derived from the mathematical models, were as follows: extraction temperature 46 °C, pressure 33.4 MPa, and extraction time 53.2 min. Under these conditions, the experimental value was 15.47 mg/g, which was well matched with value predicted by the model. The antioxidant activity of flavonoids obtained by ethanol modified SC-CO2 extraction method had higher antioxidant activity than the flavonoids extracted by conventional solvent extraction (CSE) method. The DPPH radical-scavenging ability of flavonoids obtained by ethanol modified SC-CO2 extraction method reached to 96.14 ± 1.02%, equivalent to the clearance rate of ascorbic acid at 1.2 mg/mL. Results indicated that ethanol modified SC-CO2 extraction was a suitable approach for the selective extraction of flavonoids from M. charantia L. 相似文献
7.
Melia azedarach L. is a plant with wide use in folk medicine since it contains many bioactive compounds of interest. The present study aimed to extract bioactive compounds from M. azedarach fruits by a sequential process in fixed bed using various solvent mixtures. Extractions were performed at 50 °C and 300 bar in four sequential steps using supercritical CO2 (scCO2), scCO2/ethanol, pure ethanol, and ethanol/water mixture as solvents, respectively. The efficacy of the extraction process was evaluated by extraction yield and kinetics, and analysis of extracts by: (1) thin layer chromatography (TLC), (2) phenolics content, (3) reduction of surface tension of water, (4) gas chromatography (GC–MS), (5) electrospray ionization mass spectrometry (ESI–MS) and (6) antiviral activity. The overall extraction yield reached 45% and TLC analysis showed extracts with different composition. extract obtained from CO2/ethanol mixture (SCEE) exhibited the greatest ability to reduce surface tension of water from 72.4 mN m−1 [1] of pure water to 26.9 mN m−1 of an aqueous solution of 40 g L−1. The highest phenolics contents were observed in both the hydroalcoholic extract and scCO2/ethanolic extract. Volatile oils were not detected in the supercritical extracts by GC–MS. MS analyses identified the fatty acids: linoleic, palmitic and myristic acid in the supercritical extract (SCE), and the phenolics: caffeic acid and malic acid in the other extracts. In addition, SCE and SCEE extracts showed significant inhibition percentage against Herpes Simplex Virus Type 1. The extraction process proposed in the present study produced extracts with significant potential for application in food and pharmaceutical industries. 相似文献
8.
Supercritical carbon dioxide (SC-CO2) extraction of grape marc was studied using water (W) and ethanol (EtOH) as co-solvent at 15% (w/w), 100 and 200 MPa, and 313.15, 323.15 and 333.15 K to analyze their influence upon total phenols of the extracts. The overall extraction curves were determined and suggested 10 MPa and 313.15 K as the best operating conditions for SC-CO2 + 15%W extraction, and 10 MPa and 333.15 K for SC-CO2 + 15% EtOH. The phenolic yields obtained were 63.4 g/kg of extract for SC-CO2 + 15% W and 38.8 g/kg of extract for SC-CO2 + 15% EtOH. An alternative method combining Sc-CO2 + 15% W extraction, followed by SC-CO2 + 15% EtOH was tested. This procedure provided the best results allowing to obtain the highest phenolic yield (68.0 g/kg of extract), phenol content (733.6 mg GAE/100 g DM), proanthocyanidins concentration (572.8 mg catechin/100 g DM) and antioxidant activity (2649.6 mg α-tocopherol/100 g DM). SC-CO2 methods were compared with methanol extraction. 相似文献
9.
Supercritical Fluid Extraction (SFE) was used to obtain myrtle leaf extracts, and to study the antioxidant capacity (AOC) and in vitro antimicrobial activity of those extracts. To optimize the SFE operational conditions, the response surface methodology (RSM) was adopted. The parameters studied were: pressure (P), within the range 10 to 30 MPa; temperature (T), between 35 °C and 60 °C and supercritical carbon dioxide (SCCO2) flow rate (Q) within the range 0.15 to 0.45 kg h−1. The results show a good fit to the proposed model and the optimal conditions obtained (23 MPa, 45 °C, and SCCO2 flow rate of 0.3 kg h−1) were within the experimental range. The predicted values agreed with experimental ones, thus indicating the suitability of the RSM model for the optimization of the extraction conditions being investigated. With those values remaining constant, ethanol as a co-solvent was then studied. There was an observed rise in AOC as the amount of ethanol increased, within the range studied (0–30 wt% ethanol). The extract with the highest AOC was tested for its antimicrobial activity against gram-positive and gram-negative bacteria. The minimum inhibitory concentration (MIC) values obtained showed significant inhibitory effect against gram-positive bacteria. 相似文献
10.
Echinacea species is provided as dietary supplements for various infectious and immune related disorders and has a potential role in cancer prevention. The aim of this study was to optimize the extraction of total flavonoids using different extraction methods and investigate the cytotoxic effects on various cancer cell lines (CaCo-2, MCF-7, A549, U87MG, and HeLa) and VERO (African green monkey) as a non-cancerous cell line. Box-Behnken statistical design was used to evaluate the effect of pressure (100–200 bar), temperature (40–80 °C) and ethanol as co-solvent (6–20 wt%) at a flow rate of 15 g/min for 60 min in supercritical CO2 extraction and the effect of temperature (60–100 °C), time (5–15 min) and power (300–900 W) in microwave-assisted extraction. Optimum extraction conditions were elicited as 300 bar, 80 °C and 13% co-solvent yielding 0.472 mg rutin equivalent total flavonoids/g extract in SC-CO2 extraction, whereas 60 °C, 10 min and 300 W yielded the highest (0.202 mg rutin equivalent) total flavonoids in microwave-assisted extraction. Additional trials with subcritical water (0.022 mg/g) and Soxhlet extraction with methanol (0.238 mg/g) yielded lower flavonoid contents. The exposures upto 50 μg/ml of extracts revealed no significant inhibition on the proliferation of both tested cancer cells and healthy VERO cells. 相似文献
11.
Coupling supercritical CO2 (SC-CO2) extraction with membrane separation leads to energy savings by recycling CO2 at supercritical state while separating extract components. However, high pressure operating conditions may cause physicochemical and morphological changes in polymer membranes, which in turn can adversely affect membrane performance. In this study, the effect of different flux (50 and 200 kg/m2 h), temperature (40 and 80 °C) and time (0–8 h) levels were investigated at 120 bar on two commercial reverse osmosis membranes, AK and SG using contact angle, ATR-FTIR and FE-SEM measurements. Contact angle of AK increased substantially with high flux and high temperature processing unlike SG. The peaks assigned to N–H and carbonyl groups at 1541, 1609 and 1663 cm−1 showed the highest decrease in absorbance with high flux processing while high temperature was more effective on O–H groups between 2700 and 3700 cm−1. AK membrane exhibited the formation of bead-like structures at different processing times and conditions. The effect of SC-CO2 processing on the membranes varied depending on their chemical structure, which is important to understand for further process development. 相似文献
12.
《中国化学工程学报》2014,22(11-12):1314-1321
Caffeic acid phenethyl ester (CAPE) is a natural and rare ingredient with several biological activities, but its industrial production using lipase-catalyzed esterification of caffeic acid (CA) and 2-phenylethanol (PE) in ionic liquids (ILs) is hindered by low substrate concentrations and long reaction time. To set up a high-efficiency bioprocess for production of CAPE, a novel dimethyl sulfoxide (DMSO)–IL co-solvent system was established in this study. The 2% (by volume) DMSO–[Bmim][Tf2N] system was found to be the best medium with higher substrate solubility and conversion of CA. Under the optimum conditions, the substrate concentration of CA was raised 8-fold, the reaction time was reduced by half, and the conversion reached 96.23%. The kinetics follows a ping-pong bi-bi mechanism with inhibition by PE, with kinetic parameters as follows: Vmax = 0.89 mmol · min− 1 · g− 1, Km,CA = 42.9 mmol · L− 1, Km,PE = 165.7 mmol · L− 1, and Ki,PE = 146.2 mmol · L− 1. The results suggest that the DMSO co-solvent effect has great potential to enhance the enzymatic synthesis efficiency of CAPE in ILs. 相似文献
13.
《The Journal of Supercritical Fluids》2009,50(3):323-329
Supercritical carbon dioxide (SC-CO2) was employed to extract omega-3 rich oil from Sacha inchi (Plukenetia volubilis L.) seeds and partially defatted cake. For ground seeds, the supercritical extraction was carried out at temperatures of 40, 50 and 60 °C and pressures of 300 and 400 bar, and for the cold pressed partially defatted cake, the extraction was carried out with 300 bar at 40 °C and with 400 bar at 60 °C. The global extraction yields (X0), oil solubility, fatty acid composition of the oil and tocopherol content were determined. The seed samples used in this work contained 54.3% oil, of which 50.5% was linoleinc acid (ω-3). The maximum extraction recovery for the seeds as 92% at 400 bar and 60 °C, but on one occasion a recovery of 99.1% oil was obtained when cold pressed extraction was employed, followed by supercritical extraction at 400 bar and 60 °C. A high tocopherol content of about 2–3 g/kg of oil was obtained. 相似文献
14.
Saponins are surfactants that reduce the surface tension of aqueous solutions, besides having pharmacological actions. In order to extract and fractionate saponins from Pfaffia glomerata roots and Hebanthe eriantha roots using supercritical technology, fractionated extracts were obtained from a sequential process in fixed bed using supercritical CO2 (scCO2), ethanol, and water as solvents. All extractions were carried out in four sequential steps, at 50 °C and 300 bar. In the first step, pure scCO2 was used as solvent, while (a) scCO2/etanol (70:30, w/w); (b) ethanol, and (c) ethanol/water (70:30, v/v) were used as solvents in the three subsequent steps. The extracts were analyzed by thin layer chromatography (TLC) and surface tension. The extraction yields of the four steps were 0.16, 0.55, 1.00, and 6.90% for P. glomerata roots, and 0.17, 0.58, 0.89, and 28% for H. eriantha roots, showing a predominance of high polarity compounds in these species. TLC analysis showed that the extraction process was selective according to the polarity of the solvent, and provided extracts containing different saponins, except for scCO2 extraction. The extracts from the extraction using ethanol + scCO2 (Step 2) showed the greatest ability to reduce the surface tension of water from 72 mN m−1 (pure water) to 25 mN m−1, suggesting that this step was the best for extraction of less polar saponins in the extracts. The critical micelle concentration (CMC) values were approximately 2 and 8 g L−1 for P. glomerata and H. Eriantha, respectively. These results confirmed the efficacy of the extraction process under study. 相似文献
15.
Supercritical fluid extraction from freeze-dried Eruca sativa leaves is assessed with the aim of studying the feasibility to obtain bioactive enriched fractions containing different classes of valuable compounds. Total extraction yields and compositions using pure CO2 and CO2 + selected co-solvents are compared. Overall extraction curves, fitted by the model of broken and intact cells developed by Sovová, are reported and the influence of the main parameters that affect the extraction process is analysed. The extract with the highest content in glucosinolates and phenols was collected at 30 MPa and 75 °C using 8% (w/w) of water with respect to the CO2 flow rate, whereas the fraction richest in lipids was obtained using 8% (w/w) of ethanol as co-solvent at 45 °C and 30 MPa. A process including a first step with supercritical CO2 extraction using water as co-solvent followed by a second step, where a fraction rich in lipids is extracted using ethanol as co-solvent, is proposed. SCCO2 results are compared with Soxhlet and other methods that combine organic solvents with ultrasounds. 相似文献
16.
《The Journal of Supercritical Fluids》2010,51(3):203-209
The solubility of highly selective and potent third-generation aromatase inhibitors includes the non-steroidal agents letrozole and anastrozole and the steroid exemestane in supercritical carbon dioxide (SC-CO2) has been investigated. The experiments were carried out using the simple and static method at pressures in the range of 12.1–35.5 MPa and temperatures ranging from 308 to 348 K. The mole fraction solubilities ranged from 0.22 × 10−5 to 1.88 × 10−4. Solubility data were correlated using six empirical models (Chrastil model, dV–A model, K–J model, Bartle model, Yu model and Gordillo model). The results showed that these models can be applied to satisfactory solubility predictions at different pressures and temperatures. A comparison among the six models revealed that the K–J, and Gordillo models gave much better correlations of the solubility data with an average absolute relative deviation (AARD%) ranging from 0.2 to 2.3 and from 1.6 to 2.5%, respectively. Using the correlation results, the heat of drug–CO2 solvation and that of drug vaporization was separately approximated in the range of −17.3 to −17.5 and 93.0–112.1 kJ mol−1. 相似文献
17.
The reported work aimed at the optimization of operating conditions of the supercritical fluid extraction (SFE) of spent coffee grounds (SCG) using pure or modified CO2, with particular emphasis on oil enrichment with diterpenes like kahweol, cafestol and 16-O-methylcafestol. The analysis comprised the application of Box–Behnken design of experiments and response surface methodology, and involved three operating variables: pressure (140–190 bar), temperature (40–70 °C) and cosolvent (ethanol) addition (0–5 wt.%). The best conditions to maximize total extraction yield are 190 bar/55 °C/5 wt.% EtOH, leading to 11.97% (goil/100 gSCG). In terms of the concentration of diterpenic compounds in the supercritical extracts, the best operating conditions are 140 bar/40 °C/0 wt.% EtOH, providing 102.90 mg g−1oil. The measurement of extraction curves near optimized conditions (140 bar/55 °C/0 wt.% EtOH and 190 bar/55 °C/0 wt.% EtOH) confirmed the trends of the statistical analysis and revealed that SFE enhances diterpenes concentration by 212–410% at the expenses of reducing the extraction yield between 39% and 79% in comparison to n-hexane extraction. 相似文献
18.
The combined effect of supercritical carbon dioxide (SC-CO2) and high power ultrasound (HPU) on the inactivation kinetics of Escherichia coli, Saccharomyces cerevisiae and pectin-methyl esterase (PME) in orange juice was studied in order to select models that can predict their inactivation behaviour based on process parameters. Experiments were performed at different temperatures (31–41 °C, 225 bar) and pressures (100–350 bar, 36 °C). The inactivation rate of E. coli, S. cerevisiae and PME increased with pressure and temperature during SC-CO2 + HPU treatments. The SC-CO2 + HPU inactivation kinetics of E. coli, S. cerevisiae and PME were represented by models that included temperature, pressure and treatment time as variables, based on the Biphasic, the Peleg Type B, and the fractional models, respectively. The HPU-assisted SC-CO2 batch system permits the use of mild process conditions and treatment times that can be even shorter than those of continuous SC-CO2 systems. 相似文献
19.
In this study, the essential oil of aerial parts of a species of a plant called Smyrnium cordifolium Boiss (SCB) was extracted by supercritical CO2. The essence was analyzed by the method of GC/MS. Design of experiments was carried out with response surface methodology by Minitab 16 software to optimize four operating variables of supercritical carbon dioxide (SC-CO2) extraction (pressure, temperature, CO2 flow rate and extraction dynamic time). This is the first report announcing optimization of the operation of supercritical extraction of SCB in laboratorial conditions. Optimizing process was done to achieve maximum yield extraction. Independent variables were dynamic time (td), pressure (P), temperature (T) and flow rate of SC-CO2 (Q) in the range of 30–150 min, 10–30 MPa, 40–60 °C and 0.5–1.7 ml/min, respectively. The experimental optimal recovery of essential oil (0.8431, w/w%) was obtained at 13.43 MPa, 40 °C, 150 min (dynamic) and 1.7 ml/min (CO2 flow rate). 相似文献
20.
Near-supercritical and supercritical CO2 was used to extract low-molar-mass phenolics and lipophilic compounds from Pinus pinaster wood. Extraction of samples containing sapwood and knotwood was carried out at 1025 MPa and 3050 °C to assess the influence of the operational conditions on the yields of total extracts and phenolics, as well as on the radical scavenging capacity of extracts. The use of ethanol as a co-solvent increased both the extraction yields and the concentration of phenolics in extracts. Operating under selected conditions (25 MPa, 50 °C, 10% ethanol), the extraction yield accounted for 4.1 wt% of the oven-dry wood. The extracts contained up to 7.6 g of phenolic compounds (measured as gallic acid equivalents) per 100 g extract, and showed one third of the radical scavenging capacity of Trolox. Native resin acids accounted for about 24 g per 100 g extracts, whereas flavonoids, lignans, stilbenes and juvabiones were found at lower proportions. 相似文献