Extraction and identification of proanthocyanidins from grape seed (Vitis Vinifera) using supercritical carbon dioxide

In this study, supercritical carbon dioxide extraction of proantocyanidins (PRCs) was performed and the effect of different pressure, temperature and ethanol percentage was investigated. High performance liquid chromatography was used for the analysis of the compounds and it was found that the most effective parameter on the extraction was the amount of the ethanol percentage. Each compound was extracted from grape seeds at their maximum level when different parameters were used which was probably because of their different polarities. Gallic acid (GA), epigallocatechin (EGC) and epigallocatechingallate (EGCG) were extracted at their maximum level when the 300 bar 50 °C and 20% of ethanol was used. The maximum amount of catechin (CT) and epicatechin (ECT) were obtained when 300 bar 30 °C and 20% of ethanol was used for extraction, and 250 bar, 30 °C and 15% of ethanol was needed to extract highest amount of epicatechingallate (ECG).     

Extraction of rice brain oil using supercritical carbon dioxide and propane

Extraction of rice bran lipids was performed using supercritical carbon dioxide (SC−CO₂) and liquid propane. To provide a basis for extraction efficiency, accelerated solvent extraction with hexane was performed at 100°C and 10.34 MPa. Extraction pressure was varied for propane and SC−CO₂ extractions. Also, the role of temperature in SC−CO₂ extraction efficiency was investigated at 45,65, and 85°C. For the SC−CO₂ experiments, extraction efficiencies were proportional to pressure and inversely proportional to temperature, and the maximal yield of oil achieved using SC−CO₂ was 0.222±0.013 kg of oil extracted per kg of rice bran for conditions of 45°C and 35 MPa. The maximal yield achieved with propane was 0.224±0.016 kg of oil per kg of rice bran at 0.76 MPa and ambient temperature. The maximum extraction efficiencies of both SC−CO₂ and propane were found to be significantly different from the hexane extraction baseline yield, which was 0.261±0.005 kg oil extracted per kg of rice bran. A simulated economic analysis was performed on the possibility of using SC−CO₂ and propane extraction technologies to remove oil from rice bran generated in Mississippi. Although the economic analysis was based on the maximal extraction efficiency for each technology, neither process resulted in a positive rate of return on investment.     

超临界CO_2流体萃取植物油的实验研究

建立了一套超临界流体萃取实验装置,就大豆和花生两种植物油超临界流体萃取进行了较为详细的实验研究.在探讨了压力、温度、颗粒度、空隙率以及时间等对萃取率的影响之后,获得了指导实际生产的最佳工艺参数条件.     

超临界CO_2萃取大豆油的实验研究

采用超临界CO2 萃取技术进行了大豆油的萃取实验。在压力为 2 0～ 30MPa、温度为 30 8～ 32 3K的范围内 ,考察了萃取压力、萃取温度、流体流量和物料预处理方式等条件对出油率的影响。在本文实验范围内 ,大豆油的最佳萃取工艺条件为 :压力 30MPa ,温度 313K ,物料状态为约 0 .4mm厚的大豆片。流体流量只影响萃取速率 ,而不影响最终的出油率     

Chamomile extraction with supercritical carbon dioxide: Mathematical modeling and optimization

Supercritical fluid extraction of chamomile using carbon dioxide was investigated in the current study. A model that accounts for both particle and fluid phase was presented for the supercritical extraction. The distribution coefficient of chamomile extract, between solid and solvent has been determined using genetic algorithm method. The model was solved numerically and was successfully validated with experimental data. The model was found to give superior results when compared to experimental data. The effect of particle diameter on extraction yield was investigated using the proposed model. Using genetic algorithm optimization technique 313.15 K and 20 MPa were found as the optimum temperature and pressure, respectively.     

Guava (Psidium guajava L.) seed oil obtained with a homemade supercritical fluid extraction system using supercritical CO2 and co-solvent

In this work we designed and built a homemade supercritical fluid extraction (HM-SFE) system, in which pure CO₂ and CO₂ with co-solvents were used. The HM-SFE was made by means of thermal dilatation-contraction (TDC). This HM-SFE system was used for obtaining guava (Psidium guajava L.) seed oil, using supercritical CO₂ adding ethanol as co-solvent (CO₂ SC/EtOH), extractions were performed at 313 K and different pressures (10, 20 and 30 MPa), each one in four stages of 30 min, the extract with higher yield was subjected to transesterification and high-resolution gas chromatography (HRGC) analysis. The highest extraction yield was obtained at 30 MPa (17.30% w/w), this yield was higher than one observed in a previous work using SC-CO₂, and near to the one obtained by Soxhlet extraction (20.2% w/w). HRGC enabled the identification of components of the derivatized extract as methyl esters of palmitic, oleic, linoleic, and stearic fatty acids. The results obtained with HM-SFE system was compared with a commercial SFE system, obtained very similar results. In this work was possible to construct a low cost and simple manner HM-SFE system which was employed for obtaining guava seed oil, using CO₂ SC/EtOH.     

Fractionation of thyme (Thymus vulgaris L.) by supercritical fluid extraction and chromatography

Supercritical fluid chromatography (SFC) was employed to fractionate thyme (Thymus vulgaris L.) extracts, which were obtained by supercritical carbon dioxide extraction of thyme leaves. First, different supercritical extracts were produced at 313 K and at different pressures (15, 30 and 40 MPa). Thymol, a monocyclic terpenoid with recognized antiseptic, analgesic and anti-inflammatory properties, was identified and quantified in the different samples by GC-MS. Then, the supercritical extracts were fractionated by semi-preparative SFC, and different conditions such as pressure, temperature and amount of cosolvent (ethanol) employed were studied. Around a two fold increase of thymol was achieved at 15 MPa, 50 °C and 3% ethanol cosolvent, recovering 97% of the monocyclic terpenoid extracted.     

Extraction of pomegranate seed oil using subcritical propane and supercritical carbon dioxide

Extraction of oil from pomegranate seeds as a waste product of the juice industry using supercritical carbon dioxide and subcritical propane was studied in this work. The influence of the main operating conditions of extraction, namely, the temperature and pressure of extraction on the oil extraction yield and the correspondent fatty acid profile were analyzed and reported here. Soxhlet extraction with n-hexane was done for comparison with supercritical extraction resulting in a maximum yield of oil of 22.31 wt %. Supercritical carbon dioxide and subcritical propane extracted up to 58.53% (corresponding to maximum yield of 13.06 wt %) and 76.73% (corresponding to maximum yield of 17.12 wt %) of the total amount of pomegranate seed oil as measured using Soxhlet extraction, respectively. Results indicated that the subcritical propane is a suitable and selective solvent for the extraction of the pomegranate seed oil in function of smaller times and pressures employed compared to carbon dioxide extraction. The fatty acid composition of the extracted oil showed the presence of fatty acids of C₁₆, C₁₈, C₂₀, C₂₂, and C₂₄ carbon chains. Punicic (C_18.3) was the major fatty acids and comprise up to 70% of the total fatty acid content of the extracted oil among all samples. Finally, Lack??s plug flow model as developed by Sovova was applied to both extraction systems and a good agreement with the experimental results was obtained.     

Evaluation of density-based models for the solubility of solids in supercritical carbon dioxide and formulation of a new model

Many models have been developed to calculate supercritical solubility behavior and most can be either a semi-empirical relationship or based on an equation of state. In this work, density-based, semi-empirical models were evaluated in terms of their ability to accurately correlate solid solubility in supercritical carbon dioxide. The models considered were the methods of Chrastil, del Valle and Aguilera, Adachi and Lu, Méndez-Santiago and Teja, and Bartle. Six binary systems (solid + supercritical carbon dioxide), each with three isotherms, were selected for this evaluation. The average error was calculated for all 18 isotherms with each of the models evaluated. The solid compounds used in this study were naphthalene, anthracene, fluorene, hydroquinone, 1,5-naphthalenediamine, and cholesterol. The solubility data were obtained from literature. Of the previously mentioned models, the Adachi-Lu and del Valle-Aguilera equations provided, in general, lower average error than the other models. Since the Adachi-Lu equation and the del Valle-Aguilera equation correct for different effects, a new model is proposed in this work as a combination of the previous two methods. The proposed equation provided the least overall average error compared to all other models considered in this study. The new model is particularly useful when the reduced density of the solvent is below 1 where previous models tend to fail. This work also emphasizes on the advantages of expressing density-based models in dimensionless form to avoid dimensional inconsistencies in Chrastil-type models. One of the benefits, for example, is that parameters obtained by different authors can be readily compared, regardless of the units used.     

Supercritical extraction of Hypericum caprifoliatum using carbon dioxide and ethanol + water as co-solvent

Hypericum caprifoliatum is a natural source of phloroglucinol derivatives such as hyperbrasilol B, uliginosin B and japonicin A, compounds with pharmaceutical interest due to principally their antidepressant properties. This work studies supercritical fluid extraction to obtain non-volatile compounds from the aerial parts of H. caprifoliatum as well as the influence of the co-solvent as agent of process intensification. The experimental procedures were carried out in a pilot unity. The mathematical simulation of the experimental data was performed by mean of three mathematical models aiming to promote the improvement of the knowledge about this technology. The feasibility of the mathematical model was investigated by mean of fitting of the experimental data obtained. The co-solvents tested were ethanol, water, and water–ethanol mixtures.     

Supercritical carbon dioxide extraction of oil from Mexican chia seed (Salvia hispanica L.): Characterization and process optimization

Supercritical carbon dioxide (SC-CO₂) was employed to extract oil rich in omega-3 fatty acids (FAs) from chia seeds, and the physicochemical properties of the oil were determined. A central composite rotatable design was used to analyze the impact of temperature (40 °C, 60 °C and 80 °C), pressure (250 bar, 350 bar and 450 bar) and time (60 min, 150 min and 240 min) on oil extraction yield, and a response surface methodology (RSM) was applied. The extraction time and pressure had the greatest effects on oil. The highest oil yield was 92.8% after 300 min of extraction time at 450 bar. The FA composition varied depending on operating conditions but had a high content of α-linolenic acid (44.4-63.4%) and linoleic acid (19.6-35.0%). The rheological evaluation of the oils indicated a Newtonian behavior. The viscosity of the oil decreased with the increase in temperature following an Arrhenius-type relationship.     

Near critical carbon dioxide extraction of Anise (Pimpinella Anisum L.) seed: Mathematical and artificial neural network modeling

In the current study, two models for estimating essential oil extraction yield from Anise, at high pressure condition, were used: mathematical modeling and artificial neural network (ANN) modeling. The extractor modeled mathematically using material balance in both fluid and solid phases. The model was solved numerically and validated with experimental data. Since the potential of near critical extraction is of consider able economic significance, a multi-layer feed forward ANN has been presented for accurate prediction of the mass of extract at this region of extraction. According to the network's training, validation and testing results, a three layer neural network with fifteen neurons in the hidden layer is selected as the best architecture for accurate prediction of mass of extract from Anise seed. Finally, the influence of pressure and solvent flow rate on the extraction kinetics was studied using ANN model and the optimum pressure range has been determined.     

Mathematical modeling and genetic algorithm optimization of clove oil extraction with supercritical carbon dioxide

In the present study, a mathematical modeling for extraction of oil from clove buds using supercritical carbon dioxide was performed. Mass transfer is based on local equilibrium between solvent and solid. The model was solved numerically, and model estimation was validated using experimental data. For optimization, the clove oil equilibrium constant between solid and supercritical phase was determined by a theoretical method using fugacity concept, consequently the genetic algorithm for obtaining optimal operational conditions was used. The optimal conditions which obtained the highest amount of clove oil were pressure of 10 MPa and temperature of 304.2 K.     

超临界CO2萃取的研究与应用

介绍了超临界流体的特性及其萃取的基本原则,讨论了超临界流体萃取技术的优点,评述了超临界CO2的特点,概述了国内外超临界CO2萃取技术在医药,食品,香料,石油化工以及环境保护等领域的开发及应用。     

Experimental optimization and mathematical modeling of supercritical carbon dioxide extraction of essential oil from Pogostemon cablin

The supercritical carbon dioxide extraction was applied to obtain essential oil from Pogostemon cablin in this work. Effect of extraction parameters including temperature, pressure, extraction time and particle size on extraction yield was investigated, and the response surface methodology with a Box-Behnken Design was used to achieve the optimized extraction conditions. The maximum yield of essential oil was 2.4356% under the conditions of extraction temperature 47℃, pressure 24.5 MPa and extraction time 119 min. Moreover, based on the Brunauer-Emmett-Teller theory of adsorption, a mathematical modeling was performed to correlate the measured data. The model shows a function relationship between extraction yield and time by a simple equation with three significantly adjustable parameters. These model parameters have been optimized through simulated annealing algorithm. The predicted data from the mathematical model show a good agreement with the experimental data of the different extraction parameters.     

Partial oxidation of propane in compressed carbon dioxide using CoOx/SiO2 catalysts

The application of compressed carbon dioxide as an alternative reaction medium was investigated for the heterogeneously catalysed partial oxidation of propane. The catalytic tests were performed in a stirred batch as well as in a continuous flow reactor at 553–623 K, 2.6–11.3 MPa and a CO₂:synthetic air:propane molar ratio of 94–124:4–7:1 using precipitated CoO_x/SiO₂ (2.4–3.7 wt.% Co) catalysts. In addition, the critical temperature and pressure of the reaction mixture were determined by the opalescence method in a high-pressure optical cell. The catalytic experiments revealed a significantly higher cumulative oxygenate selectivity (i.e. acetic acid, methanol, acrolein, acetone) with increasing pressure. It is supposed that the formed oxygenates were removed more easily from the catalyst surface without being totally oxidised due to the higher solvent power of the dense CO₂ in the supercritical phase.     

Extraction of pomegranate (Punica granatum L.) seed oil using superheated hexane

Superheated hexane extraction (SHHE), Soxhlet extraction and cold pressing method were compared for the extraction of pomegranate seed oil. The extraction efficiencies of different temperatures (80, 100, 120 °C), mean particle sizes (0.25, 0.50 and 1.00 mm), and n-hexane flow rates (0.5, 1.0 and 2.0 mL/min) were investigated. The fatty acids profile of the seed oils were quantitatively determined by GC-FID. The optimum extraction temperature, mean particle size, and flow rate were selected as 80 °C, 0.25 mm, and 1 mL/min, respectively. The SHHE showed a higher extraction efficiency (22.18 wt%) within 2 h than Soxhlet extraction (17.94 wt%) for 24 h and cold pressing (4.29 wt%) for 72 h. The fatty acids profile for SHHE was more similar to that obtained by cold pressing method than Soxhlet extraction.     

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.     

Kinetics of supercritical carbon dioxide extraction of borage and evening primrose seed oil

In the present work, high‐pressure extraction of borage (Borago officinalis L.) and evening primrose (Oenothera biennis L.) seed oil, containing the valuable γ‐linolenic acid (GLA), has been investigated. Extraction was performed with supercritical carbon dioxide on a semi‐continuous flow apparatus at pressures of 200 and 300 bar, and at temperatures of 40 and 60 °C. A constant flow rate of carbon dioxide in the range from 0.17 to 0.20 kg/h was maintained during extraction. The extraction yields obtained using dense CO₂ were similar to those obtained with conventional extraction using hexane as solvent. The composition of extracted crude oil was determined by GC analysis. The best results were obtained at 300 bar and 40 °C for both seed types extracted, where the quality of oil was highest with regard to GLA content. The evening primrose seed oil extracted with supercritical fluid extraction was particularly rich in unsaturated fatty acids: up to 89.7 wt‐% of total free fatty acids in the oil. The dynamic behavior of the extraction runs was analyzed using two mathematical models for describing the constant rate period and the subsequent falling rate period. Based on the experimental data, external mass transfer coefficients, diffusion coefficients and diffusivity in solid phase were estimated. Results showed good agreement between calculated and experimental data.