Optimization of ethanol modified supercritical carbon dioxide on the extract yield and antioxidant activity from Biebersteinia multifida DC

Essential oil of Biebersteinia multifida DC cultivated in Iran was obtained by hydrodistillation (HD) and supercritical fluid extraction (SFE) methods. The oil was analyzed by capillary gas chromatography using flame ionization and mass spectrometric detections. The effects of different parameters such as temperature, pressure, static extraction time, dynamic extraction time, and mole fraction of modifier on the supercritical fluid extraction (SFE) and radical scavenging activity of B. multifida oil were optimized using central composite design. Fifty two compounds were identified in the HD oil. The major components of B. multifida were (E)-Nerolidol (31.45%), Hexadecanoic acid (11.84%), Phytol (17.1%), and 6,10,14-trimethyl-2-pentadecanone (15.4%). However, by using supercritical carbon dioxide in optimum conditions, obtained only four components contain more than 91.74% of the essential oil. The optimum extraction yield and DPPH EC₅₀ via SFE method were 96% (w/w) and 27.19, respectively.     

Continuous extraction of glycerol acetates from their mixture using supercritical carbon dioxide

Supercritical carbon dioxide was used for partially selective extraction of triacetin from a mixture of triacetin, diacetin, and monoacetin with a molar ratio of 1:2:1. The extraction was carried out in two stages. In the first stage, a central composite design was used to optimize the four variables of pressure, temperature, liquid CO₂ flow rate, and extraction time at three levels using a semi-continuous, supercritical carbon dioxide extraction setup. The composition of the extract under the predicted optimum conditions (i.e., 109 bar, 56 °C, 0.86 mL min⁻¹, and 61 min) was about 69% triacetin accompanied by only 30% diacetin and no detectable monoacetin. In the second stage, the effect of the two factors, pressure (100, 109, and 140 bar) and liquid CO₂ flow rates of 0.86 and 1.5 mL min⁻¹ measured at average laboratory temperature (27 °C) and pressure (0.89 bar), were studied using a continuous, supercritical carbon dioxide fractionation setup equipped with a glass-bead packed column kept under a thermal gradient of 56-70 °C. The experimental design was organized as a 3 × 2 general factorial design. Under the best conditions (i.e., 140 bar and 1.5 mL min⁻¹), the extraction yield of triacetin and diacetin were 41.8 and 3.0%, respectively, without any detectable monoacetin as verified by GC-FID.     

超临界CO_2萃取浓缩大豆粗磷脂的研究

以浓缩大豆粗磷脂作为液态物料的模型材料进行了超临界CO2萃取研究。通过实验考察了萃取温度、压力、时间和溶剂流量等对萃取效果的影响,确定了对于该种物质萃取的最佳操作条件。通过与传统的水蒸汽蒸馏法和有机溶剂萃取法生产的产品进行对比(酸碱度、含水量、有机溶剂残余量、色泽、气味等方面),表明了超临界流体萃取技术用于热不稳定物质的萃取所具有的独特优势。     

Reactive extraction of succinic acid using supercritical carbon dioxide

Reactive extraction using supercritical carbon dioxide (scCO₂) and tri-n-octylamine (TOA) was evaluated as a separation method of succinic acid from an aqueous solution. The reactive extraction of succinic acid was performed at varying initial acid concentrations in aqueous solution (0.07–0.45 mol?dm^?3), temperature (35–65°C) and pressure (8–16 MPa). The succinic acid separation was conducted in both batch mode and semi-continuous mode. The highest reactive extraction efficiency of approx. 62% was obtained for the process conducted in semi-continuous mode at 35°C and 16 MPa for the initial acid concentrations in aqueous phase of 0.39 mol?dm^?3.     

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.     

Enrichment of antibacterial compound from the stem bark of Stereospermum fimbriatum using supercritical carbon dioxide extraction

ABSTRACT

Supercritical carbon dioxide (sc-CO₂) extraction was carried out on Stereospermum fimbriatum’s stem bark in order to obtain an enriched extract containing the targeted active compound. The recovery of its active compound, C1, was compared with the most active Soxhlet’s extract of dichloromethane. A minimum inhibitory concentration (MIC) assay was done to examine the antibacterial activity of extracts against methicillin-resistant Staphylococcus aureus. The optimum condition for an enriched extract of sc-CO₂ to have a maximum recovery of C1 at MIC value of 400 µg/mL was suggested to be operated at 40°C and pressure at 30 MPa, with addition of 6% co-solvent.     

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.     

Optimization of Ferulago Angulata oil extraction with supercritical carbon dioxide

In this study, the essential oil of aerial parts of a species of a plant called Ferulago Angulata was extracted by CO₂ to optimize the results of the supercritical extraction process and then the essence was analyzed by the method of GC/MS. This extraction has been performed using Taguchi testing method and choosing L16 array in a laboratorial pilot under the following: pressure (90, 120, 140, and 190 bar), temperature (35, 40, 45, and 55 °C), the average particles size (250, 500, 710, and 2000 μm), flow rate (3, 5, 7, and 12 ml/s) and dynamic time (25, 50, 70, and 120 min). Then optimizing process was done to achieve maximum yield extraction. The optimizing conditions are as follows: 190 bar, 35 °C, 710 μm, 12 ml/s, supercritical flow rate 12 ml/s and the final yield is 0.853%. The total yield of supercritical extraction in the mentioned conditions as well as empirically is 0.97% or about 1%. This is the first report announcing optimization of the operation of supercritical extraction of Ferulago Angulata in a laboratorial condition. In the last report of the same authors, which was also for the first time, the chemical components of this plant essence were identified through supercritical extraction and then were compared with the extraction components of other traditional methods.     

Response surface optimization of Smyrnium cordifolium Boiss (SCB) oil extraction via supercritical carbon dioxide

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 (t_d), 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).     

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.     

Simulation of a supercritical carbon dioxide extraction plant with three extraction vessels

Although SuperCritical (SC) Fluid Extraction (SCFE) has been successfully applied commercially the last three decades, there is no systematic procedure or computational tool in the literature to scale-up and optimize it. This work proposes an algorithm to simulate dynamics in a multi-vessel (≥3) high-pressure SCFE plant where extraction vessels operate in batches, and is thus forced to use simulated-countercurrent flow configuration to improve efficiency. The algorithm is applied to a three-vessel SCFE plant using a shrinking-core model to describe inner mass transfer in the substrate. As example, the extraction of oil from pre-pressed seeds using SC CO₂ at 313 K and 30 MPa is simulated. After three cycles the process reaches a pseudo-steady-state condition that simplifies the estimation of plant productivity. Use of a three- instead of two-vessel SCFE plant increases oil concentration in the stream exiting the plant and decreases CO₂ usage at the expense of increasing extraction time.     

From supercritical carbon dioxide to gas expanded liquids in extraction and chromatography of lipids

Analytical‐scale extraction and chromatography of oils, fats and other liposoluble compounds can be achieved by using supercritical carbon dioxide as a solvent. Since the 90's when supercritical fluid chromatography (SFC) was a hot topic, this technology has developed into a robust, modern analytical technique that uses any proportions of compressed CO₂ mixed with an organic solvent. Supercritical fluid extraction (SFE) on the other hand is only recently starting to reform in a similar way, towards the use of more robust extraction system and enabling mixing of compressed CO₂ with larger proportions of organic solvents. In this Feature article, the development of SFC and SFE into what options we have today is described, including the latest trend of using CO₂‐expanded liquid (CXL) as extraction solvent for lipids.     

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     

Optimization of supercritical fluid extraction of lycopene from tomato skin with central composite rotatable design model

Response surface methodology using the central composite rotatetable design (CCRD) model was used to optimize parameters for supercritical carbon dioxide extraction of lycopene (C₄₀H₅₆) from dried tomato skin. The CCRD consisting of three-factored factorial design with two levels was used in this study. The factors used were temperature of the extraction chamber (40 and 70 °C), pressure of the extraction fluid (25 and 45 MPa), and modifier concentration (5 and 15%). Judged by the lack-of-fit-test, coefficient of determination and the standard errors results from the analysis of variance have shown the model to be adequate. The linear, quadratic and cross-effects were 0.58, 0.28 and 0.05, respectively. The independent variables have significantly (p < 0.05) influenced the extraction of all trans-lycopene from tomato skin. Although, no significant (p > 0.05) individual effect of modifier concentration shown, a synergetic effect was observed. A second-degree polynomial equation was developed from a response surface analysis for all trans-lycopene yield and the highest yield was predicted at 62 °C, 45 MPa (450 bar) and 14% temperature, pressure and modifier concentration, respectively and the recovery of all trans-lycopene was 33%.     

Purification of hydrocarbons from aromatic sulfur compounds by supercritical carbon dioxide extraction

Supercritical carbon dioxide extraction to purify samples of model hydrocarbons (tetralin, decalin, and tetradecane) containing various aromatic sulfur compounds (benzothiophene, dibenzothiophene, and 4,6-dimethydibenzothiophene) was studied. The influence of extraction temperature and pressure was investigated for the extraction from a tetralin-dibenzothiophene system in the range of 293-353 K and 8-15 MPa, and it was found that the amount of tetralin extracted increased with an increase in carbon dioxide density, while the separation factor decreased with an increase in carbon dioxide density. High recovery and high separation factor values for the tetralin-dibenzothiophene system were obtained under 10 MPa at 313 K. Higher separation factor was obtained for tetralin than decalin and tetradecane, containing 4,6-dimethyldibenzothiophene than that containing dibenzothiophene.     

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.     

Removal of contaminants from polluted drilling mud using supercritical carbon dioxide extraction

Liquid drilling fluid is often called drilling mud is heavy, viscous fluid mixtures use to carry rock cuttings to the surface and lubricate and cool the drill bit. During carrying cuttings they contaminated which not only reduce their functionality but also make them a hazardous and dangerous wastes which cannot be discharged anywhere without treatment. Due to this fact, in the present study, supercritical extraction process was used to remove contaminants from the drilling mud. Regarding this, effect of different parameters including extraction temperature (313–338 K) and pressure (100–200 bar), flow rate of CO₂ (0.05–0.36 cm³/s) and static time (20–130 min) on the removal of contaminations from drilling mud was examined using the design of experiment of changing one factor at a time. The obtained results revealed that the optimum operational conditions that lead to the highest removal degree of contaminations are temperature and pressure of 333 K and 180 bar, respectively, flow rate of lower than 0.1 cm³/s and the static time of 110 min. In addition, to examine the effect of the supercritical extraction on the crystalline structure modification and removal contaminations X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses were performed which confirmed the successful removal of contaminations from the drilling mud without significant crystalline modification.     

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.     

二氧化碳超临界萃取乙基香兰素粗制品的研究

采用二氧化碳超临界萃取乙基香兰素粗品,研究萃取压力、萃取温度、萃取时间、流体流量等工艺条件对萃取效率和产品质量的影响.得出最佳工艺条件,采用萃取压力25～30 MPa,萃取温度55～60℃,流体流量5 L/h,萃取5～6 h,萃取效率可以达到95％,可以得到质量分数大于95％的乙基香兰素产品.     

Allelopathic properties of the fractions obtained from sunflower leaves using supercritical carbon dioxide: The effect of co-solvent addition

The work described here is a continuation of a previous study centered on the extraction, using supercritical carbon dioxide, of bioactive substances from sunflower leaves of the Helianthus annuus L. variety Arianna. In this study the addition of 9% of ethanol as co-solvent was analyzed. The extraction was carried out (P = 100/400 bar, T = 35/55 °C, ethanol = 9%) in order to analyze the influence of pressure, temperature and sample pre-treatment on the extraction yield and bioactivity of the extracts. The addition of 9% of ethanol to the supercritical solvent enhanced both the extraction yield and the biological activity of the extracts. The best conditions were a pressure of 400 bar and a temperature of 55 °C. In an effort to improve the bioactivity of the extract, a cascade fractionation of the extracts was carried out and this gave different results in terms of biological activities and extraction yields. The phytochemical compositions of the extracts were analyzed by thin layer chromatography. The fractionation that gave the best results was carried out at 90 bar and 40 °C in the first separator. Finally, the effect of extracts on the growth of seeds from different plants was analyzed.