Application Of Supercritical Fluid Extraction Research Articles

Approach of Supercritical Carbon Dioxide for the Extraction of Kleeb Bua Daeng Formula.

Supercritical fluid extraction (SFE) is an innovative green technology for the extraction of phytochemicals from plants. Therefore, this study aimed to evaluate the application of SFE and to optimize the extraction conditions of the Thai herbal formula, Kleeb Bua Daeng (KBD). A Box-Behnken design (BBD) with response surface methodology (RMS) was used to determine the effect of the extraction time (30-90 min), temperature (30-60 °C), and pressure (200-300 bar) on response variables including the extraction yield, total phenolic content (TPC), total flavonoid content (TFC), total carotenoid content (TCC), and total anthocyanin content (TAC) of the KBD formula. The highest percentage extraction yield (3.81%) was achieved at 60 °C, 300 bar, and 60 min of the extraction time. The highest TPC (464.56 mg gallic acid equivalents/g extract), TFC (217.19 mg quercetin equivalents/g extract), and TCC (22.26 mg β-carotene equivalents/g extract) were all achieved at 60 °C, 250 bar, and 90 min of the extraction time. On the contrary, it was not possible to quantify the total anthocyanin content as anthocyanins were not extracted by this method. The results indicated that SFE-CO2 is a suitable method of extraction for a green recovery of phytochemicals with low and moderate polarity from the KBD formula.

A preliminary multistep combination of pulsed electric fields and supercritical fluid extraction to recover bioactive glycosylated and lipidic compounds from exhausted grape marc

This article reports the first multistep combination of pulsed electric field (PEF; 3 kV/cm, 100 kJ/kg, 2 Hz, 100 ms) and supercritical fluid extraction (SFE) with CO2 (10–20 MPa, 25 mL/min [10% EtOH], 50 °C, 60 min) for exhausted grape marc (EGM). This current protocol was mainly created to recover bioactive glycosylated and lipidic compounds. In this regard, total antioxidant capacity (TAC) was enhanced up to 68% after PEF treatment compared to conventional soaking. However, re-extracting PEF-treated EGM after the application of SFE (PEF + SFE) boosted the efficiency by up to 87%. Several polyphenols (kaempferol, luteolin, scutellarin, and resveratrol, among others), together with other glycosylated structures, were identified by liquid chromatography coupled with mass spectrometry analysis. The bioactive lipidic compounds extracted by SFE, along with the carbohydrate fraction (free sugars) favourably extracted by PEF pre-treatment (mainly glucose, but also fructose and sucrose), were concurrently detected by nuclear magnetic resonance. The remaining solid fraction after treatment was also characterised. Different microscopic morphology was observed by scanning electron microscopy (SEM) on untreated, PEF, and PEF + SC–CO2–treated EGM. Differential thermogravimetric (DTG) curves determined by thermogravimetric analysis (TGA) also suggested alternative and potential means for the valorisation of this matrix.

Parameter Effects and Optimisation in Supercritical Fluid Extraction of Phenolic Compounds from Labisia pumila

Labisia pumila, locally referred to as kacip fatimah, is one of the important herbs utilised in traditional medicine. Nonetheless, to the best of the researchers’ knowledge, the optimum application of Supercritical Fluid Extraction (SFE) has not been reported for Labisia pumila (L. pumila) extraction and the understanding of this study may offer preliminary insight into the preparation of standardised extracts of L. pumila enriched with natural antioxidants prior to commercialisation at the industrial level. Response surface methodology (RSM) was used to optimise supercritical carbon dioxide extraction (SC-CO2) of functional phenolic compounds from L. pumila leaves. The factors studied were pressure, temperature, percentage of ethanol in co-solvent, and co-solvent concentration. The results demonstrated that the percentage of ethanol in co-solvent, temperature, and co-solvent concentration in the supercritical mixture had significant effects on the extraction of L. pumila. Based on the RSM results, the optimal SC-CO2 extraction conditions were at 283 bar, 32 °C, 78% (v/v) of ethanol-water in co-solvent, and 16% (v/v) of co-solvent concentration, which allowed the recovery of 14.051 ± 0.76% (g/g) of extraction yield, 1.2650 ± 0.10% (g/g) of gallic acid, 0.441 ± 0.29% (g/g) of methyl gallate, and 1.382 ± 0.37% (g/g) of caffeic acid. The experimental values were in agreement with the one predicted by RSM models, confirming the suitability of the model for optimisation of the extraction conditions.

Application of Supercritical Fluid Extraction (SFE) of Tocopherols and Carotenoids (Hydrophobic Antioxidants) Compared to Non-SFE Methods

Natural antioxidants have renewed value for human health and the food industry. Green labeling is becoming an important attribute for consumers and is impacting food processing and formulations. Clean label is another attribute that ranked third after the “free-from” claims and “a good source” of nutrient claims. Clean label attributes also are ranked higher than local, seasonal, and organic. Techniques that are able to preserve the valuable characteristics of natural antioxidants, while eliminating even trace amounts of solvent residues from their extraction and processing, are important. Supercritical fluids (SCF) are an effective green technology that can be adopted for extraction of natural antioxidants. This review is focused on the application of supercritical carbon dioxide (SCCO2) for extracting hydrophobic antioxidant compounds with an emphasis on oilseed crops and carrots. The information provided about extraction parameters helps to guide optimization of the yield of tocopherols and carotenoids. Pressure is the most effective parameter for the extraction yield of tocopherol among the other parameters, such as temperature, time, and CO2 flow rate. For carotenoid extraction, both pressure and temperature have a large impact on extraction yield. Higher yields of antioxidants, greater purity of the extracts, and larger retention of bioactivity are the main advantages of supercritical fluid extraction (SFE) in comparison to other conventional techniques. The benefits of SCF technology may open new opportunities for extracting valuable, natural and effective antioxidant compounds from food processing co-streams for use as bioactive compounds.

Pharmaceutical Applications of Supercritical Fluid Extraction of Emulsions for Micro-/Nanoparticle Formation.

Micro-/nanoparticle formulations containing drugs with or without various biocompatible excipients are widely used in the pharmaceutical field to improve the physicochemical and clinical properties of the final drug product. Among the various micro-/nanoparticle production technologies, emulsion-based particle formation is the most widely used because of its unique advantages such as uniform generation of spherical small particles and higher encapsulation efficiency (EE). For this emulsion-based micro-/nanoparticle technology, one of the most important factors is the extraction efficiency associated with the fast removal of the organic solvent. In consideration of this, a technology called supercritical fluid extraction of emulsions (SFEE) that uses the unique mass transfer mechanism and solvent power of a supercritical fluid (SCF) has been proposed to overcome the shortcomings of several conventional technologies such as solvent evaporation, extraction, and spray drying. This review article presents the main aspects of SFEE technology for the preparation of micro-/nanoparticles by focusing on its pharmaceutical applications, which have been organized and classified according to several types of drug delivery systems and active pharmaceutical ingredients. It was definitely confirmed that SFEE can be applied in a variety of drugs from water-soluble to poorly water-soluble. In addition, it has advantages such as low organic solvent residual, high EE, desirable release control, better particle size control, and agglomeration prevention through efficient and fast solvent removal compared to conventional micro-/nanoparticle technologies. Therefore, this review will be a good resource for determining the applicability of SFEE to obtain better pharmaceutical quality when researchers in related fields want to select a suitable manufacturing process for preparing desired micro-/nanoparticle drug delivery systems containing their active material.

A Doubly Green Separation Process: Merging Aqueous Two-Phase Extraction and Supercritical Fluid Extraction

Aqueous two-phase extraction (ATPE) is a green separation technique which uses mixtures of water and environmentally benign polymers such as polyethylene glycol (PEG) as solvents. One of the challenges in implementing this extraction on an industrial scale is finding a suitable method for the isolation of target compounds from water-polymer solutions after the extraction, without diminishing ecological benefits of the method. In this paper, we propose using another green separation technique, supercritical fluid extraction (SFE), for the back-extraction of low molecular weight medium polarity compounds from ATPE solutions. Experiments with two model compounds, caffeine and benzoic acid, showed principal applicability of SFE for this task. Pressure (100–300 bar) and temperature (35–75 °C) of supercritical carbon dioxide play a major role in defining extraction capability. Extraction ratios of 35% for caffeine and 42% for benzoic acid were obtained at high fluid pressure and moderate temperature at 1:6 volume phase ratio. That gives an estimation of 10–20 theoretical steps required for complete exhaustive extraction from the ATPE solution, which is readily achievable in standard counter-current column SFE. Combining these two green methods together not only serves as an environmentally friendly method for the isolation of valuable low molecular weight compounds from diluted water solutions, but also allows for simple, energy effective recuperation of ATPE solvents.

Application of supercritical fluid extraction for extraction or enrichment of phospholipids in egg and dairy products: A review

Phospholipids (PLs) are polar lipids that are found in dairy products, egg, and oilseeds. They are amphiphilic in nature and find application in many foods as a functional ingredient. As PLs are distributed in food matrix in dilute form, attempts to concentrate the same by adopting suitable technical interventions have been widely investigated. One of the more successful approaches that have been reported is the application of supercritical fluid extraction (SCFE) to extract PLs using suitable cosolvents. The extraction protocol to extract PLs from dairy products and eggs using SCFE also includes a two‐step process, namely, separation of neutral lipids using neat CO2 followed by subsequent separation of polar lipids from the residue using cosolvent and CO2. This review is an attempt to compile information on dairy and egg PLs extracted using SCFE under varied operational factors. It is expected that the compilation will serve as resource for investigators working in this research area.Practical ApplicationsMilk fat processing results in valuable by‐products which can be suitably volarized to increase profitability through processing gains and reduce environmental footprints in dairy industry. The by‐products such as buttermilk, butter serum, ghee residue, and so forth can be tapped as potential sources for phospholipid (PL). Eggs have already been recognized as a good source of PLs, which are reported to have preventive effect on pathogens, cancer protective, anti‐inflammation and cardiovascular disease. Two challenges could be anticipated in the fractionation of PLs from egg and milk by‐products. First, extraction of lipids from substrate which include polar and neutral lipids. Second, separation of neutral and polar lipids from the lipid extract. Conventional methods of extraction involve many solvents for the wide range of lipids to be extracted, which often result in incomplete extraction. Supercritical fluid extraction (SCFE) technique is reported to be useful in extraction and separation of PLs from dairy and egg products. Process intervention strategies and optimization approaches have been undertaken by various researchers to quantify and improve extractability of PLs using SCFE. The paper is a compilation of the scientific information related to extraction of dairy and egg PLs using SCFE, which will serve as a knowledge resource for researchers working in related fields.

Energy-economic analysis of the applicability of supercritical fluid extraction of ethylene oxide

A new scheme has been developed for the separation of ethylene oxide from its aqueous solution using supercritical carbon dioxide and further concentration of the product. An energy and economic comparative analysis of new methods of the separation of ethylene oxide from an aqueous solution and its further concentration with the traditional scheme has been carried out. This analysis showed that a scheme with supercritical fluid extraction with carbon dioxide and the addition of propane into the scheme is energetically and economically advantageous.

Effect of supercritical CO2 extraction variability on the yield of Tridax procumbens roots extract and (3S)-16,17-didehydrofalcarinol content

Currently, no studies have reported the application of supercritical fluid extraction (SFE) to obtain extracts of Tridax procumbens roots and to evaluate the effects of the pressure, temperature, and extraction time variables. There are few analytical investigations that have been done for the quantitation of falcarinol-type molecules in this species. In this study, a fast, new method using the SFE technology for the obtention of CO2 extract of T. procumbens, as well as its active metabolite (3S)-16,17-didehydrofalcarinol, was done. The aim was to evaluate the potential of a SFE procedure to deliver a high yield in a complex matrix and to achieve the best and selective condition. For the CO2 extract, the highest yield (0.2230 mg/g) was attained when 200 bar, 40 °C, and 4.5 h were employed; on the other hand, the maximum amount of (3S)-16,17-didehydrofalcarinol was 0.0409 mg/g operating at 150 bar, 45 °C, and 1.5 h.

Extraction and bioprocessing with supercritical fluids

Abstract Supercritical fluid (SCF) technologies have emerged as a real alternative to various natural product extraction processes and pharmaceutical production to obtain micronized particles, coprecipitates, nanocomposite polymer structures and liposomes, in addition to other increasingly larger applications described in literature. In the present work, a brief literature review of the application of supercritical fluid extraction (SFE) is presented. This is evidenced by several publications and patents, contributions from several countries and the increase of industries around the world dedicated to this technique. Next, we aim to focus the analysis of SFE on a review of the literature applied to microalgae as a substitute primitive feedstock due to its high growth rate, valuable biologically active lipophilic substances, and photosynthetic efficiency without competition with food sources or needs of arable lands. We finally discussing an SCF bioprocess with a very new perspective for liposome production focalized on its potential at industrial scale.

Tomato as Potential Source of Natural Additives for Meat Industry. A Review.

Tomato industry produces huge amounts of by-products that represent an environmental and economic problem. However, these by-products contain multiple bioactive compounds, which would make them a renewable source for obtaining natural antioxidants and colourants (carotenoids). This is in line with the preferences of the current consumer who demands more natural and healthy products. However, the lipophilic character of carotenoids means that their extraction must be carried out using toxic organic solvents. To overcome environmental and health problems of organic solvents, the application of supercritical fluid extraction (SFE) for the extraction of lipophilic compounds such as lycopene was used successfully, achieving yields similar to those obtained with conventional techniques. Nonetheless, the extraction conditions must be carefully selected, to obtain high yields and at the same time maintain a high antioxidant capacity. On the other hand, the use of tomato and tomato extracts as natural additives in meat products are reduced in comparison with other natural antioxidant/colourant extracts. However, different researches conclude that the use of tomato improved nutritional quality, reduced lipid oxidation and increased stability during the shelf-life period of meat products, while retaining or increasing sensory properties and overall acceptability, which converts tomato by-products into a promising source of natural additives.

Effects of pressure variation and dynamic extraction time in supercritical fluid extraction (SFE) with cosolvent on bioactive compounds from Orthosiphon stamineus

Supercritical Fluid Extraction (SFE) is an advance method used in extracting bioactive compounds from plants. However, carbon dioxide used as an extraction solvent in SFE has limitation in extracting polar compounds. By adding a small amount of co-solvent (polar solvent) to extract wide range (polar to non-polar) of bioactive compounds, thereby affecting the extract yields. Pressure and dynamic time play important roles in this technique. In this study, the effects of pressure variation and continuous dynamic extraction time on the bioactive compounds from Orthosiphon stamineus , which were rosmarinic acid, 3’-hydroxy-5,6,7,4’-tetramethoxyflavone, sinensetin, and eupatorin using ethanol (co-solvent) modified CO 2 SFE were discussed. The pressure variations studied were included 150, 225, and 300 bar with continuous dynamic extraction. The co-solvent used was 10% (v/v) of absolute ethanol with a flow rate at 4 mL/min. The quantification of bioactive compounds was done using HPLC. The variation of pressure and dynamic time significantly affected the total component yields of targeted bioactive compounds obtained after the extraction process, as it was increased along with increasing of extraction pressure and time. The total yields of bioactive compounds at different pressures were 4.08% (150 bar), 4.18% (225 bar) and 4.51% (300 bar). The application of SFE with co-solvent and the relationship with the yields of targeted bioactive compounds obtained from of O.stamineus were given.

The Application of Supercritical Fluid Extraction in Phenolic Compounds Isolation from Natural Plant Materials.

The separation of phenolic compounds by supercritical fluid extraction has been widely studied throughout the last two decades. This is evidenced by a number of publications and articles. Supercritical fluid extraction (SFE) has become thus the effective method of separating the mentioned group of compounds. On the other hand, SFE is a beneficial approach in plant waste materials utilization and reduction of environmental burdens caused by the wastes. The aim of the study is to gather and systematize available information on the phenolic compounds separation that have been reported so far as well as to evaluate whether there is one optimal supercritical fluid extraction method for the phenolic compounds.

Recent applications of on-line supercritical fluid extraction coupled to advanced analytical techniques for compounds extraction and identification.

In a previous review (Sánchez-Camargo etal., J. Sep. Sci. 40 (2017) 213-227), we discussed the application of on-line supercritical fluid extraction coupled to chromatographic techniques. This review includes an update of the most recent publications (from January 2016 till June 2018) on this topic, which employs advanced analytical techniques for extracting and identifying valuable analytes. Supercritical fluid extraction has been widely recognized as a green sample preparation technique, because it is efficient, environmentally friendly, powerful, and faster, offering the possibility of direct coupling to analytical instrumental techniques. Among those techniques, supercritical fluid chromatography has experienced an innovative progression in the last 10 years, and the most recent applications of supercritical fluid extraction are coupled to this advanced analytical tool. The general principles, both methodological and instrumental of on-line supercritical fluid extraction coupled to supercritical fluid chromatography are described here. Besides, applications of the mentioned coupling for analysing biological fluids, food, soil, and botanical samples are also presented and discussed. Finally, a brief description about the very recent on-line coupling of supercritical fluid extraction to ion mobility spectrometry is presented, as well as concluding remarks about the importance of using these coupled techniques in the near future.

Fitting of broken and intact cell model to supercritical fluid extraction (SFE) of sunflower oil

Abstract The present work is focused on the supercritical extraction and kinetic study of sunflower oil. The effect of operating parameters, namely pressure (20–40 MPa), temperature (333–373 K), solvent mass flow (0.83 × 10 − 4 to 2.50 × 10 − 4 kg/s), particle size (0.50–1.00 mm) and ethanol as co-solvent (0–10%) have been studied by a set of experiments. The outcomes of work show, extraction yield increases with increasing pressure, solvent mass flow and co-solvent. The retrograde phenomenon is also observed between 333 and 353 K. The experimental data have been used to simulate the broken and intact cell model and fitting parameters are optimized by the global optimization method. The model successfully fitted the experimental data at high pressure with lower particle size. Industrial relevance The sunflower seeds are a major source of good quality, high oleic acid, vegetable oil and Vitamin E. Hence, largely used in beauty care products, production of vegetable oil based fuel oil and lubricants. There are also many other applications of rich–oleic acid oils such as food, cosmetics, pharmaceuticals, biodiesel production, and also as a feedstock for the oleo-chemical industry. In recent years, due to rigid environmental regulation and health concern, high pressure extraction of the vegetable oil with supercritical carbon dioxide has received considerable attention as a promising alternative to conventional solvent extraction and mechanical process. Hence, the present work is focused on extraction of seed oil by supercritical CO 2 . Moreover, for industrial application of supercritical fluid extraction, it is very important to study the kinetic model that gives large scale extraction curves with minimum error by using model fitting parameters with small scale experiment. There are large numbers of models based on different approach suggested by various researchers to fit experimental data of supercritical fluid extraction. Amongst them, the broken and intact cell model proposed by Sovova's (1994) is widely used to fit the experimental data of vegetable oil extraction. The broken and intact cell model has three fitting parameters and many authors have applied different optimization techniques to optimize these fitting parameters. Therefore, in the present work the optimized kinetic parameters of Sovova's model for sunflower oil extraction are obtained by applying the Box complex optimization method to study the influence of pressure, temperature, particle size, co-solvent and solvent flow rate of extraction yield.

Optimisation of the Supercritical Fluid Extraction of Antioxidants from Broccoli Leaves

This work presents the application of supercritical fluid extraction (SFE), an environmentally friendly methodology, to obtain broccoli leaves extracts with a high antioxidant activity. The following processing variables: pressure, temperature, percentage of ethanol and dynamic extraction time were optimised by means of a central composite design, combined with response surface methodology. The optimised conditions were applied to the extraction of broccoli leaves from different cultivars (Naxos, Nubia, Marathon, Parthenon and Viola). The optimal values of the extraction variables were 150 bars, 35 °C, 20 % ethanol and 10 min of dynamic extraction time. Percentage of ethanol and the combined effect of pressure and time were the factors that affected the extraction the most. The results obtained from different cultivars showed that the Naxos variety provided the extracts with the highest antioxidant activity and total phenolic content; moreover, DPPH (EC 50) values were higher than those previously reported for water extracts. The extracts were recovered in a small quantity of ethanol that could be easily eliminated, obtaining a residue free of contaminants.

Application of Supercritical Fluid Extraction on Food Processing: Black-eyed Pea (Vigna Unguiculata) and Peanut (Arachis Hypogaea)

This present study investigates application of supercritical fluid carbon dioxide extraction (SCFE-CO2) for removing fats from black-eyed pea (Vigna unguiculata) and peanut (Arachis hypogaea) to produce high protein-low fat diet products. SCFE-CO2 process used Taguchi's orthogonal array at three parameters in three levels: pressures between 25-35MPa, temperatures between 40-60°C and CO2 flowrates between 10-20g/min. The results of the experiment showed that the optimum conditions of SCFE- CO2 process were 25MPa, 60°C, 10g/min for black-eyed pea and 35MPa, 60°C, 15g/min for peanut. The highest yield for black-eyed pea and peanut were 5.4% and 48.5%, respectively.

Application of supercritical fluid extraction for separation of nutraceuticals and other phytochemicals from plant material

In present work a literature review of application of supercritical fluid extraction (SFE) for isolation of nutraceuticals and some other phytochemicals up to December of 2012 is presented. Manuscript provides knowledge of SFE processes and possible aplications of SFE for extraction of bioactive compounds which serve as nutraceuticals. Compounds are classified into groups based on their chemical nature (carotenoids, flavonoids and other phenolic compounds, essential oils, lipids and fatty acids, and alkaloids and other bioactive phytochemicals) and they are reviewed in tabular form along with plant material, from which they were extracted using supercritical fluids.

Application of supercritical CO2 for extraction of polyisoprenoid alcohols and their esters from plant tissues

In this study, a method of supercritical fluid extraction (SFE) with carbon dioxide of polyisoprenoids from plant photosynthetic tissues is described. SFE was an effective extraction method for short- and medium-chain compounds with even higher yield than that observed for the "classical extraction" method with organic solvents. Moreover, SFE-derived extracts contained lower amounts of impurities (e.g., chlorophylls) than those obtained by extraction of the same tissue with organic solvents. Elevated temperature and extended extraction time of SFE resulted in a higher rate of extraction of long-chain polyisoprenoids. Ethanol cofeeding did not increase the extraction efficiency of polyisoprenoids; instead, it increased the content of impurities in the lipid extract. Optimization of SFE time and temperature gives the opportunity of prefractionation of complex polyisoprenoid mixtures accumulated in plant tissues. Extracts obtained with application of SFE are very stable and free from organic solvents and can further be used directly in experimental diet supplementation or as starting material for preparation of semisynthetic polyisoprenoid derivatives, e.g., polyisoprenoid phosphates.

Application of supercritical fluid extraction coupled with counter-current chromatography for extraction and online isolation of unstable chemical components fromRosa damascena

Supercritical fluid extraction (SFE) coupled with high-speed counter-current chromatography (HSCCC) was successfully used for the extraction and online isolation of the unstable compounds from Rosa damascene in a single extraction and separation operation in two stages. The solvent systems of SFE/HSCCC were optimized with the help of multiexponential function model. At the first stage, the upper phase of the solvent system of n-butanol-tert-butyl methyl ether-acetonitrile-0.1% aqueous TFA (1.7:1.0:0.8:4.0, v/v/v/v) was used as both the SFE entrainer and the HSCCC stationary phase, and the target compounds were eluted with the corresponding lower phase to separate the hydrophobic compounds. At the second stage, the upper phase of the solvent system of n-hexane-ethyl acetate-methanol-water (3.2:1.0:2.8:2.6, v/v/v/v) was used as both the SFE entrainer and the HSCCC stationary phase, followed by elution with the corresponding lower phase to separate the moderate hydrophobic compounds. Six compounds including formononetin, delphinidin, cyaniding, 5,6,4'-trihydroxy-7,8-dimethoxy flavone, 5,3'-dihydroxy-7,8-dimethoxy flavone, and 5-hydroxy-6,7,8,3',4'-pentamethoxy flavone were successfully separated in one extraction-separation operation within 300 min. The targeted compounds were identified by MS and NMR spectroscopy. This research has opened up great prospects for industrial application of SFE/HSCCC to the extraction and separation of unstable compounds.