Optimization Of Supercritical Fluid Extraction Research Articles

Optimization of supercritical fluid extraction of bioactive compounds from Ammodaucus leucotrichus fruits by using multivariate response surface methodology

This study explored supercritical fluid extraction (SFE) of bioactive molecules from Ammodaucus leucotrichus seeds, a little-known source of potent bioactive compounds. Response surface methodology assessed extraction parameters (pressure, temperature, and ethanol co-solvent) and their effects on global yield, total phenolic compound (TPC), total carbohydrate content (TCC), and anti-Alzheimer activity. Optimization via a Box-Behnken design identified the optimal conditions: 15 % ethanol, 300 bar, and 70 °C. Chemical profiling using GC-MS and UHPLC-q-tof-MS/MS detected over 41 metabolites. In addition, a biorefinery sequential extraction process was performed to obtain extracts with high neuroprotective potential. The SFE extracts exhibited modest AChE inhibition. Notably, sequential SFE and PLE extractions yielded extracts with enhanced antioxidant activity compared to separate processes. In conclusion, Ammodaucus leucotrichus presents a promising natural source of secondary metabolites. Its potential health benefits warrant further exploration, emphasizing the need for continued research.

Optimisation of supercritical fluid extraction of orange (Citrus sinenis L.) peel essential oil and its physicochemical properties

In this study, the choice of supercritical fluid extraction as a renewable alternative for extracting orange peel essential oil (OPEO) was motivated by concerns about sustainability with conventional solvent extraction methods. The physical and chemical characteristics of OPEO were examined to assess its potential as a sustainable resource. The extraction process was optimised, and the ideal conditions determined were 317.51 min of extraction time at 74.85 °C with a solvent-to-sample ratio of 4. Analysis of the extracted OPEO revealed significant values for saponification (121.67 mg KOH/g), acid (4.13 mg KOH/g), ester (117.54 mg KOH/g), and free fatty acid (1.56 mg KOH/g) content, demonstrating its composition. Notably, key ingredients such as Limonene (43.96%), α-pinene (15.60%), β-myrcene (10.21%), γ-terpinene (5.00%), and α-terpineol (4.15%) were found in high proportions according to chemical composition analysis. Furthermore, OPEO exhibited excellent antioxidant properties with an IC50 value of 7.73 ± 2.00 mg/mL and displayed notable antimicrobial activity against various microorganisms, including P. aeruginosa (17.7 ± 0.6 mm), E. coli (11.0 ± 0.0 mm), K. pneumoniae (10.7 ± 0.6 mm), and S. aureus (10.3 ± 0.6 mm). These findings have significant implications for the flavor and fragrance sector, as well as for the food preservation industry.

Optimization of supercritical fluid extraction of polar flavonoids from Robinia pseudoacacia L. heartwood

The black locust, known as an invasive species, represent many advantages, mainly due to its rapid growth rate and its richness with interesting flavonoids. In this study, supercritical fluid extraction of the two main flavonoids dihydrorobinetin and robinetin, was optimized using a three level Box-Behnken response surface design. The conditions investigated to influence the extraction yield of these flavonoids were temperature (40–80 °C), pressure (10–20 MPa) and modifier’s percentage EtOH:H2O 80:20 (10 %−30 %). The response was quantified using an UHPLC-DAD optimized chromatographic method. The results showed the influence of the extraction conditions on the yield of the molecules of interest. The data were fitted into a second-order polynomial equation, the multiple regression analysis showed a high determination coefficient value (R2) of 0.93. The optimal extraction conditions were 10 MPa, 80 °C and extraction phase composition of CO2:EtOH:H2O 80:16:4 for 30 min. These conditions allowed for the recovery 49.2 mg of flavonoids for 1 g of dried wood powder.

Methodological Optimization of Supercritical Fluid Extraction of Valuable Bioactive Compounds from the Acidophilic Microalga Coccomyxa onubensis.

Microalgae grow in diverse environments and possess a great biotechnological potential as they contain useful bioactive compounds. These bioactive compounds can be obtained by selective and energy-efficient extraction methods. Various industries are using the supercritical fluid extraction (SFE) method to extract these valuable bioactive compounds. Hence, for the first time, we evaluated the effects of SFE on the recovery of bioactive and antioxidant compounds using Coccomyxa onubensis, a eukaryotic acidophilic microalga of potential relevance which can be used in the field of nutraceutical and functional foods. It was isolated from the Tinto River (Pyritic Belt, Huelva, Spain), a mining region in Spain. Variables such as extraction yield, lutein purity (LP) and recovery (LR), total phenols, and antioxidant capacity (Trolox equivalents antioxidant capacity method) were studied using a Box–Behnken design based on a response surface methodology along with the overall extraction curve fitted to a spline linear model. The effects of temperature (30, 50, and 70 °C), pressure (25, 40, and 55 MPa), and the percentage of co-solvent (0, 25%, and 50% v/v ethanol) on SFE were analyzed, resulting in the co-solvent and temperature as the most significant factors followed by the pressure. Under 70 °C, 40 MPa, and 50% v/v ethanol, C. onubensis reached a maximum of 66.98% of LR. The extracts were richest in total phenols and showed the maximum antioxidant activity (36.08 mg GAEs/g extracts and 2.237 mmol TE/g extracts, respectively) under similar pressure and co-solvent percentage values and different temperatures (30 and 70 °C, respectively). The extracts obtained in this study may have potential applications in the food, nutraceutical, and cosmetic industries. SFE is a highly efficient method to valorize microorganisms living in extreme environments, which are so far unexplored using green extraction methods.

Optimization of supercritical fluid extraction of dihydrotanshinone, cryptotanshinone, tanshinone I, and tanshinone IIA from Salvia miltiorrhiza with a peanut oil modifier

Identifying an appropriate experimental design and modeling approach is key in achieving optimal extraction of dihydrotanshinone, cryptotanshinone, tanshinone I, and tanshinone IIA from danshen (Salvia miltiorrhiza) through supercritical fluid extraction (SFE) with peanut oil as a modifier. Three factors and levels were evaluated, namely flow rate (2–6 L/min), modifier concentration (40%–80%), and pressure (35–45 MPa). High-performance liquid chromatography (HPLC) was applied to quantify the four compounds, and accuracy and precision tests were conducted to verify the HPLC. The predicted optimal conditions were 3.23 L/min, 52.21%, and 38.50 MPa for flow rate, modifier concentration, and pressure, respectively; in total, 1.472, 3.690, 12.095, and 17.125 mg/g of dihydrotanshinone, cryptotanshinone, tanshinone I, and tanshinone IIA were obtained, respectively. The current results reveal SFE to be more efficient and (with a peanut oil as modifier) requiring a shorter extraction time than Soxhlet and ultrasonic extraction.

Functional properties of extracts and residual dietary fibre from pomegranate (Punica granatum L.) peel obtained with different supercritical fluid conditions

The objective of this study was the optimization of supercritical fluid extraction (SFE) using CO2 for extraction of bioactive compounds from pomegranate peel, evaluating the functional properties of different extracts (SFE extracts and alcohol-insoluble residues (AIR)). A Box–Behnken design combined with response surface methodology (RSM) was used to optimize extraction pressure (250–300 bar), temperature (45–55 °C) and time (2–4 h). The results showed that these SFE conditions have a significant effect on the responses studied. Antioxidant activities of the extracts, residual dietary fibre and pectin were the parameters that best fitted the quadratic model developed in this study. RSM optimization of these parameters was performed using Derringer's desired function methodology, estimating optimal conditions for extraction pressure (291 bar), temperature (46.5 °C) and time (2.5 h). The results reveal that supercritical technology is an interesting option for fractionating and recovering high-value compounds from pomegranate by-products.

Response Surface Methodology for Optimization of Supercritical Fluid Extraction of Orange Peel Essential Oil

Background: Orange peel essential oils were obtained using supercritical fluid extraction. This method is an important high scaling extraction method used for the extraction of plant and animal extracts.
 Objectives: The aim of this study was the optimization of the extraction of the orange peel essential oil.
 Methods: The experimental parameters of Supercritical Fluid Extraction (SFE) such as temperature, pressure, and extraction time, and modifier volume were optimized using a central composite design after a 24-1 fractional factorial design. Orange peels were collected from ripe orange and were washed, air dried, and milled. Then, a Suprex MPS/225 system in the SFE mode with a maximal operating pressure of 395 bars was used for essential oil extraction. Moreover, GC-MS and GC-FID were used for the identification and determination of oil compounds, respectively.
 Results: Eight compounds have been identified based on their retention indices and mass spectra. According to the results, α-pinene, β-pinene, myrcene, d-limonene, terpinolene, C8-aldehyde, citronellol, and linalool were identified in orange peel essential oil. The optimum SFE conditions were obtained at a pressure of 347.07 atm, temperature of 55° C, extraction time of 30.16 min, and ethanol volume of 147.05 µL. Moreover, extraction yields based on SFE varied in the range of 0.04% to 1.18% (w/w). 
 Conclusion: The Results showed supercritical fluid technology as the best alternative technique for the extraction of pure and high-quality essential oil from orange peel. It is a green method and does not have any environmental impact.

Optimization of supercritical fluid extraction of asiaticoside from Centella asiatica using Central Composite Design (CCD)

ABSTRACT The extraction of asiaticoside was performed using supercritical fluid extraction to produce highly concentrated extracts. The effects of three factors (co-solvent percentage, pressure, and temperature) on the asiaticoside content were screened using the Two-Level Factorial design and optimized using the Central Composite Design. Asiaticoside was extracted following the treatment combinations of three parameters, namely co-solvent (5–15%), temperature (70–90°C), and pressure (1–20 MPa). The optimized extraction parameters were identified at 10%, 10.5 MPa, and 80°C for co-solvent percentage, pressure, and temperature, respectively.

Conventional versus novel extraction techniques for wheat germ oil recovery: multi-response optimization of supercritical fluid extraction

ABSTRACT The goal of this study was application of conventional [Soxhlet (SOX)] versus novel [supercritical fluid (SFE), microwave-assisted (MAE) and ultrasound-assisted (UAE)] extraction techniques for wheat germ oil recovery. Even though results suggested that MAE (with methylene chloride) provided the higher polyunsaturated fatty acids yield and higher oil functional quality comparing to SFE, SOX and UAE, all obtained oils exhibited good fatty acid profile and functional quality. SFE was the most suitable technique for oil recovery as provided certain advantages comparing to all other extraction techniques due to generally similar or higher tocopherol content, antioxidant activity and absence of organic solvent residues.

Optimization of Supercritical Fluid Extraction of Paprika (cv. Reshampatti) Oil, Capsaicin and Pigments

AbstractPaprika (Capsicum annuum L.) is a spice, utilized in culinary across the globe for its colour and pungency. A study was conducted to optimize the supercritical fluid extraction (SFE) process individually for selective extraction of paprika oil, capsaicin and pigments. Paprika oil was extracted by supercritical fluid—carbon dioxide at different process parameters: temperature (35‐75°C), pressure (100‐500 bar), extraction time (60‐180 minutes) and particle size (0.25‐1.25 mm) using central composite rotatable design (CCRD). The ANOVA results showed that yields of paprika oil, capsaicin and pigments were significantly (P ≤ .05) affected by the extraction process variables. Optimized SFE conditions, 65, 65 and 57.04°C temperature; 357.8, 200.62 and 400 bar pressure; 90, 90 and 100.89 minutes extraction time; and 0.78, 0.50 and 0.89 mm particle size, were obtained for optimum yield of paprika oil, capsaicin and pigments, respectively. Experimental yield of paprika oil, capsaicin and pigments at the optimized condition for respective compounds was 4.91% (w/w), 2.10% (w/w) and 16 319.9 NCV, and had good agreement with the predicted values. Antimicrobial activity of extracted paprika oil was found against E. coli, B. subtilus and S. aureus.

Extraction of β-Carboline alkaloids and preparation of extract nanoparticles from Peganum harmala L. capsules using supercritical fluid technique

Poor water solubility of pharmacologically active ingredients causes to incomplete absorption through the gastrointestinal tract. Increasing surface area by micronization has been performed to overcome these problems. In this study, the first step entailed an optimization of supercritical fluid extraction from the capsules of Peganum harmala L. As the second step, micronization process was accomplished using a new technique based on the expansion of CO2 supercritical solvent and collected precipitates were characterized by Field Emission Scanning Electron Microscopy (FESEM). The herbal extract was qualified using HPLC- mass spectrometry and Harmaline, Harmine and Harmalol were identified as the main β-carboline alkaloids. Effect of different supercritical parameters on the extraction yield and particle size were investigated. As a result, particle size decreased as the precipitation time decreased, whereas temperature and loaded volume did not significantly affect the morphology. Optimum micronization conditions were determined as: Volume of loaded extract (50 μL), oven temperature (40 °C), equilibrium and precipitation pressure (350 and 100 bar), equilibration and precipitation time (10 min). This supercritical process is proposed as a green technique for extraction and preparation of micronized β-Carbolines and nanoparticles with an average diameter ranging from 7 to 100 nm were successfully formed.

Optimization of supercritical CO2 extraction process for oleoresin from rotten onion waste

Supercritical fluid extraction technique (SFE) was utilized to obtain the superior quality of onion oleoresin from the dried rotten onion. The effects of temperature (50, 60, 70, 80 and 90°C), pressure (150, 225, 300, 375 and 450bar), dynamic time (30, 60, 90, 120 and 150min) and particle size (0.4, 0.6, 0.8, 1.0 and 1.2mm) were evaluated with respect to oleoresin yield, sulphur content and pyruvate content in oleoresin. The optimization of supercritical fluid extraction was carried out by using a central composite rotatable design (CCRD). From the responses, optimized condition for SFE of onion oleoresin was found as 80°C temperature, 400bar pressure, 0.53mm particle size and 60min dynamic time. Oleoresin extracted at optimized SFE condition had a yield of 1.012% oleoresin, 31g sulphur content per kg of oleoresin and 10.41 μmole pyruvate per g fresh weight of onion. It was observed that SFE provided shorter extraction time, comparatively similar oleoresin yield and a higher percentage of sulphur content which represents the useful sulphur containing compounds in onion.

Supercritical fluid extraction of raspberry seed oil: Experiments and modelling

The aim of this study was the optimization of supercritical fluid extraction (SFE) of raspberry seed oil. Sequential extraction kinetic modelling and artificial neural networks (ANN) were used for this purpose. SFE was performed according to the broaden Box-Behnken experimental design with pressure, temperature and CO2 flow rate as independent variables, while the influence of particle size on extraction kinetics and adjustable model parameters was additionally evaluated. Five empirical kinetic equations and mass-transfer model proposed by Sovová were utilized for extraction kinetics modelling. According to appropriate statistical parameters (R2, SSE and AARD), the mass-transfer model exhibited the best fit of experimental data. The initial mass-transfer rate of extraction curve was used as a response variable in ANN optimization. SFE should be performed at elevated pressure and CO2 flow rate, while temperature and particle size should be held at a lower level in order to achieve a maximal initial mass-transfer rate.

Optimization of supercritical fluid extraction of Mariposa Christia Vespertilionis leaves towards antioxidant using response surface methodology

Mariposa Christia Vespertilionis (MCV) or also known as butterfly wing leaves, is popular in the traditional medicine practice. The objective of this study is to optimize the antioxidant components (based on antioxidant activity analysis) from the MCV leaves extract using Supercritical Fluid Extraction (SFE) based on different temperature, pressure, and particle size via Response Surface Methodology (RSM). Besides that, it is also to evaluate the optimal condition of different extracting antioxidant activity from MCV leaves using Design Expert 10 software. The condition range for both pressure and temperature were between 150-350 bar and 30-70 °C with constant extraction time. The size of particle samples were between 63 μm-1000 μm. The antioxidant was analyzed using UV–vis Spectrophotometer (UV-vis). The lowest antioxidant activity was 8.20 % and higher antioxidant activity was obtained at 49.76 %. Lower absorbance indicated highest free radical scavenging activities. Maximum percentage (%) indicated high scavenging activities, thus higher 1,1-diphenyl-2-picrylhydrazyl (DPPH) is a good indication for antioxidant. The predicted RSM optimal condition of antioxidant activity was at temperature 50 °C, pressure 282 bar, and particle size 500 μm, which the predicted antioxidant was 50.62 %. Upon verification through experiment, it was found out that the antioxidant activity value was close to the predicted value with an average error of less than 1%.

Extraction kinetics modeling of wheat germ oil supercritical fluid extraction

The aim of this study was the optimization of supercritical fluid extraction (SFE) of wheat germ oil obtained as by-product from industrial mill. Extraction kinetics modeling and response surface methodology (RSM) were used for that purpose. SFE was performed with broadening Box-Behnken experimental design, where pressure (250–350 bar), temperature (40–60°C), and CO2 flow rate (0.2–0.4 kg/hr) were used as independent variables. Five empirical kinetic equations were successfully utilized for modeling of SFE. Model IV (Kandiah and Spiro model) provided the best fit with experimental data, according to statistical parameters (R2, sum of squared errors and average absolute relative deviation). Furthermore, initial slope calculated from this model was used as a response variable for RSM optimization. It could be concluded that SFE should be performed at elevated pressure (350 bar) and CO2 flow rate (0.4 kg/hr), while temperature should be held at a lower level (40°C) in order to achieve a maximal initial slope. Practical applications Optimization and modeling of industrial processes are crucial factors that will determine its efficiency and profitability. This research provided information about modeling of green and environmentally friendly extraction technique, that is, SFE, which could be successfully utilized for recovery of valuable oil from food industry by-product, that is, wheat germ. Commonly used empirical models were successfully applied for modeling of extraction process and influence of SFE factors on model parameters was determined providing information about mass transfer phenomena during extraction. Further investigation provided determination of the highest initial extraction rate constant which could be applicable for optimization of industrial scale processes.

Optimization of Supercritical Fluid Extraction of Hydrocarbons from a Contaminated Soil: An Experimental Approach

Optimization of Supercritical Fluid Extraction of Hydrocarbons from a Contaminated Soil: An Experimental Approach

Cosolvent Selection for Supercritical Fluid Extraction (Sfe) of Bioactive Compounds from Orthosiphon stamineus

In this work, a preliminary study was conducted to study the effects of different types and concentrations of cosolvents based on the total yield and antioxidants capacity prior to supercritical fluid extraction (SFE) of Orthosiphon stamineus (locally referred as misai kucing). Initially, a comparison was made by cold maceration technique with nine types of different cosolvents, namely water, pure ethanol, 25% (v/v) of ethanol in water, 50% (v/v) of ethanol in water, 75% (v/v) of ethanol in water, pure methanol, 25% (v/v) of methanol in water, 50% (v/v) of methanol in water and 75% (v/v) of methanol in water. The antioxidant capacity was analysed by free radical scavenging activity of 2,2-diphenyl-1-picrylhydrazyl (DPPH), total phenolic content (TPC) and total flavonoid content (TFC). Aqueous ethanolic solvent of 50% (v/v) ethanol in water showed the highest total yield of extract of 4.64 ± 0.02%. All antioxidant assays of TPC and TFC showed the highest value of 3.42 ± 0.08 mg GAE g−1 extract, 4.7 ± 0.14 mg CAE g−1 extract, respectively and IC50 value for DPPH was 0.625 μg/mL for 50% (v/v) ethanol in water extract. Based on the overall result, ethanolic solvents gave a better result for all antioxidant assays compared to those of methanolic solvents. Using the selected cosolvent, the identification of target compounds, which were rosmarinic acid, eupatorin and sinensetin from supercritical fluid extraction was determined by using HPLC. In conclusion, ethanol-water solvent was efficient in extracting bioactive compounds in O. stamineus and also improved the total yield, thus the usage of ethanolic solvent in different concentrations should be considered for further optimisation of SFE with cosolvent studies.

Optimization of Supercritical Fluid Extraction of Phenolic Compounds from Peach Blossom (Amygdalus Persica) by Response Surface Methodology

Supercritical fluid extraction (SFE) was used for the extraction of phenolic compounds from peach blossom (Amygdalus persica). The optimum conditions of SFE were optimized by response surface methodology and confirmed at 64°C, 30 MPa, 143 min, and 35 mL ethanol (100%) as modifier for maximum total phenolic contents (54.10 mg GAE g−1 DW), which was higher than the yield achieved by ultrasonic-assisted extraction (44.04 mg GAE g−1 DW). The antioxidant activities and tyrosinase inhibitory activities of extraction extracted by SFE were 79.55% and 14.42%. Furthermore, chlorogenic acid, quercetin-3-O-galactoside, kaempferol-3-O-galactoside, quercitrin-3-O-rhamnoside, and kaempferol 4′-glucoside were identified in this study.

Optimization of supercritical fluid extraction of polyphenols from oats (Avena sativa L.) and their antioxidant activities

This research explores the effects of pressure and temperature on the supercritical extraction of polyphenols, antioxidant capacity, and total polyphenolic content from oats. Ethanol (80% v/v) was used as co-solvent, and experiments were controlled by response surface methodology (RSM). For polyphenols with C6-C1 structures (vanillin and vanillic acid), a maximum yield of 18.2 μg/g oats was obtained. Polyphenols with C6-C3 structures (caffeic, sinapic, coumaric, and ferulic acids) gave up to 1389 μg/g oats; where coumaric and ferulic acids were found in higher quantities. Avenanthramides (AVNs) yielded up to 34.52 μg/g oats, with 2p and 2c being found in higher quantities than 2f. The polyphenols, TPC (1.25 mg GAE/g of oats), and ORAC (117.88 μmol TE/g of oats) gave the highest yields at 38 MPa and 55 °C. Quadratic models adjusted very well, and a maximum polyphenol content of 1437.57 μg/g was predicted. Moreover, correlations among the polyphenols and antioxidant capacity were found, especially with the ORAC. As a result, the method here presented can be a new procedure for the extraction of polyphenols from oats.

Optimization of supercritical fluid extraction of steviol glycosides and total phenolic content from Stevia rebaudiana (Bertoni) leaves using response surface methodology and artificial neural network modeling

Stevia leaves include natural, non-caloric sweetening compounds known as steviol glycosides (SGs)–mainly stevioside (ST) and rebaudioside-A (Reb-A). Along with sweetness, stevia generates interest because of its dietetic and therapeutic significance related to the presence of other bioactive compounds in its leaves, such as phenolics, which in association with SGs may contribute to human health by exerting anti-inflammatory, antihyperglycemic, anticarries, chemopreventive, insulinotropic and diuretic properties. In this study, response surface methodology (RSM) and artificial neural network (ANN) modeling were compared in terms of their estimation capabilities for building effective models with maximum response values. A supercritical fluid extraction (SFE) process was optimized by employing a 5-level-3-factor central composite design to achieve maximum target response values for total extract yield, ST yield, Reb-A yield and total phenolic content of 15.85%, 95.76mg/g, 62.95mg/g and 25.76mg GAE/g, respectively. The optimized SFE parameters included a modifier concentration of 40%, an extraction temperature of 45°C, and a pressure of 225bar. The ANN model proved an attractive alternative to RSM owing to its improved estimation and predictive capabilities. SFE yielded higher target response values than conventional maceration extraction (24h) and was a faster, lower energy, and greener extraction method with reduced CO2 emissions and lower solvent consumption.