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.     

Comparison of essential oils compositions of Nepeta persica obtained by supercritical carbon dioxide extraction and steam distillation methods

Essential oil of Nepeta persica cultivated in Iran was obtained by steam distillation and supercritical (carbon dioxide) extraction methods. The oils were analysed by capillary gas chromatography using flame ionization and mass spectrometric detections. The compounds were identified according to their retention indices and mass spectra (EI, 70 eV). The effects of different parameters such as pressure, temperature, modifier volume and extraction times (dynamic and static) on the supercritical fluid extraction (SFE) of N. persica oil were investigated. The results showed that under the pressure of 20.3 MPa, temperature of 45 °C, methanol of 1.5% v/v), dynamic extraction time of 50 min and static extraction time of 25 min extraction was more selective for the 4αβ,7α,7aα-nepetalactone. Twelve compounds were identified in the steam-distilled oil. The major components of N. persica were 4αβ,7α,7aα-nepetalactone (26.5%), cis-β-farnesene (4.4%) and 3,4α-dihydro-4aα,7α,7aα-nepetalactone (3.5%). However, by using supercritical carbon dioxide under optimum conditions, only two components have more than 90.0% of the oil. The extraction yield based on steam distillation was 0.08% (v/w). On the other hand, using SFE extraction yield in the range of 0.22–8.90% (w/w) were obtained at different conditions. The results show that, in Iranian N. persica oil, 4αβ,7α,7aα-nepetalactone is a major component.     

Optimization of an Aqueous Extraction Process for Pomegranate Seed Oil

Response surface methodology employing a five-level, four-variable central composite rotatable design was applied to study the effects of extraction time, extraction temperature, pH and water/solid ratio on the extraction yield of pomegranate seed oil using an aqueous extraction approach. In addition, quality indices, fatty acid composition and antioxidant activity of the obtained oil were studied and compared with those of typical hexane-, cold press- and hot press-extracted oil. Aqueous extraction resulted in the maximum oil recovery of 19.3% (w/w), obtained under the following critical values: water/solid ratio (2.2:1.0, mL/g), pH 5.0, extraction temperature = 63 °C and extraction time = 375 min. This yield is lower than that obtained via hexane extraction (26.8%, w/w) and higher than the yields from cold press (7.0%, w/w) and hot press (8.6%, w/w) extraction. A comparison of the characteristics of the oils based on extraction method revealed that the unsaturated fatty acid content was highest for the oil obtained by aqueous extraction. In addition, higher levels of iodine and peroxide and lower levels of acid, p-anisidine and unsaponifiable matter were observed. The oil obtained with aqueous extraction also exhibited higher antioxidant activity than oils obtained by hexane or hot press extraction.     

Optimization of enzymatic pretreatment for n-hexane extraction of oil from Silybum marianum seeds using response surface methodology

An investigation on enzymatic pretreatment for n-hexane extraction of oil from the Silybum marianum seeds was conducted. The optimum combination of extraction parameters was obtained with the response surface methodology (RSM) at a four-variable and five-level central composite design (CCD). The optimum parameters of enzymatic pretreatment were as follows: enzyme concentration of 2.0% (w/w), temperature of 42.8 °C, reaction time of 5.6 h, and pH of 4.8. After enzymatic pretreatment, the oil was extracted by n-hexane for 1.5 h, and the oil yield on a dry basis was 45.70%, which well matched with the predicted value (45.86%). The results of the effects of the enzymatic pretreatment for n-hexane extraction of oil from the aspects of oil yield, microstructure and the fatty acid compositions showed that the enzymatic pretreatment had not affected on the fatty acid compositions, but could cause structure breakage of the S. marianum seeds and accelerate releasing extra oil, which increased the oil yield by 10.46% compared with n-hexane extraction for 1.5 h without enzymatic pretreatment, and confirmed the efficacy of enzymatic pretreatment for n-hexane extraction of oil from the S. marianum seeds.     

Aqueous enzymatic extraction of peanut oil and protein hydrolysates

The aqueous enzymatic process of simultaneously preparing oil and protein hydrolysates from peanut was investigated. The optimum parameters for hydrolysis using Alcalase 2.4L were established by the single-factor and orthogonal test. The optimal processing conditions were as follows: hydrolysis temperature 60 °C, pH 9.5, ratio of material to water 1:5 (w/w), alkaline extraction time 90 min, enzyme amount 1.5% (w/w) and hydrolysis time 5 h. Under these conditions, the free oil and protein hydrolysates yields were 79.32% and 71.38% respectively. In order to improve these yields, As1398 was chosen to hydrolyze the residue and emulsion. The total free oil and protein hydrolysates yields were increased to 91.98% and 88.21% 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.     

Optimization of process variables for essential oil components from Satureja hortensis by supercritical fluid extraction using Box-Behnken experimental design

The oil and extracts of Satureja hortensis cultivated in Iran were extracted using supercritical carbon dioxide and hydrodistillation method. The oil and extracts were analyzed by GC-FID and GC/MS. The compounds were identified according to their retention indices and mass spectra (EI, 70 eV). The effects of various parameters such as pressure, temperature, percent of modifier (methanol) and extraction time, were investigated by a fractional factorial design (2^4-1) to determine the significant parameters and their interactions. The results showed that the pressure, temperature and percent of modifier are significant (p < 0.05), but the extraction time was found to be insignificant. The response surface methodology (RSM), based on Box-Behnken design was employed to obtain the optimum conditions of the significant parameters (pressure, temperature and percent of modifier). The optimal conditions could be obtained at a pressure of 35.0 MPa, temperature of 72.6 °C, and 8.6% (v/v) for methanol. The main extracted components using SFE were γ-Terpinene (35.5%), Thymol (18.2%) and Carvacrol (29.7%).     

Recovering Bioactive Compounds from Olive Oil Filter Cake by Advanced Extraction Techniques

The potential of by-products generated during extra-virgin olive oil (EVOO) filtration as a natural source of phenolic compounds (with demonstrated bioactivity) has been evaluated using pressurized liquid extraction (PLE) and considering mixtures of two GRAS (generally recognized as safe) solvents (ethanol and water) at temperatures ranging from 40 to 175 °C. The extracts were characterized by high-performance liquid chromatography (HPLC) coupled to diode array detection (DAD) and electrospray time-of-flight mass spectrometry (HPLC-DAD-ESI-TOF/MS) to determine the phenolic-composition of the filter cake. The best isolation procedure to extract the phenolic fraction from the filter cake was accomplished using ethanol and water (50:50, v/v) at 120 °C. The main phenolic compounds identified in the samples were characterized as phenolic alcohols or derivatives (hydroxytyrosol and its oxidation product), secoiridoids (decarboxymethylated and hydroxylated forms of oleuropein and ligstroside aglycones), flavones (luteolin and apigenin) and elenolic acid derivatives. The PLE extraction process can be applied to produce enriched extracts with applications as bioactive food ingredients, as well as nutraceuticals.     

Subcritical water extraction of essential oil from Aquilaria malaccensis leaves

ABSTRACT

Hydro-distillation (HD) has been widely used in the extraction of essential oil, yet it is a low efficient method that consumes time and energy. In this work, A. malaccensis’ oils have been extracted using subcritical water extraction (SCWE) from its leaves to determine the optimum parameters using analysis of variance. Quadratic model was deduced to be most suitable to analyze SCWE parameters. Regression analysis indicated that interaction of temperature and reaction time parameters exerted great influence on the yield. Kinetic modeling was conducted to study SCWE’s mechanism, and second-order model was concluded to be the best model for SCWE. Optimum extraction conditions of essential oil were 156°C, 0.2 w/w, 25 min. Gas chromatography/mass spectroscopy characterization was conducted and results indicated that the quality of A. malaccensis’ leaves oils extracted by SCWE significantly improved compared to previous studies. Additionally, the essential oils extracted by SCWE contained several value-added compounds useful in medicine such as furfural and guaiacol. Fourier transform infrared, scanning electron microscopy, and Brunauer–Emmett–Teller and Barrett–Joyner–Halenda on the leaves samples provided further evidence for better performance of SCWE, as the sample’s pores, cell walls, cellulose, and hemicellulose were more damaged. The result showed that compared to extraction yield of HD method, that of SCWE was 2.5 times higher, while the requiring time was 8.4 times shorter. Therefore, it was concluded that SCWE is a better extraction method in terms of time, efficiency, yield, and quality.     

Optimization of supercritical carbon dioxide extraction of Passiflora seed oil

This study investigates extraction of Passiflora seed oil by using supercritical carbon dioxide. Artificial neural network (ANN) and response surface methodology (RSM) were applied for modeling and the prediction of the oil extraction yield. Moreover, process optimization were carried out by using both methods to predict the best operating conditions, which resulted in the maximum extraction yield of the Passiflora seed oil. The maximum extraction yield of Passiflora seed oil was estimated by ANN to be 26.55% under the operational conditions of temperature 56.5 °C, pressure 23.3 MPa, and the extraction time 3.72 h; whereas the optimum oil extraction yield was 25.76% applying the operational circumstances of temperature 55.9 °C, pressure 25.8 MPa, and the extraction time 3.95 h by RSM method. In addition, mean-squared-error (MSE) and relative error methods were utilized to compare the predicted values of the oil extraction yield obtained from both models with the experimental data. The results of the comparison reveal the superiority of ANN model compared to RSM model.     

Development of Pressurized Extraction Processes for Oil Recovery from Wild Almond (Amygdalus scoparia)

Wild almond Amygdalus scoparia is a very fruitful tree that is spread over an extensive region of Iran. Considering its high quality oil, the development of clean extraction processes based on the use of compressed fluids is encouraged. In this study, the main factors involved in supercritical fluid extraction (SFE) and pressurized liquid extraction (PLE) of wild almond have been optimized by using two different experimental designs and considering the oil extraction yield as a response variable; effects of time, temperature, pressure, and use of co‐solvents were studied for SFE while effects of time, temperature and type of solvent were evaluated for PLE. Results showed that the maximum oil yield using supercritical carbon dioxide was 42 %, obtained under the following conditions: extraction temperature, 40 °C; extraction pressure, 40 MPa; and 10 % ethanol as co‐solvent. The optimum extraction yield for PLE was 55 %, which was achieved using ethanol as solvent at 150 °C for 20 min. Lipidomic analysis revealed that the amount of oleic acid in the oil extracted by SFE was higher than those obtained by using other classical procedures. In addition, triacylglycerols constituted more than 98 % of the extracted oils.     

Trigonella foenum-graecum L. Seed Oil Obtained by Supercritical CO2 Extraction

Supercritical CO₂ extraction (SC-CO₂) of fenugreek (Trigonella foenum-graecum L.) seed oil and its chemical composition and antioxidant activity were investigated. A central composite design combined with response surface methodology was used to study extraction conditions including pressure, temperature, and time. The optimum extraction conditions were 28.5?MPa extraction pressure, 41?°C extraction temperature, and 118?min extraction time, where 3.78?% yield was predicted. Fenugreek seed oil extracted under optimum conditions by SC-CO₂ was mainly composed of 28.3?% C18:3, 33.45?% C18:2, 9.89?% C16, 8.1?% C18:1, 3.7?% C18, 0.71?% C20, and 0.61?% C22. The fenugreek oil was rich in unsaturated fatty acids (nearly 70?% of the total fatty acids), and polyunsaturated fatty acids accounted for 61.42?% (mass percentage) of the total amount. The 2,2-diphenyl-1-picrylhydrazyl radical-scavenging activity increased from 12.5 to 88.4?% when the concentration was increased from 1 to 12?mg/ml. The reducing power of the seed oil was concentration-dependent. The antioxidant activity of the supercritical fluid extraction extract was superior to those obtained by Soxhlet extraction.     

Application of mixture experimental design to optimize formulation and performance of thermoplastic road markings

The influence of formulation components on the physical, mechanical and optical properties of hot melt thermoplastic road markings was studied. To minimize the number of experiments, mixture method was used as an effective tool for experimental design. Binder (rosin ester and hydrocarbon based resins), pigment (TiO₂), filler (talc) and plasticizer (long oil alkyd resin and dibutyl phthalate) were taken into consideration as the key factors at different levels. A range of formulations were prepared by melt blending of variables and other required components. Softening point temperature (T_sp) and its changes (ΔT_sp), Taber abrasion resistance, color difference (ΔE) before and after exposure to the accelerated weathering conditions and heat stability test, were chosen as the key responses. A window of optimum end-use properties of thermoplastic road marking formulations was narrowed down within the range of desired responses in quadratic model using DX v.7.1.3 program.     

Deep eutectic solvents aqueous two-phase system based ultrasonically assisted extraction of ursolic acid (UA) from Cynomorium songaricum Rupr.

Deep eutectic solvents (DESs) are new green solvents that have attracted the attention of the scientific community mainly due to their unique properties and special characteristics, which are different from those of traditional solvents. A method based on ultrasonically assisted deep eutectic solvent aqueous two-phase systems (UAE-DES-ATPS) was developed for extracting ursolic acid (UA) from Cynomorium songaricum Rupr. Four different types of choline chloride-based DESs were prepared. Choline chloride-glucose (ChCl-Glu) exhibited good selective extraction ability. An optimum DES-ATPS of 36% (w/w) ChCl-Glu and 25% (w/w) K₂HPO₄ was considered to be a satisfactory system for extracting UA. Response surface methodology (RSM) method was utilized to optimize the extraction of UA using UAE-DES-ATPS. The quadratic models were extremely significant (p?<?0.01) for all the parameters studied with high correlation coefficients (R²) of 0.9593. The optimum ultrasound-assisted conditions were as follows: solvent to solid ratio of 15:1 (g/g), ultrasound power density of 4.7?W·mL^?1, and extraction time of 54?min. Compared with the conventional UAE method, the yields were basically the same, but the presented method had higher purity. The structure of UA did not change between pure UA and UA in the upper phase using UV–vis and FT-IR. This approach using ChCl-based DES-ATPS as a novel extraction system and ultrasound as a source of energy provided a better choice for the separation of active components from other natural products.     

Supercritical fluid extraction of volatile oil from Lippia alba (Mill.) cultivated in Aragón (Spain)

The objective of this study is the supercritical extraction of the volatile oil from Lippia alba (Mill.) cultivated in Aragón. The influence of extraction pressure and temperature and cosolvent percentage on overall yield and volatile oil composition was studied. The supercritical extraction conditions were optimized using the 2007 crop; operating at 35.0 MPa, 40 °C and 5% of ethanol as cosolvent, 2009 and 2011 crops were also tested. Supercritical fluid extract compositions and overall yields were compared with the extracts obtained by conventional extraction techniques such as hydrodistillation (HD) and organic solvent extraction (OSE). Four terpenoids (linalool, 1,8-cineole, β-caryophyllene and β-caryophyllene oxide) were selected as target compounds and their content in the different extracts was monitored by gas chromatography. Linalool was selected as indicator of the plant adaptation to the commercial purposes. HD is the technique that provides the highest percentage of linalool in all the extracts, but showed always the lowest overall yields; whereas, SFE extracts provides a good balance between the overall yield and presence of the four target compounds.     

Ethanol-Modified Supercritical Carbon Dioxide Extraction of the Bioactive Lipid Components of <Emphasis Type="Italic">Camelina sativa</Emphasis> Seed

Camelina sativa seed is an underutilized oil source that attracts a growing interest, but it requires more research on its composition and processing. Its high omega‐3 content and growing demand for clean food processing technologies make conventional oil extraction less attractive. In this study, the effect of extraction methods on the bioactive lipid composition of the camelina seed lipid was investigated, and its bioactive lipid composition was modified at the extraction stage using ethanol‐modified supercritical carbon dioxide (SC‐CO₂). Ethanol‐modified SC‐CO₂ extractions were carried out at varying temperatures (50 and 70 °C), pressures (35 and 45 MPa), and ethanol concentrations (0–10%, w/w), and were compared to SC‐CO₂, cold press, and hexane extraction. The highest total lipid yield (37.6%) was at 45 MPa/70 °C/10% (w/w) ethanol. Phospholipids and phenolic content increased significantly with ethanol‐modified SC‐CO₂ (p < 0.05). SC‐CO₂ with 10% (w/w) ethanol concentration selectively increased phosphatidylcholine (PC) content. Apparent solubility of camelina seed lipids in SC‐CO₂, determined using the Chrastil model, ranged from 0.0065 kg oil/kg CO₂ (35 MPa/50 °C) to 0.0133 kg oil/kg CO₂ (45 MPa/70 °C). Ethanol‐modified SC‐CO₂ extraction allowed modification of the lipid composition that was not possible with the conventional extraction methods. This is a promising green method for extraction and fractionation of camelina seed lipids to separate and enrich its bioactives.     

Separation of Bromelain by Aqueous Two Phase Flotation

Aqueous two phase flotation (ATPF) system of polyethylene glycol (PEG) and potassium phosphate is studied for the separation and partial purification of bromelain from the pineapple fruit (Annanus comosus L. Merryl). The effect of PEG molecular weight (1500–20000), concentration of phase forming components (PEG 12–18% w/w and potassium phosphate 14–20% w/w), system pH, nitrogen flow rate, and flotation time were studied and optimum conditions for ATPF were obtained. At optimum conditions of the system, i.e., 14% w/w PEG 1500, 18% w/w potassium phosphate, 80 mL/min of nitrogen flow rate and pH 7, maximum yield of 91.47% and purification fold of 4.26 were obtained. ATPF was found to be an effective technique for the purification of bromelain from pineapple fruit with higher extraction yield and purification fold as compared to aqueous two phase extraction (ATPE).     

Comparison of isopropanol and hexane for extraction of vitamin E and oryzanols from stabilized rice bran

The effects of solvent-to-bran ratio (2∶1 and 3∶1, w/w), extraction temperature (40 and 60°C), and time (5, 10, 15, 20, and 30 min) were studied for hexane and isopropanol extraction. Increasing the solvent-to-bran ratios and extraction temperature increased the amounts of crude oil, vitamin E and oryzanol recovered for both solvents. An extraction time of 15 min was sufficient for optimum crude oil, vitamin E, and oryzanol extraction. Preheated isopropanol (3∶1 solvent/bran ratio and 60°C) extracted less crude oil (P<.05) but more vitamin E (P<.05) and similar amounts of oryzanol (P>.05) relative to preheated hexane. The data suggest that isopropanol is a promising alternative solvent to hexane for extraction of oil from stabilized rice bran.     

DNNSA反胶团萃取湿法磷酸中Fe3＋的机理研究

对萃取剂二壬基萘磺酸(DNNSA)萃取分离湿法磷酸中Fe3 的性能和机理做了初步研究.考察了萃取剂浓度c(HD)、水相酸度w(P2O5)、反应温度、油相和水相体积比V(O/A)等因素对萃取率的影响,并用斜率法研究了萃取剂浓度和水相酸度对萃取平衡的影响.试验结果表明,萃取剂浓度越高,萃取效果越好;在高、低酸度时,HD分别与Fe3 和FeHPO 4进行反应,并生成不同的萃合物 FeD3·5HD和FeHPO4D·7HD,表明其萃取机理受酸浓度的影响而发生了变化.