[Study on condition for extraction of arctiin from fruits of Arctium lappa using supercritical fluid extraction].

Science.gov (United States)

Dong, Wen-hong; Liu, Ben

2006-08-01

To study the feasibility of supercritical fluid extraction (SFE) for arctiin from the fruits of Arctium lappa. The extracts were analyzed by HPLC, optimum extraction conditions were studied by orthogonal tests. The optimal extraction conditions were: pressure 40 MPa, temperature 70 degrees C, using methanol as modifier carrier at the rate of 0.55 mL x min(-1), static extraction time 5 min, dynamic extraction 30 min, flow rate of CO2 2 L x min(-1). SFE has the superiority of adjustable polarity, and has the ability of extracting arctiin.

Steps of Supercritical Fluid Extraction of Natural Products and Their Characteristic Times

OpenAIRE

Sovová, H. (Helena)

2012-01-01

Kinetics of supercritical fluid extraction (SFE) from plants is variable due to different micro-structure of plants and their parts, different properties of extracted substances and solvents, and different flow patterns in the extractor. Variety of published mathematical models for SFE of natural products corresponds to this diversification. This study presents simplified equations of extraction curves in terms of characteristic times of four single extraction steps: internal diffusion, exter...

Intraspecific variability of Holostylis reniformis: concentration of lignans, as determined by maceration and supercritical fluid extraction (SFE-CO{sub 2}), as a function of plant provenance and plant parts

Energy Technology Data Exchange (ETDEWEB)

Martins, Gislaine F.; Pereira, Marcos D.P.; Lopes, Lucia M.X., E-mail: lopesxl@iq.unesp.br [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP), Araraquara, SP (Brazil). Instituto de Quimica; Silva, Tito da [Universidade Federal do Maranhao (UFMA), Imperatriz, MA (Brazil). Centro de Ciencias Sociais, Saude e Tecnologia; Rosa, Paulo de T. Vieira e; Barbosa, Fernanda P. [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Instituto de Quimica; Messiano, Gisele B. [Instituto Federal de Sao Paulo, SP (Brazil); Krettli, Antoniana U. [Fundacao Oswaldo Cruz (FIOCRUZ), Belo Horizonte, MG (Brazil). Instituto Rene Rachou

2014-04-15

Maceration and supercritical fluid extraction were used to prepare extracts from parts of plants (Holostylis reniformis) collected in two different regions of Brazil. {sup 1}H NMR, HPLC-DAD-ESI/MS, HPLC-DAD, GC-MS, and chemometric techniques were used to analyse lignans in the extracts and showed that yields of SFE-CO{sub 2} were less than or equal to those of hexane maceration extracts. These analyses, in conjunction with the concentrations of aliphatic hydrocarbons, fatty acids and their methyl and ethyl derivatives in the extracts, also allowed the chemical composition of parts and provenance of the plant to be differentiated. (author)

The use of supercritical fluid extraction as a sample preparation technique for soils

International Nuclear Information System (INIS)

Levy, J.M.; Dolata, L.A.; Rosselli, A.C.; Ravey, R.M.

1994-01-01

Using off-line supercritical fluid extraction (SFE), polynuclear aromatic hydrocarbons (PAHs) were extracted at different levels from various soil and sediment matrices. Based upon GC/MS measurements a number of SFE operational parameters including pressure, temperature and flow rate, were optimized to yield the highest efficiencies with the best precision

Evaluation of supercritical fluid extraction/gas chromatography/matrix isolation-infrared spectrometry for analysis of organic compounds

International Nuclear Information System (INIS)

Bopari, A.S.; Bierma, D.R.; Applegate, D.V.

1991-01-01

Analysis of soil samples for organic compounds typically first requires Soxhlet extraction or sonication. These processes are time consuming and generate large amounts of waste solvent. Supercritical fluid extraction (SFE), which uses a supercritical fluid such as carbon dioxide, has recently been shown to extract organic compounds from soil samples in good yields. Moreover, SFE does not generate waste solvent and can be performed rapidly. Gas Chromatography/Matrix Isolation-Infrared Spectrometry (GC/MI-IR) has been used in our laboratories for determining organic compounds present in extracts from various matrices. The authors have interfaced an SFE extraction apparatus to GC/MI-IR instruments. In this paper the utility of SPE/GC/MI-IR instrumentation is discussed

Extraction of uranium from simulated ore by the supercritical carbon dioxide fluid extraction method with nitric acid-TBP complex

International Nuclear Information System (INIS)

Dung, Le Thi Kim; Imai, Tomoki; Tomioka, Osamu; Nakashima, Mikio; Takahashi, Kuniaki; Meguro, Yoshihiro

2006-01-01

The supercritical fluid extraction (SFE) method using CO 2 as a medium with an extractant of HNO 3 -tri-n-butyl phosphate (TBP) complex was applied to extract uranium from several uranyl phosphate compounds and simulated uranium ores. An extraction method consisting of a static extraction process and a dynamic one was established, and the effects of the experimental conditions, such as pressure, temperature, and extraction time, on the extraction of uranium were ascertained. It was found that uranium could be efficiently extracted from both the uranyl phosphates and simulated ores by the SFE method using CO 2 . It was thus demonstrated that the SFE method using CO 2 is useful as a pretreatment method for the analysis of uranium in ores. (author)

Remediation of flare pit soils using supercritical fluid extraction

Energy Technology Data Exchange (ETDEWEB)

Nagpal, V.; Guigard, S.E. [Alberta Univ., Edmonton, AB (Canada). Dept. of Civil Engineering

2005-09-01

A laboratory study was conducted to examine the ability of supercritical fluid extraction (SFE) to remove petroleum hydrocarbons (PHCs) from two flare pit soils in Alberta. SFE is a technology for remediation of contaminated soils. In order to determine the optimal extraction conditions and to understand the effects of pressure, temperature, supercritical carbon dioxide flow rate, soil type, and extraction time on the extraction efficiency of SFE, extractions were performed on two flare pit soils at various pressures and temperatures. Chemicals in the study included diesel oil, SAE 10-30W motor oil, n-decane, hexadecane, tetratriacontane and pentacontane. The best extraction conditions were defined as conditions that result in a treated soil with a PHC concentration that meets the regulatory guidelines of the Canadian Council of Ministers of the Environment in the Canada-wide standard for PHC is soil. The study results indicate that the efficiency of the SFE process is solvent-density dependent for the conditions studied. The highest extraction efficiency for both soils was obtained at conditions of 24.1 MPa and 40 degrees C. An increase in pressure at a fixed temperature led to an increase in the extraction efficiency while an increase in temperature at a fixed pressure led to a decrease in the extraction efficiency. The treated soils were observed to be lighter in colour, drier, and grainier than the soil prior to extraction. It was concluded that SFE is an effective method for remediating flare pit soils. 63 refs., 4 tabs., 5 figs.

Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction.

Science.gov (United States)

Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim

2017-01-01

The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%-61.85%) and oleic acid (1.64%-18.97%). Thymoquinone (0.72%-21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly ( P essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique.

Rapid Determination of Two Triterpenoid Acids in Chaenomelis Fructus Using Supercritical Fluid Extraction On-line Coupled with Supercritical Fluid Chromatography.

Science.gov (United States)

Zhang, Xiaotian; Ji, Feng; Li, Yueqi; He, Tian; Han, Ya; Wang, Daidong; Lin, Zongtao; Chen, Shizhong

2018-01-01

In this study, an on-line supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) method was developed for the rapid determination of oleanoic acid and ursolic acid in Chaenomelis Fructus. After optimization of the conditions, the two triterpenoid acids was obtained by SFE using 20% methanol as a modifier at 35°C in 8 min. They were resolved on a Shim-pack UC-X Diol column (4.6 × 150 mm, 3 μm) in 14 min (0 - 10 min, 5 - 10%; 10 - 14 min, 10% methanol in CO 2 ) with a backpressure of 15 MPa at 40°C. The on-line SFE-SFC method could be completed within 40 min (10.79 mg/g dry plant, R s = 2.36), while the ultrasound-assisted extraction and HPLC method required at least 90 min (3.55 mg/g dry plant, R s = 1.92). This on-line SFE-SFC method is powerful to simplify the pre-processing and quantitative analysis of natural products.

On-line supercritical fluid extraction-supercritical fluid chromatography-mass spectrometry of polycyclic aromatic hydrocarbons in soil.

Science.gov (United States)

Wicker, A Paige; Carlton, Doug D; Tanaka, Kenichiro; Nishimura, Masayuki; Chen, Vivian; Ogura, Tairo; Hedgepeth, William; Schug, Kevin A

2018-06-01

On-line supercritical fluid extraction - supercritical fluid chromatography - mass spectrometry (SFE-SFC-MS) has been applied for the determination of polycyclic aromatic hydrocarbons (PAHs) in soil. The purpose of this study was to develop and validate the first on-line SFE-SFC-MS method for the quantification of PAHs in various types of soil. By coupling the sample extraction on-line with chromatography and detection, sample preparation is minimized, diminishing sample loss and contamination, and significantly decreasing the required extraction time. Parameters for on-line extraction coupled to chromatographic analysis were optimized. The method was validated for concentrations of 10-1500 ng of PAHs per gram of soil in Certified Reference Material (CRM) sediment, clay, and sand with R 2  ≥ 0.99. Limits of detection (LOD) were found in the range of 0.001-5 ng/g, and limits of quantification (LOQ) in the range of 5-15 ng/g. The method developed in this study can be effectively applied to the study of PAHs in the environment, and may lay the foundation for further applications of on-line SFE-SFC-MS. Copyright © 2018 Elsevier B.V. All rights reserved.

Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction

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Ghahramanloo KH

2017-07-01

Full Text Available Kourosh Hasanzadeh Ghahramanloo,1 Behnam Kamalidehghan,2 Hamid Akbari Javar,3 Riyanto Teguh Widodo,1 Keivan Majidzadeh,4 Mohamed Ibrahim Noordin1 1Department of Pharmacy, Faculty of Medicine, University of Malaya, Kuala Lumpur, Malaysia; 2Medical Genetics Department, National Institute of Genetic Engineering and Biotechnology (NIGEB, 3Department of Pharmaceutics, Faculty of Pharmacy, Tehran University of Medical Sciences (TUMS, 4Breast Cancer Research Center (BCRC Academic Center for Education, Culture and Research, Tehran, Iran Abstract: The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%–61.85% and oleic acid (1.64%–18.97%. Thymoquinone (0.72%–21.03% was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly (P<0.05 higher than that achieved by the solvent extraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique. Keywords: Nigella sativa L., essential oil extraction, supercritical fluid extraction, solvent extraction, fatty acid composition, thymoquinone, linoleic acid

Sustainable extraction of molecules for potable alcohol, cosmetics and pharmaceuticals: extraction in supercritical fluids

International Nuclear Information System (INIS)

Leone, Gian Paolo; Ferri, Donatella

2015-01-01

Since many years the Laboratory of Agro-Industrial Innovation (UTAGRI-INN) ENEA proposed research and development of extraction processes with supercritical fluids (SFE, Supercritical Fluid Extraction), aiming on the sustainability of the process characteristics. The technique, in fact, makes no use of organic solvents, It has reduced energy consumption and requires a number of process step lower than the extractions traditional. The process also responds to the requirements required by the regulations for food use, cosmetics and pharmaceutical extracts. [it

Sustainable extraction of molecules for human food, cosmetic and pharmaceutical products: extraction in supercritical fluids

International Nuclear Information System (INIS)

Leone, GianPaolo; Ferri, Donatella

2015-01-01

Since several years, the ENEA Innovation Laboratory for Agro-Industrial, proposed activities of research and development of extraction processes with supercritical fluids (SFE, Supercritical Fluid Extraction), focusing on sustainability characteristics of the process. The technique, in fact, makes no use of organic solvents, has a low energy consumption and requires a lower number of process steps compared to conventional extractions. The process also responds to the requirements imposed by the legislation for human food, cosmetic and pharmaceutical extracts. [it

Optimization of microwave-assisted extraction and supercritical fluid extraction of carbamate pesticides in soil by experimental design methodology.

Science.gov (United States)

Sun, Lei; Lee, Hian Kee

2003-10-03

Orthogonal array design (OAD) was applied for the first time to optimize microwave-assisted extraction (MAE) and supercritical fluid extraction (SFE) conditions for the analysis of four carbamates (propoxur, propham, methiocarb, chlorpropham) from soil. The theory and methodology of a new OA16 (4(4)) matrix derived from a OA16 (2(15)) matrix were developed during the MAE optimization. An analysis of variance technique was employed as the data analysis strategy in this study. Determinations of analytes were completed using high-performance liquid chromatography (HPLC) with UV detection. Four carbamates were successfully extracted from soil with recoveries ranging from 85 to 105% with good reproducibility (approximately 4.9% RSD) under the optimum MAE conditions: 30 ml methanol, 80 degrees C extraction temperature, and 6-min microwave heating. An OA8 (2(7)) matrix was employed for the SFE optimization. The average recoveries and RSD of the analytes from spiked soil by SFE were 92 and 5.5%, respectively except for propham (66.3+/-7.9%), under the following conditions: heating for 30 min at 60 degrees C under supercritical CO2 at 300 kg/cm2 modified with 10% (v/v) methanol. The composition of the supercritical fluid was demonstrated to be a crucial factor in the extraction. The addition of a small volume (10%) of methanol to CO2 greatly enhanced the recoveries of carbamates. A comparison of MAE with SFE was also conducted. The results indicated that >85% average recoveries were obtained by both optimized extraction techniques, and slightly higher recoveries of three carbamates (propoxur, propham and methiocarb) were achieved using MAE. SFE showed slightly higher recovery for chlorpropham (93 vs. 87% for MAE). The effects of time-aged soil on the extraction of analytes were examined and the results obtained by both methods were also compared.

COMPARISONS OF SOXHLET EXTRACTION, PRESSURIZED LIQUID EXTRACTION, SUPERCRITICAL FLUID EXTRACTION, AND SUBCRITICAL WATER EXTRACTION FOR ENVIRONMENTAL SOLIDS: RECOVERY, SELECTIVITY, AND EFFECTS ON SAMPLE MATRIX. (R825394)

Science.gov (United States)

Extractions of a polycyclic aromatic hydrocarbon (PAH)-contaminated soil from a former manufactured gas plant site were performed with a Soxhlet apparatus (18 h), by pressurized liquid extraction (PLE) (50 min at 100°C), supercritical fluid extraction (SFE) (1 h at 150°...

SUPERCRITICAL FLUID EXTRACTION OF POLYCYCLIC AROMATIC HYDROCARBON MIXTURES FROM CONTAMINATED SOILS

Science.gov (United States)

Highly contaminated (with PAHs) topsoils were extracted with supercritical CO2 to determine the feasibility and mechanism of supercritical fluid extraction (SFE). Effect of SCF density, temperature, cosolvent type and amount, and of slurrying the soil with water were ...

Multivessel supercritical fluid extraction of food items in Total Diet Study.

Science.gov (United States)

Hopper, M L; King, J W; Johnson, J H; Serino, A A; Butler, R J

1995-01-01

An off-line, large capacity, multivessel supercritical fluid extractor (SFE) was designed and constructed for extraction of large samples. The extractor can simultaneously process 1-6 samples (15-25 g) by using supercritical carbon dioxide (SC-CO2), which is relatively nontoxic and nonflammable, as the solvent extraction medium. Lipid recoveries for the SFE system were comparable to those obtained by blending or Soxhlet extraction procedures. Extractions at 10,000 psi, 80 degrees C, expanded gaseous CO2 flow rates of 4-5 L/min (35 degrees C), and 1-3 h extraction times gave reproducible lipid recoveries for pork sausage (relative standard deviation [RSD], 1.32%), corn chips (RSD, 0.46%), cheddar cheese (RSD, 1.14%), and peanut butter (RSD, 0.44%). In addition, this SFE system gave reproducible recoveries (> 93%) for butter fortified with cis-chlordane and malathion at the 100 ppm and 0.1 ppm levels. Six portions each of cheddar cheese, saltine crackers, sandwich cookies, and ground hamburger also were simultaneously extracted with SC-CO2 and analyzed for incurred pesticide residues. Results obtained with this SFE system were reproducible and comparable with results from organic-solvent extraction procedures currently used in the Total Diet Study; therefore, use and disposal of large quantities of organic solvents can be eliminated.

Supercritical fluid extraction of phenolic compounds and antioxidants from grape (Vitis labrusca B.) seeds.

Science.gov (United States)

Ghafoor, Kashif; Al-Juhaimi, Fahad Y; Choi, Yong Hee

2012-12-01

Supercritical fluid extraction (SFE) technique was applied and optimized for temperature, CO₂ pressure and ethanol (modifier) concentration using orthogonal array design and response surface methodology for the extract yield, total phenols and antioxidants from grape (Vitis labrusca B.) seeds. Effects of extraction temperature and pressure were found to be significant for all these response variables in SFE process. Optimum SFE conditions (44 ~ 46 °C temperature and 153 ~ 161 bar CO₂ pressure) along with ethanol (extract yield (12.09 %), total phenols (2.41 mg GAE/ml) and antioxidants (7.08 mg AAE/ml), were used to obtain extracts from grape seeds. The predicted values matched well with the experimental values (12.32 % extract yield, 2.45 mg GAE/ml total phenols and 7.08 mg AAE/ml antioxidants) obtained at optimum SFE conditions. The antiradical assay showed that SFE extracts of grape seeds can scavenge more than 85 % of 1, 1-diphenyl-2-picrylhydrazyl (DPPH) radicals. The grape seeds extracts were also analyzed for hydroxybenzoic acids which included gallic acid (1.21 ~ 3.84 μg/ml), protocatechuic acid (3.57 ~ 11.78 μg/ml) and p-hydroxybenzoic acid (206.72 ~ 688.18 μg/ml).

Supercritical fluid extraction of uranium and neodymium nitrates

International Nuclear Information System (INIS)

Sujatha, K.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R.

2011-01-01

Supercritical fluid extraction (SFE) of uranyl nitrate and neodymium nitrate salts from a mixture was investigated in the present study using Sc-CO 2 modified with various ligands such as organophosphorous compounds, amides, and diketones. Preferential extraction of uranyl nitrate over neodymium nitrate was demonstrated using Sc-CO 2 modified with amide, di-(2ethylhexyl) isobutyramide (D2EHIBA). (author)

Characterization of Arachis hypogaea L. oil obtained from different extraction techniques and in vitro antioxidant potential of supercritical fluid extraction extract

Directory of Open Access Journals (Sweden)

Rishika Chauhan

2016-01-01

Full Text Available Aim: The present investigation was aimed to characterize the fixed oil of Arachis hypogaea L. using five different extraction methods: Supercritical fluid extraction (SFE, ultrasound assistance extraction, soxhlet extraction, solvent extraction, and three phase partitioning method. Materials and Methods: The SFE conditions (temperature, pressure, and volume of CO 2 were optimized prior for better yield. The extracted oils were analyzed and compared for their physiochemical parameters, high-performance thin layer chromatography (HPTLC, gas chromatography-mass spectrometry (GC-MS, and Fourier transform infrared spectrometry (FT-IR fingerprinting. Anti-oxidant activity was also determined using DPPH and superoxide scavenging method. Results: The main fatty acids were oleic, linoleic, palmitic, and stearic acids as obtained by GC-MS. HPTLC analysis revealed the presence of similar major components in chromatograms. Similarly, the pattern of peaks as obtained in FT-IR and GC-MS spectra of same oils by different extraction methods was superimposable. Conclusion: Analysis reported that the fixed oil of A. hypogaea L. is a good source of unsaturated fatty acid, mainly n-6 and n-9 fatty acid with a significant antioxidant activity of oil obtained from SFE extraction method.

Optimization of co-solvent addition in supercritical fluid extraction of fat with carbon dioxide

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Ivanov Dušica S.

2011-01-01

Full Text Available This investigation is concerned with supercritical fluid extraction (SFE using CO2, as an analytical technique for total fat extraction from food and feed samples. Its most significant advantages are safety, cleanness, and shorter extraction time. The main limitation of this technique includes the difficulty of extracting polar lipids due to the non-polar character of the solvent (CO2 used for the extraction. The influence of ethanol as a co-solvent on the SFE of mash pig feed was investigated in this paper. Total fat content was determined by SFE and Soxhlet method for ten commercially available mesh pig feeds. Yields of the fat extracted by both methods were plotted one against the other and compared. Statistically significant difference (p ≤ 0.05 has been found only between the total fat obtained by the Soxhlet extraction and SFE by pure CO2. Based on the mathematical model, maximum yield of the extracted fat is achieved at an ethanol addition of 0.67 ml/g of sample, when the other parameters are the same as recommended by the producer’s procedure.

Comparison study of moisture content, colour properties and essential oil compounds extracted by hydrodistillation and supercritical fluid extraction between stem and leaves of lemongrass (Cymbopogun citratus)

Science.gov (United States)

Kamaruddin, Shazlin; Mustapha, Wan Aida Wan; Haiyee, Zaibunnisa Abdul

2018-04-01

The objectives of this study were to compare the properties of moisture content, colour and essential oil compounds between stem and leaves of lemongrass (Cymbopogun citratus). The essential oil was extracted using two different methods which are hydrodistillation and supercritical fluid extraction (SFE). There was no significant difference of moisture content between stem and leaves of lemongrass. The lightness (L) and yellowness (+b) values of the stems were significantly higher (pleaves. The highest yield of essential oil was obtained by extraction using supercritical fluid extraction (SFE) in leaves (˜ 0.7%) by treatment at 1700psi and 50°C. The main compound of extracted essential oil was citral (geranial and neral).

Studies on supercritical fluid extraction of uranium from sodium diuranate

International Nuclear Information System (INIS)

Prabhat, Parimal; Vithal, G.K.; Rao, Ankita; Kumar, Pradeep; Tomar, B.S.

2014-01-01

Crude sodium diuranate (SDU) produced from phosphoric acid by solvent extraction process with di-2-ethyl hexyl phosphoric acid (D2EHPA) and tri-n-butyl phosphate(TBP) contains iron and other rare earth impurities along with uranium. For further use of this uranium for fuel fabrication and its subsequent use in nuclear reactors, it has to be purified up to nuclear grade ammonium diuranate (ADU) specifications. Conventionally crude SDU is being purified by dissolving it in nitric acid followed by solvent extraction process using TBP in diluent. Use of large amount of acid and organic solvents for industrial processes is an environmental concern. Nowadays there are efforts to minimize use of acid and organic solvents in industrial processes. Supercritical Fluid Extraction (SFE) of uranium from different matrices (solid as well as liquid) has been reported by several authors in recent years. Near complete extraction of uranium from UO 2 (powder, green pellet and sintered pellet) using TBP-HNO 3 adduct by SFE has been reported. We attempted to explore possibility to purify crude SDU to nuclear grade by SFE of uranium from crude SDU matrix and study the effect of different operational parameters, mode of extraction and complexation

Supercritical fluid extraction from spent coffee grounds and coffee husks: antioxidant activity and effect of operational variables on extract composition.

Science.gov (United States)

Andrade, Kátia S; Gonçalvez, Ricardo T; Maraschin, Marcelo; Ribeiro-do-Valle, Rosa Maria; Martínez, Julian; Ferreira, Sandra R S

2012-01-15

The present study describes the chemical composition and the antioxidant activity of spent coffee grounds and coffee husks extracts, obtained by supercritical fluid extraction (SFE) with CO(2) and with CO(2) and co-solvent. In order to evaluate the high pressure method in terms of process yield, extract composition and antioxidant activity, low pressure methods, such as ultrasound (UE) and soxhlet (SOX) with different organic solvents, were also applied to obtain the extracts. The conditions for the SFE were: temperatures of 313.15K, 323.15K and 333.15K and pressures from 100 bar to 300 bar. The SFE kinetics and the mathematical modeling of the overall extraction curves (OEC) were also investigated. The extracts obtained by LPE (low pressure extraction) with ethanol showed the best results for the global extraction yield (X(0)) when compared to SFE results. The best extraction yield was 15±2% for spent coffee grounds with ethanol and 3.1±04% for coffee husks. The antioxidant potential was evaluated by DPPH method, ABTS method and Folin-Ciocalteau method. The best antioxidant activity was showed by coffee husk extracts obtained by LPE. The quantification and the identification of the extracts were accomplished using HPLC analysis. The main compounds identified were caffeine and chlorogenic acid for the supercritical extracts from coffee husks. Copyright © 2011 Elsevier B.V. All rights reserved.

Studies on In-situ Chelation/Supercritical Fluid Extraction of Lanthanides and Actinides Using a Radiotracer Technique

International Nuclear Information System (INIS)

Lin, Yuehe; Wu, Hong; Smart, Neil G.; Wai, Chien M.

2001-01-01

Radioisotope tracer techniques were used to study the process of in-situ chelation/supercritical fluid extraction(SFE) of La3+ and Lu3+ from solid matrix using mixed ligand hexafluoroacetylacetone (HFA) and tributylphosphate (TBP) as chelating agents. A lab-built SFE extactor was used in this study and the extractor design was optimized based on the experimental results. Quantitative recovery of La and Lu was achieved when the extrator design was optimized. Extraction of uranium from real world samples was also investigated to demonstrate the capability of this chelation/SFE technology for environmental remediation applications. A novel on-line back extraction technique for the recovery of metal ions and regeneration of ligands is also reported.

Extraction of Plutonium From Spiked INEEL Soil Samples Using the Ligand-Assisted Supercritical Fluid Extraction (LA-SFE) Technique

International Nuclear Information System (INIS)

Fox, R.V.; Mincher, B.J.; Holmes, R.G.G.

1999-01-01

In order to investigate the effectiveness of ligand-assisted supercritical fluid extraction for the removal of transuranic contaminations from soils an Idaho National Engineering and Environmental Laboratory (INEEL) silty-clay soil sample was obtained from near the Radioactive Waste Management Complex area and subjected to three different chemical preparations before being spiked with plutonium. The spiked INEEL soil samples were subjected to a sequential aqueous extraction procedure to determine radionuclide portioning in each sample. Results from those extractions demonstrate that plutonium consistently partitioned into the residual fraction across all three INEEL soil preparations whereas americium partitioned 73% into the iron/manganese fraction for soil preparation A, with the balance partitioning into the residual fraction. Plutonium and americium were extracted from the INEEL soil samples using a ligand-assisted supercritical fluid extraction technique. Initial supercritical fluid extraction runs produced plutonium extraction technique. Initial supercritical fluid extraction runs produced plutonium extraction efficiencies ranging from 14% to 19%. After a second round wherein the initial extraction parameters were changed, the plutonium extraction efficiencies increased to 60% and as high as 80% with the americium level in the post-extracted soil samples dropping near to the detection limits. The third round of experiments are currently underway. These results demonstrate that the ligand-assisted supercritical fluid extraction technique can effectively extract plutonium from the spiked INEEL soil preparations

Field—Based Supercritical Fluid Extraction of Hydrocarbons at Industrially Contaminated Sites

Directory of Open Access Journals (Sweden)

Peggy Rigou

2002-01-01

Full Text Available Examination of organic pollutants in groundwaters should also consider the source of the pollution, which is often a solid matrix such as soil, landfill waste, or sediment. This premise should be viewed alongside the growing trend towards field-based characterisation of contaminated sites for reasons of speed and cost. Field-based methods for the extraction of organic compounds from solid samples are generally cumbersome, time consuming, or inefficient. This paper describes the development of a field-based supercritical fluid extraction (SFE system for the recovery of organic contaminants (benzene, toluene, ethylbenzene, and xylene and polynuclear aromatic hydrocarbons from soils. A simple, compact, and robust SFE system has been constructed and was found to offer the same extraction efficiency as a well-established laboratory SFE system. Extraction optimisation was statistically evaluated using a factorial analysis procedure. Under optimised conditions, the device yielded recovery efficiencies of >70% with RSD values of 4% against the standard EPA Soxhlet method, compared with a mean recovery efficiency of 48% for a commercially available field-extraction kit. The device will next be evaluated with real samples prior to field deployment.

Supercritical fluid extraction of uranium and thorium employing dialkyl amides

International Nuclear Information System (INIS)

Rao, Ankita; Kumar, Pradeep

2014-01-01

Extraction and purification of actinides from different matrices is of utmost importance to the nuclear industry. In recent decades, supercritical fluid extraction (SFE) has emerged as a promising alternative to solvent extraction owing to its inherent potential of minimization of liquid waste generation. N,N-dialkyl aliphatic amides have been proposed to be an alternative to TBP in the reprocessing of spent nuclear fuel due to several attractive features like innocuous nature of degradation products (mainly carboxylic acids/ amines), possibility of complete incineration of the used extractant leading to reduction in volume of secondary waste. Also, physico-chemical properties of this class of extractants can be tuned by the judicious choice of alkyl groups. In the present work, N,N-dialkyl aliphatic amides with varying alkyl groups viz. N,N-dibutyl-2-ethylhexanamide (DBEHA), N,N-dibutyl-3,3-dimethylbutanamide (DBDMBA), N,N-dihexyloctanamide (DHOA), N,N-disecbutylpentamide (DBPA), N,N-dibutyloctanamide (DBOA), have been evaluated for supercritical fluid extraction (SFE) of uranium and thorium from nitric acid medium as well as tissue paper matrix. Amides were obtained from Department of Chemistry, Delhi University and were used as such. This fact could be exploited for separation of thorium and uranium

Supercritical fluid extraction of selected pharmaceuticals from water and serum.

Science.gov (United States)

Simmons, B R; Stewart, J T

1997-01-24

Selected drugs from benzodiazepine, anabolic agent and non-steroidal anti-inflammatory drug (NSAID) therapeutic classes were extracted from water and serum using a supercritical CO2 mobile phase. The samples were extracted at a pump pressure of 329 MPa, an extraction chamber temperature of 45 degrees C, and a restrictor temperature of 60 degrees C. The static extraction time for all samples was 2.5 min and the dynamic extraction time ranged from 5 to 20 min. The analytes were collected in appropriate solvent traps and assayed by modified literature HPLC procedures. Analyte recoveries were calculated based on peak height measurements of extracted vs. unextracted analyte. The recovery of the benzodiazepines ranged from 80 to 98% in water and from 75 to 94% in serum. Anabolic drug recoveries from water and serum ranged from 67 to 100% and 70 to 100%, respectively. The NSAIDs were recovered from water in the 76 to 97% range and in the 76 to 100% range from serum. Accuracy, precision and endogenous peak interference, if any, were determined for blank and spiked serum extractions and compared with classical sample preparation techniques of liquid-liquid and solid-phase extraction reported in the literature. For the benzodiazepines, accuracy and precision for supercritical fluid extraction (SFE) ranged from 1.95 to 3.31 and 0.57 to 1.25%, respectively (n = 3). The SFE accuracy and precision data for the anabolic agents ranged from 4.03 to 7.84 and 0.66 to 2.78%, respectively (n = 3). The accuracy and precision data reported for the SFE of the NSAIDs ranged from 2.79 to 3.79 and 0.33 to 1.27%, respectively (n = 3). The precision of the SFE method from serum was shown to be comparable to the precision obtained with other classical preparation techniques.

Supercritical fluid extraction of uranium for its purification from various yellow cake matrices

International Nuclear Information System (INIS)

Prabhat, Parimal; Rao, Ankita; Tomar, B.S.; Kumar, Pradeep

2016-01-01

Uranium is produced from different uranium ores as crude yellow cake of different chemical composition such as sodium diuranate (SDU), ammonium diuranate (ADU), magnesium diuranate (MDU), high temperature uranium peroxide (HTUP) etc. This depends on nature of ores and ore processing methods, availability of required facilities at processing site and other economic as well as environmental factors. These yellow cakes are further processed to produce pure uranium suitable for fuel fabrication facility by conventional solvent extraction process. Supercritical Fluid Extraction (SFE) is being developed as an alternate method for separation in nuclear fields due to its inherent potential to minimize liquid waste generation and process simplification. In present study, SFE of uranium from various yellowcake of different chemical composition has been carried out. Chemical parameter such as effect of TBP amount on SFE of uranium has been carried out and optimized at 2 ml for 200 mg SDU. Instrumental parameter such as temperature and pressure on SFE of uranium has been optimized at 323 K and 15.2 MPa. Extraction efficiency (%) achieved at optimized condition is 91.45 ± 0.2, 97.01 ± 0.75 and 96.72 ± 0.27 for SDU, MDU and HTUP respectively. Purity of uranium before SFE and after has been compared. Further studies is in progress for better understanding of chemical composition of matrix on SFE of uranium and improving purity of uranium separated from this route. (author)

Supercritical fluid extraction: spectroscopic study of interactions comparison to solvent extraction

Energy Technology Data Exchange (ETDEWEB)

Rustenholtz Farawila, A

2005-06-15

Supercritical fluid carbon dioxide (SF-CO{sub 2}) was chosen to study Supercritical Fluid Extraction (SFE) of cesium and uranium. At first, crown ethers were considered as chelating agents for the SFE of cesium. The role of water and its interaction with crown ethers were especially studied using Fourier-Transform Infra-Red (FT-IR) spectroscopy in SF-CO{sub 2}. A sandwich configuration between two crown ethers and a water molecule was observed in the SF-CO{sub 2} phase for the first time. The equilibrium between the single and the bridge configurations was defined. The enthalpy of the hydrogen bond formation was also calculated. These results were then compared to the one in different mixtures of chloroform and carbon tetra-chloride using Nuclear Magnetic Resonance (NMR). To conclude this first part and in order to understand the whole picture of the recovery of cesium, I studied the role of water in the equilibrium between the cesium and the di-cyclo-hexano18-crown-6.In a second part, the supercritical fluid extraction of uranium was studied in SF-CO{sub 2}. For this purpose, different complexes of Tributyl Phosphate (TBP), nitric acid and water were used as chelating and oxidizing agents. I first used FT-IR to study the TBP-water interaction in SF-CO{sub 2}. These results were then compared to the one obtained with NMR in chloroform. NMR spectroscopy was also used to understand the TBP-nitric acid-water interaction first alone and then in chloroform. To conclude my research work, I succeeded to improve the efficiency of uranium extraction and stripping into water for a pilot-plant where enriched uranium is extracted from incinerated waste coming from nuclear fuel fabrication. TBP-nitric acid complexes were used in SF-CO{sub 2} for the extraction of uranium from ash. (author)

Supercritical fluid extraction: spectroscopic study of interactions comparison to solvent extraction

International Nuclear Information System (INIS)

Rustenholtz Farawila, A.

2005-06-01

Supercritical fluid carbon dioxide (SF-CO 2 ) was chosen to study Supercritical Fluid Extraction (SFE) of cesium and uranium. At first, crown ethers were considered as chelating agents for the SFE of cesium. The role of water and its interaction with crown ethers were especially studied using Fourier-Transform Infra-Red (FT-IR) spectroscopy in SF-CO 2 . A sandwich configuration between two crown ethers and a water molecule was observed in the SF-CO 2 phase for the first time. The equilibrium between the single and the bridge configurations was defined. The enthalpy of the hydrogen bond formation was also calculated. These results were then compared to the one in different mixtures of chloroform and carbon tetra-chloride using Nuclear Magnetic Resonance (NMR). To conclude this first part and in order to understand the whole picture of the recovery of cesium, I studied the role of water in the equilibrium between the cesium and the di-cyclo-hexano18-crown-6.In a second part, the supercritical fluid extraction of uranium was studied in SF-CO 2 . For this purpose, different complexes of Tributyl Phosphate (TBP), nitric acid and water were used as chelating and oxidizing agents. I first used FT-IR to study the TBP-water interaction in SF-CO 2 . These results were then compared to the one obtained with NMR in chloroform. NMR spectroscopy was also used to understand the TBP-nitric acid-water interaction first alone and then in chloroform. To conclude my research work, I succeeded to improve the efficiency of uranium extraction and stripping into water for a pilot-plant where enriched uranium is extracted from incinerated waste coming from nuclear fuel fabrication. TBP-nitric acid complexes were used in SF-CO 2 for the extraction of uranium from ash. (author)

Characterization of Linum usitatissimum L. oil obtained from different extraction technique and in vitro antioxidant potential of supercritical fluid extract

Science.gov (United States)

Chauhan, Rishika; Chester, Karishma; Khan, Yasmeen; Tamboli, Ennus Tajuddin; Ahmad, Sayeed

2015-01-01

Aim: Present investigation was aimed to characterize the fixed oil of Linum usitatissimum L. using five different extraction methods: Supercritical fluid extraction (SFE), ultrasound-assistance, soxhlet extraction, solvent extraction, and three phase partitioning method. Materials and Methods: The SFE conditions (temperature, pressure, and volume of CO2) were optimized prior for better yield. The extracted oils were analyzed and compared for their physiochemical parameters, high performance thin layer chromatography (HPTLC), gas chromatography-mass spectrometry (GC-MS), and Fourier-transformed infrared spectroscopy (FT-IR) fingerprinting. Antioxidant activity was also determined using 1,1-diphenyl-2-picrylhydrazyl and superoxide scavenging method. Result: The main fatty acids were α-linolenic acid, linoleic acid, palmitic acid, and stearic acid as obtained by GC-MS. HPTLC analysis revealed the presence of similar major components in chromatograms. Similarly, the pattern of peaks, as obtained in FT-IR and GC-MS spectra of same oils by different extraction methods, were superimposable. Conclusion: Analysis reported that the fixed oil of L. usitatissimum L. is a good source of n-3 fatty acid with the significant antioxidant activity of oil obtained from SFE extraction method. PMID:26681884

Characterization of Linum usitatissimum L. oil obtained from different extraction technique and in vitro antioxidant potential of supercritical fluid extract

Directory of Open Access Journals (Sweden)

Rishika Chauhan

2015-01-01

Full Text Available Aim: Present investigation was aimed to characterize the fixed oil of Linum usitatissimum L. using five different extraction methods: Supercritical fluid extraction (SFE, ultrasound-assistance, soxhlet extraction, solvent extraction, and three phase partitioning method. Materials and Methods: The SFE conditions (temperature, pressure, and volume of CO2 were optimized prior for better yield. The extracted oils were analyzed and compared for their physiochemical parameters, high performance thin layer chromatography (HPTLC, gas chromatography-mass spectrometry (GC-MS, and Fourier-transformed infrared spectroscopy (FT-IR fingerprinting. Antioxidant activity was also determined using 1,1-diphenyl-2-picrylhydrazyl and superoxide scavenging method. Result: The main fatty acids were α-linolenic acid, linoleic acid, palmitic acid, and stearic acid as obtained by GC-MS. HPTLC analysis revealed the presence of similar major components in chromatograms. Similarly, the pattern of peaks, as obtained in FT-IR and GC-MS spectra of same oils by different extraction methods, were superimposable. Conclusion: Analysis reported that the fixed oil of L. usitatissimum L. is a good source of n-3 fatty acid with the significant antioxidant activity of oil obtained from SFE extraction method.

Instrument for Solvent Extraction and Analysis (ISEE) of Organics from Regolith Simulant Using Supercritical Fluid Extraction and Chromatography

Science.gov (United States)

Franco, Carolina; Hintze, Paul E.

2017-01-01

ISEE is an instrument with the potential to perform extractions from regolith found on the surface of asteroids and planets, followed by characterization and quantitation of the extracts using supercritical fluid extraction (SFE) and chromatography (SFC). SFE is a developed technique proven to extract a wide range of organic compounds. SFC is similar to High Performance Liquid Chromatography (HPLC) but has the advantage of performing chiral separations without needing to derivatize the chiral compounds. CO2 will be the solvent for both stages as it is readily available in the Mars atmosphere. ISEE will capture CO2 from the environment, and use it for SFE and SFC. If successful, this would allow ISEE to perform analysis of organic compounds without using consumables. This paper will present results on a preliminary, proof-of-principle effort to use SFE and SFC to extract and analyze lunar regolith simulant spiked with organic compounds representing a range of organics that ISEE would expect to characterize. An optimization of variables for the extraction of the organics from the spiked regolith was successfully developed, using 138 bar pressure and 40 C temperature. The extraction flow rate was optimized at 2% SLPM with 30% methanol modifier. The extractions were successful with a value of 77.3+/- 0.9% of organics extracted. However, the recovery of organics after the extraction was very low with only 48.5+/-14.2%. Moreover, three columns were selected to analyze multiple samples at a time; two of them are Viridis HSS C18 SB and Torus DIOL, and the third column, specific for chiral separations, has not yet been selected yet.

Application of response surface methodology for the optimization of supercritical fluid extraction of essential oil from pomegranate (Punica granatum L.) peel.

Science.gov (United States)

Ara, Katayoun Mahdavi; Raofie, Farhad

2016-07-01

Essential oils and volatile components of pomegranate ( Punica granatum L.) peel of the Malas variety from Meybod, Iran, were extracted using supercritical fluid extraction (SFE) and hydro-distillation methods. The experimental parameters of SFE that is pressure, temperature, extraction time, and modifier (methanol) volume were optimized using a central composite design after a (2 4-1 ) fractional factorial design. Detailed chemical composition of the essential oils and volatile components obtained by hydro-distillation and optimum condition of the supercritical CO 2 extraction were analyzed by GC-MS, and seventy-three and forty-six compounds were identified according to their retention indices and mass spectra, respectively. The optimum SFE conditions were 350 atm pressure, 55 °C temperature, 30 min extraction time, and 150 µL methanol. Results showed that oleic acid, palmitic acid and (-)-Borneol were major compounds in both extracts. The optimum extraction yield was 1.18 % (w/w) for SFE and 0.21 % (v/w) for hydro-distillation.

Supercritical Fluid Extract of Spent Coffee Grounds Attenuates Melanogenesis through Downregulation of the PKA, PI3K/Akt, and MAPK Signaling Pathways

Directory of Open Access Journals (Sweden)

Huey-Chun Huang

2016-01-01

Full Text Available The mode of action of spent coffee grounds supercritical fluid CO2 extract (SFE in melanogenesis has never been reported. In the study, the spent coffee grounds were extracted by the supercritical fluid CO2 extraction method; the chemical constituents of the SFE were investigated by gas chromatography-mass spectrometry (GC-MS. The effects of the SFE and its major fatty acid components on melanogenesis were evaluated by mushroom tyrosinase activity assay and determination of intracellular tyrosinase activity and melanin content. The expression level of melanogenesis-related proteins was analyzed by western blotting assay. The results revealed that the SFE of spent coffee grounds (1–10 mg/mL and its major fatty acids such as linoleic acid and oleic acid (6.25–50 μM effectively suppressed melanogenesis in the B16F10 murine melanoma cells. Furthermore, the SFE decreased the expression of melanocortin 1 receptor (MC1R, microphthalmia-associated transcription factor (MITF, tyrosinase, tyrosinase-related protein-1 (TRP-1, and tyrosinase-related protein-2 (TRP-2. The SFE also decreased the protein expression levels of p-JNK, p-p38, p-ERK, and p-CREB. Our results revealed that the SFE of spent coffee grounds attenuated melanogenesis in B16F10 cells by downregulation of protein kinase A (PKA, phosphatidylinositol-3-kinase (PI3K/Akt, and mitogen-activated protein kinases (MAPK signaling pathways, which may be due to linoleic acid and oleic acid.

Comparison of supercritical fluid and Soxhlet extractions for the quantification of hydrocarbons from Euphorbia macroclada.

Science.gov (United States)

Ozcan, Adnan; Ozcan, Asiye Safa

2004-10-08

This study compares conventional Soxhlet extraction and analytical scale supercritical fluid extraction (SFE) for their yields in extracting of hydrocarbons from arid-land plant Euphorbia macroclada. The plant material was firstly sequentially extracted with supercritical carbon dioxide, modified with 10% methanol (v/v) in the optimum conditions that is a pressure of 400atm and a temperature of 50 degrees C and then it was sonicated in methylene chloride for an additional 4h. E. macroclada was secondly extracted by using a Soxhlet apparatus at 30 degrees C for 8h in methylene chloride. The validated SFE was then compared to the extraction yield of E. macroclada with a Soxhlet extraction by using the Student's t-test at the 95% confidence level. All of extracts were fractionated with silica-gel in a glass column to get better hydrocarbon yields. Thus, the highest hydrocarbons yield from E. macroclada was achieved with SFE (5.8%) when it compared with Soxhlet extractions (1.1%). Gas chromatography (GC) analysis was performed to determine the quantitative hydrocarbons from plant material. The greatest quantitative hydrocarbon recovery from GC was obtained by supercritical carbon dioxide extract (0.6mgg(-1)).

Comparison of mentha extracts obtained by different extraction methods

Directory of Open Access Journals (Sweden)

Milić Slavica

2006-01-01

Full Text Available The different methods of mentha extraction, such as steam distillation, extraction by methylene chloride (Soxhlet extraction and supercritical fluid extraction (SFE by carbon dioxide (CO J were investigated. SFE by CO, was performed at pressure of 100 bar and temperature of40°C. The extraction yield, as well as qualitative and quantitative composition of obtained extracts, determined by GC-MS method, were compared.

Determination of persistent organic pollutants in solid environmental samples using accelerated solvent extraction and supercritical fluid extraction. Exhaustive extraction and sorption/desorption studies of PCBs

Energy Technology Data Exchange (ETDEWEB)

Bjoerklund, E.

1998-10-01

Human activity is constantly causing environmental problems due to production and release of numerous chemicals. A group of compounds of special concern is persistent organic pollutants (POP). These toxic, lipophilic chemicals have a high chemical and biological stability, and tend to accumulate in the lipid phase of living organisms. A major sink for POPs are sediments, and consequently these are important for the distribution of POPs in the aquatic environment. Traditionally, determination of POPs relay on exhaustive extraction using liquid extraction techniques (e.g. Soxhlet extraction developed in the late 19th century) followed by gas chromatographic analysis. Since liquid-solid extraction normally requires large volumes of organic solvents in combination with long extraction times and extract clean-up, there has been an increasing demand for improved technology. This should result in reduced organic solvent consumption and sample preparation time, at the same time improving the environment and cutting costs for POP monitoring. In this thesis two modern techniques with capability of fulfilling at least one of these goals have been investigated: (1) Supercritical Fluid Extraction (SFE), and (2) Accelerated Solvent Extraction (ASE). Polychlorinated biphenyls (PCBs) were chosen as model compounds in all experiments performed on environmental matrices, since they cover a relatively large range of physiochemical parameters. Important parameters influencing the overall extraction efficiency in ASE and SFE, are discussed and illustrated for a large number of sediments. It was demonstrated that, by careful consideration of the experimental parameters, both techniques are capable of replacing old methods such as Soxhlet extraction. ASE is somewhat faster than SFE, but the extracts generated in SFE are much cleaner and can be analyzed without sample clean-up. Consequently the overall sample preparation time may be substantially lower using SFE. However, ASE is important

Particle Formation by Supercritical Fluid Extraction and Expansion Process

Directory of Open Access Journals (Sweden)

Sujuan Pan

2013-01-01

Full Text Available Supercritical fluid extraction and expansion (SFEE patented technology combines the advantages of both supercritical fluid extraction (SFE and rapid expansion of supercritical solution (RESS with on-line coupling, which makes the nanoparticle formation feasible directly from matrix such as Chinese herbal medicine. Supercritical fluid extraction is a green separation technology, which has been developed for decades and widely applied in traditional Chinese medicines or natural active components. In this paper, a SFEE patented instrument was firstly built up and controlled by LABVIEW work stations. Stearic acid was used to verify the SFEE process at optimized condition; via adjusting the preexpansion pressure and temperature one can get different sizes of particles. Furthermore, stearic acid was purified during the SFEE process with HPLC-ELSD detecting device; purity of stearic acid increased by 19%, and the device can purify stearic acid.

Evaluation of the essential oil of Foeniculum vulgare Mill (fennel) fruits extracted by three different extraction methods by GC/MS.

Science.gov (United States)

Hammouda, Faiza M; Saleh, Mahmoud A; Abdel-Azim, Nahla S; Shams, Khaled A; Ismail, Shams I; Shahat, Abdelaaty A; Saleh, Ibrahim A

2014-01-01

Hydrodistillation (HD) and steam-distillation, or solvent extraction methods of essential oils have some disadvantages like thermal decomposition of extracts, its contamination with solvent or solvent residues and the pollution of residual vegetal material with solvent which can be also an environmental problem. Thus, new green techniques, such as supercritical fluid extraction and microwave assisted techniques, are potential solutions to overcome these disadvantages. The aim of this study was to evaluate the essential oil of Foeniculum vulgare subsp. Piperitum fruits extracted by three different extraction methods viz. Supercritical fluid extraction (SFE) using CO2, microwave-assisted extraction (MAE) and hydro-distillation (HD) using gas chromatography-mass spectrometry (GC/MS). The results revealed that both MAE and SFE enhanced the extraction efficiency of the interested components. MAE gave the highest yield of oil as well as higher percentage of Fenchone (28%), whereas SFE gave the highest percentage of anethol (72%). Microwave-assisted extraction (MAE) and supercritical fluid extraction (SFE) not only enhanced the essential oil extraction but also saved time, reduced the solvents use and produced, ecologically, green technologies.

A field-portable supercritical fluid extractor for characterizing sources of waterborne organic compounds

International Nuclear Information System (INIS)

Fruchter, J.S.; Wright, B.W.

1992-01-01

Supercritical fluid extraction (SFE) is a viable alternative to current methods of liquid extraction for analyzing semivolatile organic compounds in contaminated solid matrices, such as soil and sediment. Because the SFE method is rapid (less than 30 min), large quantities of glassware and large volumes of solvent are not required, and there are fewer sample-handling and sample-preparation steps than in conventional liquid extraction methods, SFE lends itself to in-the-field extraction of solid samples. Laboratory-scale and portable SFE instruments were designed and tested both in the laboratory and in the field. The SFE method was validated through two recovery studies using individual polycyclic aromatic hydrocarbon (PAH) standards ranging from two to six rings in size and through two Soxhlet extraction comparison studies. Supercritical fluid extraction followed by gas chromatography was applied to 20 coal-tar-contaminated soil samples from three locations, 10 petroleum-oil-tar-contaminated soil samples, and 20 polychlorinated-biphenyl-contaminated soil samples. The SFE apparatus was transported and used in the field at four locations across the United States. Carbon dioxide was used as the extraction fluid

Supercritical Fluid Extraction of Bacterial and Archaeal Lipid Biomarkers from Anaerobically Digested Sludge

Directory of Open Access Journals (Sweden)

Koichi Fujie

2012-03-01

Full Text Available Supercritical fluid extraction (SFE was used in the analysis of bacterial respiratory quinone (RQ, bacterial phospholipid fatty acid (PLFA, and archaeal phospholipid ether lipid (PLEL from anaerobically digested sludge. Bacterial RQ were determined using ultra performance liquid chromatography (UPLC. Determination of bacterial PLFA and archaeal PLEL was simultaneously performed using gas chromatography-mass spectrometry (GC-MS. The effects of pressure, temperature, and modifier concentration on the total amounts of RQ, PLFA, and PLEL were investigated by 23 experiments with five settings chosen for each variable. The optimal extraction conditions that were obtained through a multiple-response optimization included a pressure of 23.6 MPa, temperature of 77.6 °C, and 10.6% (v/v of methanol as the modifier. Thirty nine components of microbial lipid biomarkers were identified in the anaerobically digested sludge. Overall, the SFE method proved to be more effective, rapid, and quantitative for simultaneously extracting bacterial and archaeal lipid biomarkers, compared to conventional organic solvent extraction. This work shows the potential application of SFE as a routine method for the comprehensive analysis of microbial community structures in environmental assessments using the lipid biomarkers profile.

Feasibility of ion-pair/supercritical fluid extraction of an ionic compound--pseudoephedrine hydrochloride.

Science.gov (United States)

Eckard, P R; Taylor, L T

1997-02-01

The supercritical fluid extraction (SFE) of an ionic compound, pseudoephedrine hydrochloride, from a spiked-sand surface was successfully demonstrated. The effect of carbon dioxide density (CO2), supercritical fluid composition (pure vs. methanol modified), and the addition of a commonly used reversed-phase liquid chromatographic ion-pairing reagent, 1-heptanesulfonic acid, sodium salt, on extraction efficiency was examined. The extraction recoveries of pseudoephedrine hydrochloride with the addition of the ion-pairing reagent from a spiked-sand surface were shown to be statistically greater than the extraction recoveries without the ion-pairing reagent with both pure and methanol-modified carbon dioxide.

Variability of standard artificial soils: Physico-chemical properties and phenanthrene desorption measured by means of supercritical fluid extraction

International Nuclear Information System (INIS)

Bielská, Lucie; Hovorková, Ivana; Komprdová, Klára; Hofman, Jakub

2012-01-01

The study is focused on artificial soil which is supposed to be a standardized “soil like” medium. We compared physico-chemical properties and extractability of Phenanthrene from 25 artificial soils prepared according to OECD standardized procedures at different laboratories. A substantial range of soil properties was found, also for parameters which should be standardized because they have an important influence on the bioavailability of pollutants (e.g. total organic carbon ranged from 1.4 to 6.1%). The extractability of Phe was measured by supercritical fluid extraction (SFE) at harsh and mild conditions. Highly variable Phe extractability from different soils (3–89%) was observed. The extractability was strongly related (R 2 = 0.87) to total organic carbon content, 0.1–2 mm particle size, and humic/fulvic acid ratio in the following multiple regression model: SFE (%) = 1.35 * sand (%) − 0.77 * TOC (%)2 + 0.27 * HA/FA. - Highlights: ► We compared properties and extractability of Phe from 25 different artificial soils. ► Substantial range of soil properties was found, also for important parameters. ► Phe extractability was measured by supercritical fluid extraction (SFE) at 2 modes. ► Phe extractability was highly variable from different soils (3–89%). ► Extractability was strongly related to TOC, 0.1–2 mm particles, and HA/FA. - Significant variability in physico-chemical properties exists between artificial soils prepared at different laboratories and affects behavior of contaminants in these soils.

Effect of solvent type and ratio on betacyanins and antioxidant activity of extracts from Hylocereus polyrhizus flesh and peel by supercritical fluid extraction and solvent extraction.

Science.gov (United States)

Fathordoobady, Farahnaz; Mirhosseini, Hamed; Selamat, Jinap; Manap, Mohd Yazid Abd

2016-07-01

The main objective of the present study was to investigate the effect of solvent type and ratio as well as the extraction techniques (i.e. supercritical fluid extraction (SFE) and conventional solvent extraction) on betacyanins and antioxidant activity of the peel and fresh extract from the red pitaya (Hylocereus polyrhizus). The peel and flesh extracts obtained by SFE at 25MPa pressure and 10% EtOH/water (v/v) mixture as a co-solvent contained 24.58 and 91.27mg/100ml total betacyanin, respectively; while the most desirable solvent extraction process resulted in a relatively higher total betacyanin in the peel and flesh extracts (28.44 and 120.28mg/100ml, respectively). The major betacyanins identified in the pitaya peel and flesh extracts were betanin, isobetanin, phyllocactin, butyrylbetanin, isophyllocactin and iso-butyrylbetanin. The flesh extract had the stronger antioxidant activity than the peel extract when the higher proportion of ethanol to water (E/W) was applied for the extraction. Copyright © 2016 Elsevier Ltd. All rights reserved.

[Optimization of SFE-CO2 Extraction for Ursolic Acid from Punica granatum Peel by Plackett-Burman and Central Composite Design].

Science.gov (United States)

Wang, Zhan-yi; Jin, Mei-hua; Wang, Yu-hai; Zhang, Li-hua; Bi, Hai-dan; Li, Zhuo-wa

2015-03-01

The optimum extraction of ursolic acid from Punica granatum peel by SFE-CO2 was investigated. Based on the design of Plackett-Burman(PB), significant factors influencing the yield of ursolic acid in the operation process were filtered, with the extraction rate of ursolic acid as the index. The results obtained by steepest ascent method approximated the maximum area of ursolic acid yield. Then the Central Composite Design(CCD) design was used to carry on the response surface optimization of significant factors, getting a two order mathematical model affecting the ursolic acid yield, as well as the optimum process conditions. The best technological conditions of the extraction of ursolic acid from Punica granatum peel by SFE-CO2 were that the extraction temperature was 46. 29 °C, extraction time was 91. 6 min and the extraction pressure was 34. 49 MPa. Under the optimal conditions, verification test of ursolic acid yield was 12. 508 mg/g, approximating to the predicted value of 12. 645 mg/g. The PB test and CCD test design are combined to optimize the extraction process of ursolic acid from Punica granatum peel by SFE-CO2. The screening results are statistically significant and the process operation is feasible.

Investigation of parameters affecting the online combination of supercritical fluid extraction with capillary gas chromatography

NARCIS (Netherlands)

Lou, X.W.; Janssen, J.G.M.; Cramers, C.A.M.G.

1996-01-01

Two different injectors, a split/splitless injector and a programmed temperature vaporizer (PTV) injector were investigated as the interface in on-line supercritical fluid extraction (SFE)-capillary gas chromatography (cGC). The parameters affecting the chromatographic peak shapes as well as the

Supercritical fluid extraction-capillary gas chromatography: on-line coupling with a programmed temperature vaporizer

NARCIS (Netherlands)

Houben, R.J.; Janssen, J.G.M.; Leclercq, P.A.; Rijks, J.A.; Cramers, C.A.M.G.

1990-01-01

A simple and versatile system is described for the on-line coupling of SFE to capillary GC. The interfacing consists of a programmed temperature vaporizer (PTV) injector. With this injector it is possible to combine solute trapping, elimination of a high flow of extraction fluid, and quantitative

A comparative study of conventional and supercritical fluid extraction methods for the recovery of secondary metabolites from Syzygium campanulatum Korth#

Science.gov (United States)

Memon, Abdul Hakeem; Hamil, Mohammad Shahrul Ridzuan; Laghari, Madeeha; Rithwan, Fahim; Zhari, Salman; Saeed, Mohammed Ali Ahmed; Ismail, Zhari; Majid, Amin Malik Shah Abdul

2016-01-01

Syzygium campanulatum Korth is a plant, which is a rich source of secondary metabolites (especially flavanones, chalcone, and triterpenoids). In our present study, three conventional solvent extraction (CSE) techniques and supercritical fluid extraction (SFE) techniques were performed to achieve a maximum recovery of two flavanones, chalcone, and two triterpenoids from S. campanulatum leaves. Furthermore, a Box-Behnken design was constructed for the SFE technique using pressure, temperature, and particle size as independent variables, and yields of crude extract, individual and total secondary metabolites as the dependent variables. In the CSE procedure, twenty extracts were produced using ten different solvents and three techniques (maceration, soxhletion, and reflux). An enriched extract of five secondary metabolites was collected using n-hexane:methanol (1:1) soxhletion. Using food-grade ethanol as a modifier, the SFE methods produced a higher recovery (25.5%‒84.9%) of selected secondary metabolites as compared to the CSE techniques (0.92%‒66.00%). PMID:27604860

A comparative study of conventional and supercritical fluid extraction methods for the recovery of secondary metabolites from Syzygium campanulatum Korth.

Science.gov (United States)

Memon, Abdul Hakeem; Hamil, Mohammad Shahrul Ridzuan; Laghari, Madeeha; Rithwan, Fahim; Zhari, Salman; Saeed, Mohammed Ali Ahmed; Ismail, Zhari; Majid, Amin Malik Shah Abdul

2016-09-01

Syzygium campanulatum Korth is a plant, which is a rich source of secondary metabolites (especially flavanones, chalcone, and triterpenoids). In our present study, three conventional solvent extraction (CSE) techniques and supercritical fluid extraction (SFE) techniques were performed to achieve a maximum recovery of two flavanones, chalcone, and two triterpenoids from S. campanulatum leaves. Furthermore, a Box-Behnken design was constructed for the SFE technique using pressure, temperature, and particle size as independent variables, and yields of crude extract, individual and total secondary metabolites as the dependent variables. In the CSE procedure, twenty extracts were produced using ten different solvents and three techniques (maceration, soxhletion, and reflux). An enriched extract of five secondary metabolites was collected using n-hexane:methanol (1:1) soxhletion. Using food-grade ethanol as a modifier, the SFE methods produced a higher recovery (25.5%‒84.9%) of selected secondary metabolites as compared to the CSE techniques (0.92%‒66.00%).

Magnetite nanoparticles coated with covalently immobilized ionic liquids as a sorbent for extraction of non-steroidal anti-inflammatory drugs from biological fluids

International Nuclear Information System (INIS)

Amiri, Maryam; Yadollah, Yamini; Safari, Meysam; Asiabi, Hamid

2016-01-01

Magnetic core-shell nanoparticles (mag-NPs) of type SiO_2-Fe_3O_4 were covalently modified with the ionic liquid dimethyl octadecyl[3-(trimethoxysilyl propyl)]ammonium chloride. The NPs were characterized via FTIR and scanning electron microscopy and evaluated with respect to the extraction of the nonsteroidal anti-inflammatory drugs (NSAIDs) tolmetin, indometacin and naproxen from blood samples. Supercritical fluid extraction was used to eliminate matrix effects before extraction with the mag-NPs. The effects of pH value of sample solution, amount of adsorbent, times of adsorption and desorption, salt effect, type and volume of suitable solvent for desorption were optimized. Under optimum conditions, magnetic solid phase extraction (MSPE) resulted in limits of detection that range between 0.1 and 0.3 μg L"−"1. In case of supercritical fluid extraction along with magnetic solid phase extraction (SFE- MSPE), the LODs ranged from 0.2 to 0.3 mg kg"−"1. The analytical ranges for all of the NSAIDs varied within 0.2–15 mg kg"-"1 and 0.1–250 μg L"−"1 in the SFE-MSPE and MSPE methods, respectively. The relative standard deviations for the extraction of the NSAIDs from blood samples via SFE-MSPE are <10.2%. (author)

Supercritical Fluid Extraction of Eucalyptus globulus Bark—A Promising Approach for Triterpenoid Production

Science.gov (United States)

Domingues, Rui M. A.; Oliveira, Eduardo L. G.; Freire, Carmen S. R.; Couto, Ricardo M.; Simões, Pedro C.; Neto, Carlos P.; Silvestre, Armando J. D.; Silva, Carlos M.

2012-01-01

Eucalyptus bark contains significant amounts of triterpenoids with demonstrated bioactivity, namely triterpenic acids and their acetyl derivatives (ursolic, betulinic, oleanolic, betulonic, 3-acetylursolic, and 3-acetyloleanolic acids). In this work, the supercritical fluid extraction (SFE) of Eucalyptus globulus deciduous bark was carried out with pure and modified carbon dioxide to recover this fraction, and the results were compared with those obtained by Soxhlet extraction with dichloromethane. The effects of pressure (100–200 bar), co-solvent (ethanol) content (0, 5 and 8% wt), and multistep operation were studied in order to evaluate the applicability of SFE for their selective and efficient production. The individual extraction curves of the main families of compounds were measured, and the extracts analyzed by GC-MS. Results pointed out the influence of pressure and the important role played by the co-solvent. Ethanol can be used with advantage, since its effect is more important than increasing pressure by several tens of bar. At 160 bar and 40 °C, the introduction of 8% (wt) of ethanol greatly improves the yield of triterpenoids more than threefold. PMID:22837719

Supercritical fluid extraction of grape seeds: extract chemical composition, antioxidant activity and inhibition of nitrite production in LPS-stimulated Raw 264.7 cells.

Science.gov (United States)

Pérez, Concepción; Ruiz del Castillo, María Luisa; Gil, Carmen; Blanch, Gracia Patricia; Flores, Gema

2015-08-01

Grape by-products are a rich source of bioactive compounds having broad medicinal properties, but are usually wasted from juice/wine processing industries. The present study investigates the use of supercritical fluid extraction (SFE) for obtaining an extract rich in bioactive compounds. First, some variables involved in the extraction were applied. SFE conditions were selected based on the oil mass yield, fatty acid profile and total phenolic composition. As a result, 40 °C and 300 bar were selected as operational conditions. The phenolic composition of the grape seed oil was determined using LC-DAD. The antioxidant activity was determined by ABTS and DPPH assays. For the anti-inflammatory activity the inhibition of nitrite production was assessed. The grape seed oil extracted was rich in phenolic compounds and fatty acids with significant antioxidant and anti-inflammatory activities. From these results, added economic value to this agroindustrial residue is proposed using environmentally friendly techniques.

Feasibility studies on supercritical fluid extraction of uranium from phosphoric acid

International Nuclear Information System (INIS)

Dubey, B.P.; Agarwal, A.K.

2014-01-01

Supercritical fluid extraction (SFE) is a promising novel technology for extraction of many materials. Work has been carried out worldwide on SFE of uranium from various matrices. However, there are no references indicating the R and D on uranium extraction from phosphoric acid using this technology. Heavy Water Board is involved in technology development for recovery of uranium from secondary source, hence it was considered prudent to investigate the technology of SFE for this purpose. Various experiments were carried out with both WPA (P 2 O 5 content 28%) and MGPA (P 2 O 5 content 54%) using bench scale facility available with one of the private party. Extraction experiments were carried out using several chelating agents including TBP, D2EHPA, D2EHPA+TBP/TOPO, TTA, TTA+TBP etc. Feasibility studies revealed the hydrodynamics of operation indicating liquid expansion by about three times during flow of super critical (SC) CO 2 . No flooding was observed when the extraction column filled 20% of its volume capacity, no carryover of entrained/extracted liquid with SC CO 2 with MGPA, material balance of inputs and outputs established i.e. 100% recovery of MGPA and chelating agent, No operational problems with raw MGPA (untreated). No significant extraction of impurities from phosphoric acid to SC CO 2 , 40℃ temperature and 160 bar pressure found ideal for extraction experiments since no other materials found extracted at these conditions and no apparent change/deterioration in PA and chelating agents. Experiments established feasibility of SCE with CO 2 , proper recovery of PA and chelating agents, no need for pretreatment/gunk removal from PA; however, extraction of uranium was found inadequate even though ORP of feed acid was boosted by H 2 O 2 addition. Investigations revealed that SCE column created reducing environment in phosphoric acid, which was not favourable for uranium extraction, which resulted in difficulty in extraction of Uranium. HWB has now designed

Supercritical Fluid Extraction of Quinones from Compost for Microbial Community Analysis

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Ni Luh Gede Ratna Juliasih

2015-01-01

Full Text Available Supercritical fluid extraction (SFE was used to extract quinones from compost to monitor the microbial community dynamics during composting. The 0.3 g of dried compost was extracted using 3 mL min−1 of carbon dioxide (90% and methanol (10% at 45°C and 25 MPa for a 30 min extraction time. The extracted quinones were analysed using ultra performance liquid chromatography (UPLC with 0.3 mL min−1 of methanol mobile phase for a 50 min chromatographic run time. A comparable detected amount of quinones was obtained using the developed method and an organic solvent extraction method, being 36.06 μmol kg−1 and 34.54 μmol kg−1, respectively. Significantly low value of dissimilarity index (D between the two methods (0.05 indicated that the quinone profile obtained by both methods was considered identical. The developed method was then applied to determine the maturity of the compost by monitoring the change of quinone during composting. The UQ-9 and MK-7 were predominant quinones in the initial stage of composting. The diversity of quinone became more complex during the cooling and maturation stages. This study showed that SFE had successfully extracted quinones from a complex matrix with simplification and rapidity of the analysis that is beneficial for routine analysis.

Preparative isolation and purification of capsaicin and dihydrocapsaicin from Capsici Fructus using supercritical fluid extraction combined with high speed countercurrent chromatography.

Science.gov (United States)

Yan, Rongwei; Zhao, Leilei; Tao, Junfei; Zou, Yong; Xu, Xinjun

2018-05-01

Supercritical fluid extraction with CO 2 (SFE-CO 2 ) was utilized for extraction of capsaicin (CA) and dihydrocapsaicin (DHCA) from Capsici Fructus, and then a two-step enrichment method for separating capsaicinoids from SFE-CO 2 extracts was developed. The process involved extraction with aqueous methanol and crystallization by alkali extraction and acid precipitation. Finally, a consecutive high-speed countercurrent chromatography (HSCCC) separation method was successfully applied in the purification of CA and DHCA from capsaicinoid crystal. The extraction pressure, extraction temperature and volume of co-solvent were optimized at 33 MPa, 41 °C and 75 mL, respectively, using response surface methodology; the extraction rates of CA and DHCA were about 93.18% and 93.49%, respectively. 407.43 mg capsaicinoid crystal was isolated from the SFE-CO 2 extracts obtained from 100 g capsicum powder by the two-step enrichment method. About 506 mg and 184 mg CA and DHCA with purities up to 98.31% and 96.68%, respectively, were obtained from 1 g capsaicinoid crystal in one HSCCC of three consecutive sample loadings without exchanging any solvent system. This method comprising SFE-CO 2 , a two-step enrichment and HSCCC was efficient, powerful and practical for the large-scale preparation of CA and DHCA from Capsici Fructus with high purity and high yield. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Obtaining of the antioxidants by supercritical fluid extraction

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Babović Nada V.

2011-01-01

Full Text Available One of the important trends in the food industry today is demand for natural antioxidants from plant material. Synthetic antioxidants such as butylated hydroxytoluene (BHT, and butylated hydroxyanisole (BHA are now being replaced by the natural antioxidants because of theirs possible toxicity and as they may act as promoters of carcinogens. The natural antioxidants may show equivalent or higher antioxidant activity than the endogenous or the synthetic antioxidants. Thus, great effort is being devoted to the search for alternative and cheap sources of natural antioxidants, as well as to the development of efficient and selective extraction techniques. The supercritical fluid extraction (SFE with carbon dioxide is considered to be the most suitable method for producing natural antioxidants for the use in food industry. The supercritical extract does not contain residual organic solvents as in conventional extraction processes, which makes these products suitable for use in food, cosmetic and pharmaceutical industry. The recovery of antioxidants from plant sources involves many problematic aspects: choice of an adequate source (in terms of availability, cost, difference in phenolic content with variety and season; selection of the optimal recovery procedure (in terms of yield, simplicity, industrial application, cost; chemical analysis of extracts (for optimization purposes a fast colorimetric method is more preferable than a chromatographic one; evaluation of the antioxidant power (preferably by the different assay methods. The paper presents information about different operational methods for SFE of bioactive compounds from natural sources. It also includes the various reports on the antioxidant activity of the supercritical extracts from Lamiaceae herbs, in comparison with the activity of the synthetic antioxidants and the extracts from Lamiaceae herbs obtained by the conventional methods.

Cytotoxic Activity of Kenaf Seed Oils from Supercritical Carbon Dioxide Fluid Extraction towards Human Colorectal Cancer (HT29) Cell Lines.

Science.gov (United States)

Abd Ghafar, Siti Aisyah; Ismail, Maznah; Saiful Yazan, Latifah; Fakurazi, Sharida; Ismail, Norsharina; Chan, Kim Wei; Md Tahir, Paridah

2013-01-01

Kenaf (Hibiscus cannabinus) from the family Malvaceae, is a valuable fiber plant native to India and Africa and is currently planted as the fourth commercial crop in Malaysia. Kenaf seed oil contains alpha-linolenic acid, phytosterol such as β -sitosterol, vitamin E, and other antioxidants with chemopreventive properties. Kenaf seeds oil (KSO) was from supercritical carbon dioxide extraction fluid (SFE) at 9 different permutations of parameters based on range of pressures from 200 to 600 bars and temperature from 40 to 80°C. They were 200/40, 200/60, 200/80, 400/40, 400/60, 400/80, 600/40, 600/60, and 600/80. Extraction from 9 parameters of KSO-SFE was screened for cytotoxicity towards human colorectal cancer cell lines (HT29) and mouse embryonic fibroblast (NIH/3T3) cell lines using MTS assay. KSO-SFE at 600/40 showed the strongest cytotoxicity towards HT29 with IC50 of 200 µg/mL. The IC50 for NIH/3T3 was not detected even at highest concentration employed. Cell cycle analysis showed a significant increase in the accumulation of KSO-SFE-treated cells at sub-G1 phase, indicating the induction of apoptosis by KSO-SFE. Further apoptosis induction was confirmed by Annexin V/PI and AO/PI staining.

NOVAS APLICAÇÕES DE SISTEMAS SFE "HOME MADE".: I. PLANTAS MEDICINAIS BRASILEIRAS

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Fernando M. LANÇAS

1997-12-01

Full Text Available Neste trabalho, apresenta-se uma visão geral da evolução do uso da SFE (extração com fluido supercrítico na análise de plantas medicinais brasileiras dentro das pesquisas desenvolvidas pelo Laboratório de Cromatografia do IQSC-USP. Utilizou-se como fluido extrator o CO2, puro ou modificado com solventes de polaridade baixa a alta (pentano, solventes halogenados, álcoois, água, para a extração seletiva de princípios ativos de Maytenus aquifolium ("espinheira santa" e Mikania glomerata ("guaco", respectivamente contendo triterpenos e cumarina. Os extratos obtidos por SFE foram analisados por CGAR (cromatografia gasosa de alta resolução, CLAE-DAD (cromatografia líquida de alta eficiência com detector" photodiodearray" ou CCD (cromatografia de camada delgada. A SFE forneceu resultados similares ou melhores do que os obtidos com métodos convencionais de extração (Soxhlet, maceração, etc, indicando o potencial uso da SFE para análise e/ou produção de preparações contendo estas plantas medicinais.Further applications of "home made" SFE systems. I. Brazilian medicinal plants. In this paper, an overview on the evolution of the utilization of SFE for the analysis of Brazilian medicinal plants in the research developed by the Laboratório de Cromatografia, IQSC-USP, is presented. CO2, pure or with modifiers from low to high polarity (pentane, halogenated solvents, alcohols, water were used for the selective extraction of active compounds. Maytenus aquifolium (known popularly in Brazil as" espinheira santa", and Mikania glomerata ("guaco", containing respectively triterpenes and coumarin, were studied. The extracts obtained by SFE showed similar or better results than of those extracts obtained by conventional extraction methods (Soxhlet, maceration, etc., which indicates the potential of SFE technique in the analysis and/or production of phytomedicines.

Removal of plutonium from real time waste using supercritical fluid extraction

International Nuclear Information System (INIS)

Sujatha, K.; Sivaraman, N.; Kumar, R.; Srinivasan, T.G.; Vasudeva Rao, P.R.

2010-01-01

Supercritical fluid extraction (SFE) technique was carried out for the recovery of plutonium from cellulose waste matrix using supercritical carbon dioxide (SC-CO 2 ) modified with suitable ligands such as octylphenyl N,N-diisobutyl carbamoylmethyl phosphine oxide (φCMPO), tri-n-butyl phosphate (TBP), acetyl acetone, trifluoro acetyl acetone and theonyltrifluoroacetyl acetone (TTA). The maximum plutonium recovery was found to be 99.8% when SC-CO 2 modified with CMPO was employed. About 15mg of plutonium was recovered from waste. (author)

Application of supercritical fluid extraction (SFE) to predict bioremediation efficacy of long-term composting of PAH-contaminated soil

Czech Academy of Sciences Publication Activity Database

Cajthaml, Tomáš; Šašek, Václav

2005-01-01

Roč. 39, č. 21 (2005), s. 8448-8452 ISSN 0013-936X R&D Projects: GA ČR GP206/03/P078 Institutional research plan: CEZ:AV0Z50200510 Keywords : SFE * long-term composting * PAH Subject RIV: EE - Microbiology, Virology Impact factor: 4.054, year: 2005

Effect of soil contaminant extraction method in determining toxicity using the Microtox(reg.) assay

International Nuclear Information System (INIS)

Harkey, G.A.; Young, T.M.

2000-01-01

This project examined the influence of different extraction methods on the measured toxicity of contaminated soils collected from manufactured gas plant (MGP) sites differing in soil composition and contaminant concentration. Aged soils from a number of MGP sites were extracted using a saline solution, supercritical fluid extraction (SFE), and Soxhlet extraction. Toxicity was assessed using two forms of Microtox tests: acute aqueous tests on saline and SFE soil extracts and solid-phase tests (SPTs) on soil particles. Microtox SPTs were performed on soils before and after SFE to determine resulting toxicity reduction. Three hypotheses were tested: (1) Toxicity of soil extracts is related to contaminant concentrations of the extracts, (2) measured toxicity significantly decreases with less vigorous methods of extraction, and (3) supercritical fluid extractability correlates with measured toxicity. The EC50s for SPTs performed before and after SFE were not different for some soils but were significantly greater after extraction for other soils tested. The most significant toxicity reductions were observed for soils exhibiting the highest toxicity in both preextraction SPTs and acute aqueous tests. Acute Microtox tests performed on SFE extracts showed significantly lower EC50s than those reported from saline-based extraction procedures. Toxicity of the soils measured by Microtox SPTs was strongly correlated with both SFE efficiency and measures of contaminant aging. Data from this project provide evidence of sequestration and reduced availability of polycyclic aromatic hydrocarbons (PAHs) from soils extracted via physiologically based procedures compared to vigorous physical extraction protocols

HPLC/MS identification of the polyphenols present in an extract of Myrtus communis L. obtained by supercritical fluid extraction

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Paula Pereira

2017-12-01

Full Text Available In this work, we studied an extract obtained by supercritical fluid extraction (SFE using a simpler method of cosolvent (ethanol addition. Instead of using a liquid pump, which is the most common process, the ethanol was directly introduced in the extraction cell, immediately after loading the cell with the plant sample. it was our intent to investigate if this change would have any effect in the composition of the extract obtained. The experimental conditions used were: temperature 48° C, pressure 10 MPa, supercritical fluid (SCF flow rate 130.71dm3h-1 (0.238 kgh-1 and an ethanol volume of 104 cm3. The composition of the extract obtained was different from previous tests, and the compounds identified by HPLC-MS were quinic acid, quinic acid 3,5-di-O-gallate, quinic acid 3,4,5-galloyl, myricetin-galactoside gallate, quercetin-galactoside gallate, quercetin, and myricetin-galactosiderhamnoside.

Extraction, fatty acid profile and antioxidant activity of sesame extract (Sesamum Indicum L.

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R. H. R. Carvalho

2012-06-01

Full Text Available This article carried out the extraction of sesame oil by using three extraction techniques: supercritical fluid extraction (SFE, Soxhlet and sequential extraction. The SFE was performed using supercritical carbon dioxide (SC-CO2 as solvent and ethanol as cosolvent. Tests were performed at 20 MPa, 35ºC and a flow rate of 2.5 g CO2/min with a total extraction time of 210 minutes. The Soxhlet extraction was performed for 8 hours, using petroleum ether and ethanol as solvents, until the exhaustion of the oil contained in the seeds. The sequential extraction used ethyl ether, ethanol and water as solvents. The Soxhlet extraction was the most effective (58.93%, while the SFE technique obtained 26.47% as the best result. The antioxidant activity (AA was determined by the β-carotene/linoleic acid system, with good oxidation inhibition percentages (29.32-83.49% for all the extracts. The main fatty acids (FA in sesame oil were oleic and linoleic acids.

Cytotoxic Activity of Kenaf Seed Oils from Supercritical Carbon Dioxide Fluid Extraction towards Human Colorectal Cancer (HT29 Cell Lines

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Siti Aisyah Abd Ghafar

2013-01-01

Full Text Available Kenaf (Hibiscus cannabinus from the family Malvaceae, is a valuable fiber plant native to India and Africa and is currently planted as the fourth commercial crop in Malaysia. Kenaf seed oil contains alpha-linolenic acid, phytosterol such as β-sitosterol, vitamin E, and other antioxidants with chemopreventive properties. Kenaf seeds oil (KSO was from supercritical carbon dioxide extraction fluid (SFE at 9 different permutations of parameters based on range of pressures from 200 to 600 bars and temperature from 40 to 80°C. They were 200/40, 200/60, 200/80, 400/40, 400/60, 400/80, 600/40, 600/60, and 600/80. Extraction from 9 parameters of KSO-SFE was screened for cytotoxicity towards human colorectal cancer cell lines (HT29 and mouse embryonic fibroblast (NIH/3T3 cell lines using MTS assay. KSO-SFE at 600/40 showed the strongest cytotoxicity towards HT29 with IC50 of 200 µg/mL. The IC50 for NIH/3T3 was not detected even at highest concentration employed. Cell cycle analysis showed a significant increase in the accumulation of KSO-SFE-treated cells at sub-G1 phase, indicating the induction of apoptosis by KSO-SFE. Further apoptosis induction was confirmed by Annexin V/PI and AO/PI staining.

Studies on supercritical fluid extraction of uranium and thorium from liquid and solid matrix

International Nuclear Information System (INIS)

Kumar, Pradeep; Pal, Ankita; Saxena, M.K.; Ramakumar, K.L.

2006-05-01

Supercritical fluid extraction (SFE) is being widely used in pharmaceutical and food industry. Because of its simplicity, ease of operation and more importantly the reduction in the analytical waste generation, this technique is being viewed as a potential application technique in nuclear industry also. CO 2 is employed as supercritical fluid (SCF) as it is easily recyclable, non-toxic, chemically inert, radiochemically stable and inexpensive. Radioanalytical chemistry section (Radiochemistry and Isotope group) has recently procured a supercritical fluid extraction/chromatography system. The present report describes the work carried out on the system. Detailed study on uranium and thorium extraction from highly acidic medium and tissue paper matrix has been carried out. Direct dissolution and extraction of uranium compounds employing SCF has been carried out. CO 2 was employed as supercritical fluid along with very small amount of Tri n-butyl phosphate (TBP) and Tri n-octyl phosphine oxide (TOPO) as co-solvents. The effect of various operating parameters like CO 2 flow rate, co-solvent percentage, temperature and pressure on extraction was investigated and parameters for maximum extraction were optimized. For comparison, the modes of extraction viz. static and dynamic and modes of complexation viz. in-situ and online were studied. Uranium extraction of ∼98% has been achieved from nitric acid medium employing TBP as co-solvent in 30 minutes extraction time, whereas with TOPO ∼99% uranium extraction could be achieved. Uranium from tissue paper matrix could be extracted upto the extent of 98% with TOPO as co-solvent whereas with TBP extraction of (66.83± 9.80)% was achievable. Direct dissolution of UO 2 , U 3 O 8 , U metal, U-Al alloy solids into SCF CO 2 was carried out employing TBP-HNO 3 complex and SFE of uranium was performed using TBP as co-solvent. UO 2 and U 3 O 8 solids could be dissolved within 20 minutes and extraction of ∼98% was achieved. For U

Application of supercritical fluid extraction in analytical science

International Nuclear Information System (INIS)

Kumar, Pradeep

2015-01-01

In the recent years, supercritical fluid extraction (SFE) has emerged as a promising alternative to conventional solvent extraction process owing to its potential to minimize the generation of the liquid volume and simplification of the extraction process.This technology is some times referred to as 'green technology' and 'clean technology'. Supercritical fluid extraction process assumes significance as it exhibits practical advantages such as enhanced extraction rate due to rapid mass transfer in supercritical fluid medium and change of solvent properties such as density by tuning pressure/temperature conditions. Supercritical fluids (SCF) offer faster, cleaner and efficient extraction owing to low viscosity, high density, low surface tension and better diffusivity properties. Higher diffusivity than liquids facilitates rapid mass transfer and faster completion of reaction. Due to low viscosity and surface tension, SCF can penetrate deep inside the material, extracting the component of interest. Liquid like solvating characteristics of SCFs enable dissolution of compounds whereas gas like diffusion characteristics provide conditions for high degree of extraction in shorter time duration. CO 2 has been widely employed as supercritical fluid owing to its moderate critical constants (Pc= 72.9 atm, Tc =304.3 K, ñ c = 0.47 g mL -1 ) and attractive properties such as being easily available, recyclable, non-toxic, chemically inert, non inflammable and radio-chemically stable. SCF finds application in variety of fields. In nuclear industry for separation and purification of actinides from liquids and solid matrices. In food industry, Decaffeination of coffee is done by SCF. Pharmaceutical industry, organic compounds can be extracted from plants by SC CO 2 avoiding liquid solvent usage. SCF may also be utilised for the production of fine powders. In polymer and plastics industries, examples of applications include the impregnation of medical material

Fatty acid composition and antioxidant activity of oils from two cultivars of Cantaloupe extracted by supercritical fluid extraction

Energy Technology Data Exchange (ETDEWEB)

Ismail, M.; Mariod, A.; Bagalkotkar, G.; Ling, H. S

2010-07-01

The effect of supercritical fluid extraction (SFE) fractionation of three oil fractions (1st, 2nd, 3rd fraction) on the fatty acid composition and antioxidant activity of oils from two cultivars of cantaloupe were investigated. Rock melon oil (RMO) and Golden Langkawi oil (GLO) were extracted using SFE and the major fatty acids for both cultivars were linoleic, oleic, palmitic, and stearic acid. The SFA decreased from 15.78 to 14.14% in RMO 1st fraction, and MUFA decreased from 18.30 to 16.56% in RMO 2nd fraction, while PUFA increased from 65.9 to 69.30% in RMO 3rd fraction. On the other hand SFA decreased from 16.35 to 13.91% in GLO 1{sup s}t fraction, and MUFA decreased from 17.50 to 15.57% in GLO 2nd fraction, while PUFA increased from 66.15 to 70.52% in GLO 3rd fraction. The different fractions of the two oils showed high antioxidant activity in reducing the oxidation of {beta}-carotene in beta-carotene bleaching assay (BCB) and the quenching of 1,1-diphenyl-2-picrylhydrazyl (DPPH). (Author) 41 refs.

Online recovery of radiocesium from soil, cellulose and plant samples by supercritical fluid extraction employing crown ethers and calix-crown derivatives as extractants

International Nuclear Information System (INIS)

Kanekar, A.S.; Pathak, P.N.; Mohapatra, P.K.

2014-01-01

Two crown ethers (CEs) viz. dibenzo18crown6, and dibenzo12crown7 and three calix-crown derivatives viz. (octyloxy)calix[4]arene-mono-crown-6 (CMC), calix[4]arene-bis(o-benzocrown-6) (CBC), and calix[4]arene-bis(naphthocrown-6) (CNC) were evaluated for the recovery of 137 Cs from synthetic soil, cellulose (tissue paper), and plant samples by supercritical fluid extraction (SFE) route. CEs showed poor extraction of 137 Cs from soil matrix. SFE experiments using 1 × 10 -3 M solutions of CMC, CBC and CNC in acetonitrile at 3 M HNO 3 as modifiers displayed better extraction of 137 Cs, viz. 21(±2) % (CMC), 16.5(±3) % (CBC), and 4(±1) % (CNC). It was not possible to recover 137 Cs quantitatively from soil matrix. The inefficient extraction of 137 Cs from soil matrix was attributed to its incorporation into the interstitial sites. Experiments on tissue papers using CMC showed near quantitative 137 Cs recovery. On the other hand, recovery from plant samples varied between 50(±5) % (for stems) and 75(±5) % (for leaves). (author)

Supercritical fluid extraction and chromatographic analysis (HRGC-FID and HRGC-MS of Lupinus spp. alkaloids

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Nossack Ana C.

2000-01-01

Full Text Available The alkaloid extracts from Lupinus spp., obtained by conventional methods (maceration/sonication - solid phase extraction; maceration/sonication - liquid-liquid extraction and SFE (supercritical fluid extraction using CO2 and modified CO2 (CO2/MeOH, CO2/EtOH, CO2/iPrOH and CO2/H2O were analysed by HRGC-FID (high resolution gas chromatography - flame ionization detector and HRGC-MS (high resolution gas chromatography - mass spectrometry. The HRGC-FID quantitative analyses were performed with an internal standard method for quantification of lupanine, multiflorine and a spartein-like alkaloid. HRGC-MS allowed identification of the chemical constituents (alkaloids and other compounds from these extracts.

Extraction of semivolatile organic compounds from high-efficiency particulate air (HEPA) filters by supercritical carbon dioxide

International Nuclear Information System (INIS)

Schilling, J.B.

1997-09-01

Supercritical fluid extraction (SFE) using unmodified carbon dioxide has been explored as an alternative method for the extraction of semivolatile organic compounds from high-efficiency particulate air (HEPA) filters. HEPA filters provide the final stage of containment on many exhaust systems in US Department of Energy (DOE) facilities by preventing the escape of chemical and radioactive materials entrained in the exhausted air. The efficiency of the filters is tested by the manufacturer and DOE using dioctylphthalate (DOP), a substance regulated by the US Environmental Protection Agency under the Resource Conservation and Recovery Act. Therefore, the filters must be analyzed for semivolatile organics before disposal. Ninety-eight acid, base, and neutral semivolatile organics were spiked onto blank HEPA material and extracted using SFE, Soxhlet, automated Soxhlet, and sonication techniques. The SFE conditions were optimized using a Dionex SFE-703 instrument. Average recoveries for the 98 semivolatile compounds are 82.7% for Soxhlet, 74.0% for sonication, 70.2% for SFE, and 62.9% for Soxtec. Supercritical fluid extraction reduces the extraction solvent volume to 10--15 mL, a factor of 20--30 less than Soxhlet and more than 5 times less than Soxtec and sonication. Extraction times of 30--45 min are used compared to 16--18 h for Soxhlet extraction

Estudo dos métodos de extração de carotenóides em cenoura por fluido supercrítico (efs e convencional A study of the methods of carotenoid extraction in carrots using supercritical fluid extraction (sfe and conventional methods

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Ellem Waleska Nascimento da Fonseca Contado

2010-12-01

Full Text Available A cenoura (Daucus carota L. , planta da família das umbelíferas, produz uma raiz aromática e comestível, sendo uma das hortaliças mais cultivadas no Brasil. Representa a principal fonte de origem vegetal em carotenóides pró-vitamínicos A, especialmente o á e o β-caroteno, sendo, também, uma grande fonte de fibra dietética, antioxidantes e minerais. Conduziu-se este trabalho, com o objetivo de avaliar dois processos de extração de β-caroteno, fluído super crítico (EFS e o convencional e analisar a composição centesimal da cenoura in natura. O teor de β-caroteno obtido pela extração por EFS e por convencional foi de 2.457 e 2.455 µg/100g, respectivamente. Os valores médios encontrados para a matéria-seca da cenoura foram de: matéria-seca = 8,9%; extrato etéreo = 0,29%; cinzas = 8,11%; fibra bruta = 14,57%, proteína bruta = 6,4%, extrato não nitrogenado = 6,3% e valor calórico = 27,7kcal. Conclui-se que a extração de carotenóides em cenoura pelo fluido supercritico é uma técnica de separação viável, pois este fluido é inerte, não deixa resíduo final e não gera resíduo ambiental. Pelos teores encontrados conclui-se também que as cenouras são boas fontes de fibras, apresentam alto teor de umidade e baixo teor de gorduras, cinzas e valor calórico.The carrot (Daucus carota L. is a plant of the Umbelliferae family. It produces an aromatic and edible root, and is one of the most widely cultivated vegetable in Brazil. It represents the main source of plant-origin, pro-vitamin A carotenoids, especially α and β-carotene, and is also a great source of dietary fiber, antioxidants and minerals. This study aimed to evaluate two methods of extraction of β-carotene, supercritical fluid (SFE and conventional, and to examine the proximate composition of the carrot in nature. The contents of β-carotene obtained by SFE and by conventional extraction were 2,457 and 2,455 µg/100g, respectively. The average values found

Dicty_cDB: SFE109 [Dicty_cDB

Lifescience Database Archive (English)

Full Text Available SF (Link to library) SFE109 (Link to dictyBase) - - - Contig-U10771-1 SFE109P (Link... to Original site) SFE109F 197 SFE109Z 630 SFE109P 827 - - Show SFE109 Library SF (Link to library) Clone ID SFE109 (Link to dict...yBase) Atlas ID - NBRP ID - dictyBase ID - Link to Contig Contig-U10771-1 Original site URL http://dict...anslated Amino Acid sequence elnykfhftlnttqiei*inknfllflf*fffyfqi*iqlcfilkllllptiink*INKI FLKKK--- ---VTTSQCESLIQAGVDGLRVGMGVGSICT...fkfnsvsy*nyyyyqpslink*ik ff*kk--- ---VTTSQCESLIQAGVDGLRVGMGVGSICTTQEVMACGRPQATAVFKCALYSSQYNVPI IADGGIRTIGHII

Determination of lycopene in food by on-line SFE coupled to HPLC using a single monolithic column for trapping and separation

Czech Academy of Sciences Publication Activity Database

Pól, Jaroslav; Hyötyläinen, T.; Ranta-Aho, O.; Riekkola, M. L.

2004-01-01

Roč. 1052, 1-2 (2004), s. 25-31 ISSN 0021-9673 R&D Projects: GA AV ČR KJB4031405 Grant - others:Academy of Finland Projects(FI) 48867; Academy of Finland Projects(FI) 52746 Institutional research plan: CEZ:AV0Z4031919 Keywords : lycopene * on-line SFE-LC * supercritical fluid extraction Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.359, year: 2004

Antioxidant Properties of Essential Oil Extracted from Pinus morrisonicola Hay Needles by Supercritical Fluid and Identification of Possible Active Compounds by GC/MS.

Science.gov (United States)

Cheng, Ming-Ching; Chang, Wen-Hua; Chen, Chih-Wei; Li, Wen-Wing; Tseng, Chin-Yin; Song, Tuzz-Ying

2015-10-20

Pine (Pinus morrisonicola Hay, PM) needles have been used as folk medicine for their antihypertension and lipid-lowering effects. As supercritical fluid extraction (SFE) is considered an ideal technique for the extraction of essential oil from plant materials, the present work investigated the optimal SFE conditions and the protective effects of different resulting fractions of PM needles on lipid peroxidation and foam cell production in macrophages. Nine PM needle extracts (PME1-9) were obtained in 1%-4% yields using different SFE conditions, of which PME1 had the lowest yield (1.1%) and PME3 the highest (3.9%). PME3 exhibited lower cytotoxic effects and stronger inhibition of lipid peroxidation and formation of foam cell in RAW 264.7 macrophages than those of other PME extracts. PME3-1 purified from PME3 by column and thin layer chromatography inhibited LDL oxidation more effectively than did PME3 in a cell-free system oxidized by Cu(2+). PME3-1 dose-dependently (25-100 μg/mL) decreased conjugated diene levels and foam cell formation induced by ox-LDL. GC/MS analyses revealed that 1-docosene, neophytadiene, and methyl abietate were increased 5.2-, 1.7- and 4.3-fold in PME3-1 relative to PME3. A new hydrocarbon compound, cedrane-8,13-diol, was identified in PME3-1. Overall, the present study demonstrates the optimal extraction conditions of SFE of PM and identifies the most potent antioxidant fractions and possible active compounds in PM.

Antioxidant Properties of Essential Oil Extracted from Pinus morrisonicola Hay Needles by Supercritical Fluid and Identification of Possible Active Compounds by GC/MS

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Ming-Ching Cheng

2015-10-01

Full Text Available Pine (Pinus morrisonicola Hay, PM needles have been used as folk medicine for their antihypertension and lipid-lowering effects. As supercritical fluid extraction (SFE is considered an ideal technique for the extraction of essential oil from plant materials, the present work investigated the optimal SFE conditions and the protective effects of different resulting fractions of PM needles on lipid peroxidation and foam cell production in macrophages. Nine PM needle extracts (PME1–9 were obtained in 1%–4% yields using different SFE conditions, of which PME1 had the lowest yield (1.1% and PME3 the highest (3.9%. PME3 exhibited lower cytotoxic effects and stronger inhibition of lipid peroxidation and formation of foam cell in RAW 264.7 macrophages than those of other PME extracts. PME3-1 purified from PME3 by column and thin layer chromatography inhibited LDL oxidation more effectively than did PME3 in a cell-free system oxidized by Cu2+. PME3-1 dose-dependently (25–100 μg/mL decreased conjugated diene levels and foam cell formation induced by ox-LDL. GC/MS analyses revealed that 1-docosene, neophytadiene, and methyl abietate were increased 5.2-, 1.7- and 4.3-fold in PME3-1 relative to PME3. A new hydrocarbon compound, cedrane-8,13-diol, was identified in PME3-1. Overall, the present study demonstrates the optimal extraction conditions of SFE of PM and identifies the most potent antioxidant fractions and possible active compounds in PM.

Comparison of different methods for extraction from Tetraclinis articulata: yield, chemical composition and antioxidant activity.

Science.gov (United States)

Herzi, Nejia; Bouajila, Jalloul; Camy, Séverine; Romdhane, Mehrez; Condoret, Jean-Stéphane

2013-12-15

In the present study, three techniques of extraction: hydrodistillation (HD), solvent extraction (conventional 'Soxhlet' technique) and an innovative technique, i.e., the supercritical fluid extraction (SFE), were applied to ground Tetraclinis articulata leaves and compared for extraction duration, extraction yield, and chemical composition of the extracts as well as their antioxidant activities. The extracts were analyzed by GC-FID and GC-MS. The antioxidant activity was measured using two methods: ABTS(•+) and DPPH(•). The yield obtained using HD, SFE, hexane and ethanol Soxhlet extractions were found to be 0.6, 1.6, 40.4 and 21.2-27.4 g/kg respectively. An original result of this study is that the best antioxidant activity was obtained with an SFE extract (41 mg/L). The SFE method offers some noteworthy advantages over traditional alternatives, such as shorter extraction times, low environmental impact, and a clean, non-thermally-degraded final product. Also, a good correlation between the phenolic contents and the antioxidant activity was observed with extracts obtained by SFE at 9 MPa. Copyright © 2013 Elsevier Ltd. All rights reserved.

Supercritical fluid extraction of triterpenes and aliphatic hydrocarbons from olive tree derivatives

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Aimen Issaoui

2017-05-01

Full Text Available Olive leaves and tree bark were extracted through supercritical fluid extraction (SFE and the chemical composition of the extracted mixture was determined by Gas Chromatography–Mass Spectrometry (GC–MS. Both samples contain a great number of triterpenes as squalene, which were used since 1997 as a main constituent of the flu vaccine (FLUAD, and the alpha-tocopherol the most biologically active form of vitamin E. We also underline the presence of many aliphatic compounds such nonacosane and heptacosane in low concentrations. The extractions were carried out at 313 and 333 K, at a pressure varying from 90 to 250 bars and using pure carbon dioxide in its supercritical phase. Therefore, their solubilities at equilibrium were numerically optimized via two assumptions and compared with the experimental values. Indeed, a good agreement between several results was shown.

Supercritical Fluid Extraction of Eucalyptus globulus Bark—A Promising Approach for Triterpenoid Production

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Carlos M. Silva

2012-06-01

Full Text Available Eucalyptus bark contains significant amounts of triterpenoids with demonstrated bioactivity, namely triterpenic acids and their acetyl derivatives (ursolic, betulinic, oleanolic, betulonic, 3-acetylursolic, and 3-acetyloleanolic acids. In this work, the supercritical fluid extraction (SFE of Eucalyptus globulus deciduous bark was carried out with pure and modified carbon dioxide to recover this fraction, and the results were compared with those obtained by Soxhlet extraction with dichloromethane. The effects of pressure (100–200 bar, co-solvent (ethanol content (0, 5 and 8% wt, and multistep operation were studied in order to evaluate the applicability of SFE for their selective and efficient production. The individual extraction curves of the main families of compounds were measured, and the extracts analyzed by GC-MS. Results pointed out the influence of pressure and the important role played by the co-solvent. Ethanol can be used with advantage, since its effect is more important than increasing pressure by several tens of bar. At 160 bar and 40 °C, the introduction of 8% (wt of ethanol greatly improves the yield of triterpenoids more than threefold.

Comparison of the Apoptotic Effects of Supercritical Fluid Extracts of Antrodia cinnamomea Mycelia on Hepatocellular Carcinoma Cells

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Hsiu-Man Lien

2014-06-01

Full Text Available Antrodia cinnamomea (AC has been widely used as a folk medicine in the prevention and treatment of liver diseases, such as hepatitis, hepatic fibrosis, and hepatocellular carcinoma. Previous studies have indicated that triterpenoids and benzenoids show selective cytotoxicity against human hepatoma cell lines. The aim of the study was to compare the triterpenoid content of extract and the extract-induced cytotoxicity in HepG2 cells from mycelia extracts of solid state cultured AC obtained by supercritical fluid extraction (SFE and the conventional solvent extraction method. SFE with CO2 mixed with a constant amount of ethanol co-solvent (10% of CO2 volume applied at different temperatures and pressures (40, 60 and 80 °C and, 20.7, 27.6 and 34.5 Mpa was also compared in the study. Although the extraction yield of triterpenoids (59.7 mg/g under the optimal extraction conditions of 34.5 MPa (5000 psi/60 °C (designated as sample S-5000-60 was equivalent to the extraction yield using conventional liquid solvent extraction with ethanol (ETOH-E at room temperature (60.33 mg/g, the cytotoxicity of the former against the proliferation of HepG2 cell line measured as the inhibition of 50% of cell growth activity (IC50 at dosages of 116.15, 57.82 and 43.96 µg/mL was superior to that of EtOH-E at 131.09, 80.04 and 48.30 µg/mL at 24, 48 and 72 h, respectively. Additionally, we further proved that the apoptotic effect of S-5000-60 presented a higher apoptosis ratio (21.5% than ETOH-E (10.5% according to annexin V-FITC and propidium iodide double staining assay results. The high affinity and selectivity of SFE on bioactive components resulted in a higher extraction efficiency than conventional solvent extraction. The chemical profile of the obtained extracts from solid state cultivated mycelium of AC was also determined by high-performance liquid chromatography electrospray ionization tandem mass spectrometry (LC-MS/MS, whereby three benzenoids and four

Phytosterols and their extraction from various plant matrices using supercritical carbon dioxide: a review.

Science.gov (United States)

Uddin, Md Salim; Sarker, Md Zaidul Islam; Ferdosh, Sahena; Akanda, Md Jahurul Haque; Easmin, Mst Sabina; Bt Shamsudin, Siti Hadijah; Bin Yunus, Kamaruzzaman

2015-05-01

Phytosterols provide important health benefits: in particular, the lowering of cholesterol. From environmental and commercial points of view, the most appropriate technique has been searched for extracting phytosterols from plant matrices. As a green technology, supercritical fluid extraction (SFE) using carbon dioxide (CO2) is widely used to extract bioactive compounds from different plant matrices. Several studies have been performed to extract phytosterols using supercritical CO2 (SC-CO2) and this technology has clearly offered potential advantages over conventional extraction methods. However, the efficiency of SFE technology fully relies on the processing parameters, chemistry of interest compounds, nature of the plant matrices and expertise of handling. This review covers SFE technology with particular reference to phytosterol extraction using SC-CO2. Moreover, the chemistry of phytosterols, properties of supercritical fluids (SFs) and the applied experimental designs have been discussed for better understanding of phytosterol solubility in SC-CO2. © 2014 Society of Chemical Industry.

Supercritical fluid extraction of lanthanides and actinides from solid materials with a fluorinated β-diketone

International Nuclear Information System (INIS)

Lin, Y.; Brauer, R.D.; Laintz, K.E.; Wai, C.M.

1993-01-01

Direct extraction of metal ions by supercritical carbon dioxide is highly inefficient because of the charge neutralization requirement and the weak solute-solvent interactions. One suggested approach of extracting metal ions by supercritical carbon dioxide is to convert the charged species into metal chelates using a chelating agent in the fluid phase. This paper describes a method of extracting lanthanide and uranyl ions from a solid material by supercritical carbon dioxide containing a fluorinated beta-diketone, 2,2-dimethyl-6,6,7,7,8,8,8-heptafluoro-3,5-octanedione(FOD). Potential applications of this SFE method for separating the f-block elements from environmental samples are discussed. 13 refs., 2 tabs

Impacts of Extraction Methods in the Rapid Determination of Atrazine Residues in Foods using Supercritical Fluid Chromatography and Enzyme-Linked Immunosorbent Assay: Microwave Solvent vs. Supercritical Fluid Extractions

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Mohamed H. El-Saeid

2005-01-01

Full Text Available It is an accepted fact that many food products that we eat today have the possibility of being contaminated by various chemicals used from planting to processing. These chemicals have been shown to cause illnesses for which some concerned government agencies have instituted regulatory mechanisms to minimize the risks and the effects on humans. It is for these concerns that reliable and accurate rapid determination techniques are needed to effect proper regulatory standards for the protection of people's nutritional health. This paper, therefore, reports the comparative evaluation of the extraction methods in the determination of atrazine (commonly used in agricultural as a herbicide residues in foods using supercritical fluid chromatography (SFC and enzyme-linked immunosorbent assay (ELISA techniques. Supercritical fluid extraction (SFE and microwave solvent extraction (MSE methods were used to test samples of frozen vegetables, fruit juice, and jam from local food markets in Houston. Results showed a high recovery percentage of atrazine residues using supercritical fluid coupled with ELISA and SFC than with MSE. Comparatively, however, atrazine was detected 90.9 and 54.5% using SFC and ELISA techniques, respectively. ELISA technique was, however, less time consuming, lower in cost, and more sensitive with low detection limit of atrazine residues than SFC technique.

Supercritical Fluid Extraction and Ultra Performance Liquid Chromatography of Respiratory Quinones for Microbial Community Analysis in Environmental and Biological Samples

OpenAIRE

Hanif, Muhammad; Atsuta, Yoichi; Fujie, Koichi; Daimon, Hiroyuki

2012-01-01

Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE) and ultra performance liquid chromatography (UPLC) method for the analysis of bacterial respiratory quinones (RQ) in environmental and biological samples. RQ profile analysi...

Extraction of Lepidium apetalum Seed Oil Using Supercritical Carbon Dioxide and Anti-Oxidant Activity of the Extracted Oil

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Xuchong Tang

2011-12-01

Full Text Available The supercritical fluid extraction (SFE of Lepidium apetalum seed oil and its anti-oxidant activity were studied. The SFE process was optimized using response surface methodology (RSM with a central composite design (CCD. Independent variables, namely operating pressure, temperature, time and flow rate were evaluated. The maximum extraction of Lepidium apetalum seed oil by SFE-CO2 (about 36.3% was obtained when SFE-CO2 extraction was carried out under the optimal conditions of 30.0 MPa of pressure, 70 °C of temperature, 120 min of extraction time and 25.95 L/h of flow rate. GC-MS analysis showed the presence of four fatty acids in Lepidium apetalum seed oil, with a high content (91.0% of unsaturated fatty acid. The anti-oxidant activity of the oil was assessed by the 2,2-diphenyl-1-picrylhydrazyl (DPPH radical-scavenging assay and 2,2′-azino- bis(3-ethylbenzthiazoline-6-sulphonic acid diammonium salt (ABTS test. Lepidium apetalum seed oil possessed a notable concentration-dependent antioxidant activity, with IC50 values of 1.00 and 3.75 mg/mL, respectively.

Phytochemical profile and anticholinesterase and antimicrobial activities of supercritical versus conventional extracts of Satureja montana.

Science.gov (United States)

Silva, Filipa V M; Martins, Alice; Salta, Joana; Neng, Nuno R; Nogueira, José M F; Mira, Delfina; Gaspar, Natália; Justino, Jorge; Grosso, Clara; Urieta, José S; Palavra, António M S; Rauter, Amélia P

2009-12-23

Winter savory Satureja montana is a medicinal herb used in traditional gastronomy for seasoning meats and salads. This study reports a comparison between conventional (hydrodistillation, HD, and Soxhlet extraction, SE) and alternative (supercritical fluid extraction, SFE) extraction methods to assess the best option to obtain bioactive compounds. Two different types of extracts were tested, the volatile (SFE-90 bar, second separator vs HD) and the nonvolatile fractions (SFE-250 bar, first and second separator vs SE). The inhibitory activity over acetyl- and butyrylcholinesterase by S. montana extracts was assessed as a potential indicator for the control of Alzheimer's disease. The supercritical nonvolatile fractions, which showed the highest content of (+)-catechin, chlorogenic, vanillic, and protocatechuic acids, also inhibited selectively and significantly butyrylcholinesterase, whereas the nonvolatile conventional extract did not affect this enzyme. Microbial susceptibility tests revealed the great potential of S. montana volatile supercritical fluid extract for the growth control and inactivation of Bacillus subtilis and Bacillus cereus, showing some activity against Botrytis spp. and Pyricularia oryzae. Although some studies were carried out on S. montana, the phytochemical analysis together with the biological properties, namely, the anticholinesterase and antimicrobial activities of the plant nonvolatile and volatile supercritical fluid extracts, are described herein for the first time.

Bioassay-guided supercritical fluid extraction of cyclooxygenase-2 inhibiting substances in Plantago major L.

Science.gov (United States)

Stenholm, A; Göransson, U; Bohlin, L

2013-02-01

Selective extraction of plant materials is advantageous for obtaining extracts enriched with desired constituents, thereby reducing the need for subsequent chromatography purification. Such compounds include three cyclooxygenase-2 (COX-2) inhibitory substances in Plantago major L. targeted in this investigation: α-linolenic acid (α-LNA) (18:3 ω-3) and the triterpenic acids ursolic acid and oleanolic acid. To investigate the scope for tuning the selectivity of supercritical fluid extraction (SFE) using bioassay guidance, and Soxhlet extraction with dichloromethane as solvent as a reference technique, to optimise yields of these substances. Extraction parameters were varied to optimise extracts' COX-2/COX-1 inhibitory effect ratios. The crude extracts were purified initially using a solid phase extraction (SPE) clean-up procedure and the target compounds were identified with GC-MS, LC-ESI-MS and LC-ESI-MS² using GC-FID for quantification. α-LNA was preferentially extracted in dynamic mode using unmodified carbon dioxide at 40°C and 172 bar, at a 0.04% (w/w) yield with a COX-2/COX-1 inhibitory effect ratio of 1.5. Ursolic and oleanolic acids were dynamically extracted at 0.25% and 0.06% yields, respectively, with no traces of (α-LNA) and a COX-2/COX-1-inhibitory effect ratio of 1.1 using 10% (v/v) ethanol as polar modifier at 75°C and 483 bar. The Soxhlet extracts had ursolic acid, oleanolic acid and αLNA yields up to 1.36%, 0.34% and 0.15%, respectively, with a COX-2/COX-1 inhibitory effect ratio of 1.2. The target substances can be extracted selectively by bioassay guided optimisation of SFE conditions. Copyright © 2012 John Wiley & Sons, Ltd.

Extraction of Stevia rebaudiana bertoni sweetener glycosides by supercritical fluid methods.

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Juan José Hinojosa-González

2017-05-01

Full Text Available Aim. The aim was to evaluate the supercritical carbon dioxide extraction method with and without the addition of co-solvent to the system (mixture water: ethanol to obtain the glycosides from leaves of Stevia rebaudiana Bertoni. Methods. A SFT-150 SFE / SFR model with CO2 as a fluid was used for the supercritical extraction. The variables studied were temperature, pressure, extraction time and the presence or absence of the co-solvent (water-ethanol mixture in a concentration of 70:30 v/v, incorporated in different proportions to determine the effect on yield. The amount of glycoside sweeteners was analyzed by High Performance Liquid Chromatography (HPLC. Results. The pressure was the factor that favored the extraction, which was selective in obtaining Rebaudioside A with yields no greater than 2%. The inclusion of the co-solvent achieved an increase in yield to values of 2.9% Conclusion. Supercritical CO2 individually and mixed with ethanol-water as a co-solvent was not efficient to extract Stevia rebaudiana stevioside sweeteners

Optimisation of supercritical fluid extraction of polycyclic aromatic hydrocarbons and their nitrated derivatives adsorbed on highly sorptive diesel particulate matter

International Nuclear Information System (INIS)

Portet-Koltalo, F.; Oukebdane, K.; Dionnet, F.; Desbene, P.L.

2009-01-01

Supercritical fluid extraction (SFE) was performed to extract complex mixtures of polycyclic aromatic hydrocarbons (PAHs), nitrated derivatives (nitroPAHs) and heavy n-alkanes from spiked soot particulates that resulted from the incomplete combustion of diesel oils. This polluted material, resulting from combustion in a light diesel engine and collected at high temperature inside the particulate filter placed just after the engine, was particularly resistant to conventional extraction techniques, such as soxhlet extraction, and had an extraction behaviour that differed markedly from certified reference materials (SRM 1650). A factorial experimental design was performed, simultaneously modelling the influence of four SFE experimental factors on the recovery yields, i.e.: the temperature and the pressure of the supercritical fluid, the nature and the percentage of the organic modifier added to CO 2 (chloroform, tetrahydrofuran, methylene chloride), as a means to reach the optimal extraction yields for all the studied target pollutants. The results of modelling showed that the supercritical fluid pressure had to be kept at its maximum level (30 MPa) and the temperature had to be kept relatively low (75 o C). Under these operating conditions, adding 15% of methylene chloride to the CO 2 permitted quantitative extraction of not only light PAHs and their nitrated derivatives, but also heavy n-alkanes from the spiked soots. However, heavy polyaromatics were not quantitatively extracted from the refractory carbonaceous solid surface. As such, original organic modifiers were tested, including pyridine, which, as a strong electron donor cosolvent (15% into CO 2 ), was the most successful. The addition of diethylamine to pyridine, which enhanced the electron donor character of the cosolvent, even increased the extraction yields of the heaviest PAHs, leading to a quantitative extraction of all PAHs (more than 79%) from the diesel particulate matter, with detection limits

A new method based on supercritical fluid extraction for polyacetylenes and polyenes from Echinacea pallida (Nutt.) Nutt. roots.

Science.gov (United States)

Tacchini, Massimo; Spagnoletti, Antonella; Brighenti, Virginia; Prencipe, Francesco Pio; Benvenuti, Stefania; Sacchetti, Gianni; Pellati, Federica

2017-11-30

The genus Echinacea (Asteraceae) includes species traditionally used in phytotherapy. Among them, Echinacea pallida (Nutt.) Nutt. root extracts are characterized by a representative antiproliferative activity, due to the presence of acetylenic compounds. In this study, supercritical fluid extraction (SFE) was applied and compared with conventional Soxhlet extraction (SE) in order to obtain a bioactive extract highly rich in polyacetylenes and polyenes from E. pallida roots. The composition of the extracts was monitored by means of HPLC-UV/DAD and HPLC-ESI-MS n by using an Ascentis Express C 18 column (150mm×3.0mm I.D., 2.7μm, Supelco, Bellefonte, PA, USA) with a mobile phase composed of (A) water and (B) acetonitrile, under gradient elution. By keeping SFE time at the threshold of 1h (15min static and 45min dynamic for 1 cycle) with the oven temperature set at 40-45°C and 90bar of pressure, an overall extraction yield of 1.18-1.21% (w/w) was obtained, with a high selectivity for not oxidized lipophilic compounds. The biological activity of the extracts was evaluated against human non-small lung A549 and breast carcinoma MCF-7 cancer cell lines. The cytotoxic effect of the SFE extract was more pronounced towards the MCF-7 than the A549 cancer cells, with IC 50 values ranging from 21.01±2.89 to 31.11±2.l4μg/mL; cell viability was affected mainly between 24 and 48h of exposure. The results show the possibility of a new "green" approach to obtain extracts highly rich in genuine polyacetylenes and polyenes from E. pallida roots. The bioactivity evaluation confirmed the cytotoxicity of E. pallida extracts against the considered cancer cell lines, especially against MCF-7 cells, thus suggesting to represent a valuable tool for applicative purposes in cancer prevention. Copyright © 2017 Elsevier B.V. All rights reserved.

NOVAS APLICAÇÕES DE SISTEMAS SFE" HOME MADE".: II. PLANTAS DA AMÉRICA DO SUL

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Fernando M. LANÇAS

1997-12-01

Full Text Available O Laboratório de Cromatografia do IQSC-USP tem desenvolvido pesquisas em conjunto com outros grupos de pesquisa do Brasil e da América Latina, visando a futura implantação da SFE (extração com fluido supercrítico nestes laboratórios. No presente trabalho, apresenta-se alguns dos resultados obtidos na cooperação com pesquisadores do Chile e da Venezuela, direcionados para a SFE de substâncias de potencial interesse econômico, princípios ativos ou substâncias tóxicas: triglicerídeos, ácidos graxos, flavonóides, alcalóides, etc. Foram estudadas plantas nativas do Chile e da Venezuela, algumas delas nunca estudadas por métodos fitoquímicos convencionais e pertencentes a várias famílias vegetais: Leguminosae, Chrysobalanaceae, Annonnaceae, etc. O uso da SFE em conjunto com CGAR-EM (cromatografia gasosa de alta resolução - espectrometria de massas ou CLAE-DAD (cromatografia líquida de alta eficiência com detector" photodiodearray" permitiu a identificação de algumas substâncias presentes em baixa concentração, a partir de pequenas quantidades de material vegetal; estes dados são de grande importância para a caracterização química das espécies estudadas.Further applications of "home made" SFE systems. II. South American plants. The Laboratório de Cromatografia, IQSC-USP, has been developing joint research projects with other research groups from Brazil and Latin America, aiming a future implementation of SFE (supercritical fluid extraction in these laboratories. In the present work, some of the results obtained in the cooperation with researchers from Chile and Venezuela, focused to SFE of potential economical interest compounds, active compounds or toxic molecules, are presented: triglycerides, fatty acids, flavonoids, alkaloids, etc. Native plants from Chile and Venezuela, belonging to several families (Leguminosae, Chrysobalanaceae, Annonnaceae, etc. were studied, some of them never studied by conventional

NOVAS APLICAÇÕES DE SISTEMAS SFE "HOME MADE": III. ENERGIA QUÍMICA E ELÉTRICA

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Fernando M. LANÇAS

1997-12-01

Full Text Available Este trabalho apresenta três aplicações da SFE com diferentes fluídos supercríticos, matrizes e sistemas de extração. Um sistema estático "home made" foi utilizado na pesquisa de fontes alternativas de insumos químicos e energéticos tais como o bagaço de cana-de-açucar e o carvão mineral. Foram usados, respectivamente, o etanol (sem e com catalisador e o tolueno como fluídos extratores e hidrogênio como gás de pressurização. Na extração dos contaminantes do óleo mineral adsorvidos em bauxita, foi utilizado o dióxido de carbono como fluído extrator em um sistema "home made"/dinâmico. Estudos visando a maximização do rendimento de alguns dos processos também foram realizados, utilizando o planejamento fatorial e a metodologia da superfície de resposta. Os produtos de maior interesse neste trabalho (fração de resinas, obtidos do processo de extração do bagaço de cana-de-açucar e aqueles contaminantes do óleo isolante adsorvidos em bauxita extraídos com fluídos supercríticos foram caracterizados usando cromatografia gasosa de alta resolução com detector de ionização de chama (CGAR - DIC e cromatografia gasosa de alta resolução com detector seletivo de massas (CGAR - EM após fracionamento por cromatografia líquida preparativa em 8 frações distintas.This work presents three aplications of SFE with different supercritical fluids, samples and extraction systems. A home made static system was utilized in the search for alternative chemicals and energetics resources such as sugar cane bagasse and mineral coal. Ethanol (with and without catalyst and toluene were used, respectively ,as extraction fluids and hydrogen as pressurization gas. The adsorbed contaminants of mineral oil in bauxite were also extracted with carbon dioxide as extractor fluid in a home made dinamical system. Maximization of yields in some processes was studied using factorial design and response surface methodologies. The products

Cytotoxic Activity of Kenaf Seed Oils from Supercritical Carbon Dioxide Fluid Extraction towards Human Colorectal Cancer (HT29) Cell Lines

OpenAIRE

Abd Ghafar, Siti Aisyah; Ismail, Maznah; Saiful Yazan, Latifah; Fakurazi, Sharida; Ismail, Norsharina; Chan, Kim Wei; Md Tahir, Paridah

2013-01-01

Kenaf (Hibiscus cannabinus) from the family Malvaceae, is a valuable fiber plant native to India and Africa and is currently planted as the fourth commercial crop in Malaysia. Kenaf seed oil contains alpha-linolenic acid, phytosterol such as ? -sitosterol, vitamin E, and other antioxidants with chemopreventive properties. Kenaf seeds oil (KSO) was from supercritical carbon dioxide extraction fluid (SFE) at 9 different permutations of parameters based on range of pressures from 200 to 600 bars...

A fully continuous supercritical fluid extraction system for contaminated soil

International Nuclear Information System (INIS)

Ryan, M.; Stiver, W.H.

2007-01-01

Brownfield sites are contaminated sites in an urban setting. There are hundreds of thousands of such sites, where contaminants migrate to the atmosphere, seep into groundwater, runoff into surface water and enter the food chain through plant uptake and soil ingestion. The Sydney Tar Ponds alone contain more than a million tonnes of contaminated soils and sediments. Soil vapour extraction, incineration, bioremediation, solvent extraction and land filling are among the remediation techniques that have been developed for brownfield sites over the years. However, no single technology is ideally suited to all cases because of the diversity of contaminants and diversity of site characterization. This paper focused on supercritical fluid extraction (SFE) which is well suited to sites contaminated with polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and heavy metal. A fully continuous laboratory-scale SFE process for a slurry-based system was designed and constructed to handle the supercritical carbon dioxide (SC-CO 2 ) and the soil slurry. The system continuously pumps carbon dioxide under supercritical conditions and soil slurry into a counter-current contacting column. The testing soil was Delhi loamy sand, spiked with 10 mg/g of naphthalene. The soil slurry ranged from 0.0028 g dry soil per g slurry to 0.072 g/g. The operating temperature was 43 degrees C and the operating pressure was 7.7 MPa. Near steady state, fully continuous flow was achieved with runs lasting up to 2 hours. The quantifiable recoveries of naphthalene from the soil slurry was demonstrated and the mass transfer coefficients for the system were quantified in order to provide the foundation to advance to a full-scale system and costing analysis. 14 refs., 1 tab., 3 figs

A fully continuous supercritical fluid extraction system for contaminated soil

Energy Technology Data Exchange (ETDEWEB)

Ryan, M.; Stiver, W.H. [Guelph Univ., ON (Canada). School of Engineering

2007-04-15

Brownfield sites are contaminated sites in an urban setting. There are hundreds of thousands of such sites, where contaminants migrate to the atmosphere, seep into groundwater, runoff into surface water and enter the food chain through plant uptake and soil ingestion. The Sydney Tar Ponds alone contain more than a million tonnes of contaminated soils and sediments. Soil vapour extraction, incineration, bioremediation, solvent extraction and land filling are among the remediation techniques that have been developed for brownfield sites over the years. However, no single technology is ideally suited to all cases because of the diversity of contaminants and diversity of site characterization. This paper focused on supercritical fluid extraction (SFE) which is well suited to sites contaminated with polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and heavy metal. A fully continuous laboratory-scale SFE process for a slurry-based system was designed and constructed to handle the supercritical carbon dioxide (SC-CO{sub 2}) and the soil slurry. The system continuously pumps carbon dioxide under supercritical conditions and soil slurry into a counter-current contacting column. The testing soil was Delhi loamy sand, spiked with 10 mg/g of naphthalene. The soil slurry ranged from 0.0028 g dry soil per g slurry to 0.072 g/g. The operating temperature was 43 degrees C and the operating pressure was 7.7 MPa. Near steady state, fully continuous flow was achieved with runs lasting up to 2 hours. The quantifiable recoveries of naphthalene from the soil slurry was demonstrated and the mass transfer coefficients for the system were quantified in order to provide the foundation to advance to a full-scale system and costing analysis. 14 refs., 1 tab., 3 figs.

Technical design issues for a field-portable supercritical fluid extractor

Energy Technology Data Exchange (ETDEWEB)

Wright, B.W.; Zemanian, T.S.; Robins, W.H.; Wright, C.W.

1995-01-01

Supercritical fluid extraction is gaining acceptance as an alternative sample preparation method for trace organic analysis. The development of SFE instrumentation optimized for field use requires taking several technical design issues including size and weight requirements, user-friendly operation, and technical performance capabilities into consideration. Parameters associated with a prototype SFE instrument under development for potential use in conducting on-site inspections of the Chemical Weapons Convention and its preliminary technical and operational performance are described.

Quantitative aspects of directly coupled supercritical fluid extraction-capillary gas chromatography with a conventional split/splitless injector as interface

OpenAIRE

Lou, X.W.; Janssen, J.G.M.; Cramers, C.A.

1993-01-01

The quant. aspects of online supercrit. fluid extn.-capillary gas chromatog. (SFE-GC) with a split/splitless injector as interface were studied. Special attention was paid to the discrimination behavior and the reproducibility of the split/splitless interface. A simple exptl. set-up is proposed that allows accurate quantitation in online SFE-split GC. The results obtained in online SFE-GC compare favorably with those from conventional GC with split injection. Discrimination is absent when wor...

Comparison of supercritical fluid extraction and Soxhlet extraction for the determination of PCBs in seaweed samples.

Science.gov (United States)

Punín Crespo, M O; Lage Yusty, M A

2005-06-01

The efficiency of supercritical fluid extraction for the determination of 12 polychlorinated biphenyls from algae samples is compared to Soxhlet extraction. Analytical detection limits for the individual congeners ranged from 0.62 microgl(-1) to 19 microgl(-1). Recovery was tested for both methods using standard addition procedure. At maximum spike level of concentration, the mean recoveries were not significantly different (P>0.05) of all PCBs studied, with the exception of PCBs 28, 52, 77 and 169. Method precision for Soxhlet extraction (yield comparable results, SFE offers the advantage of detecting all PCBs studied at lower concentrations, reducing extraction time, and reducing the amount of solvents needed. The optimized methods were applied to the analysis of three real seaweed samples, except for PCB101 the concentrations of all PCBs were low or below the detection limits. The levels of PCB101 found in sample 1 were 6.6+/-0.54 ng g(-1) d.w., in sample 2 the levels were 8.2+/-0.86 ng g(-1) d.w. and in sample 3 they were 7.7+/-0.08 ng g(-1) d.w.

Characterisation of organic compounds in aerosol particles from a finnish forest by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Shimmo, Masahiko; Jaentti, Jaana; Hartonen, Kari; Hyoetylaeinen, Tuulia; Riekkola, Marja-Liisa [Laboratory of Analytical Chemistry, Department of Chemistry, University of Helsinki, P.O. Box 55, 00014, Helsinki (Finland); Aalto, Pasi; Kulmala, Markku [Division of Atmospheric Sciences, Department of Physical Sciences, University of Helsinki, P.O. Box 64, 00014, Helsinki (Finland)

2004-04-01

During the European Union project Quantification of Aerosol Nucleation in the European Boundary Layer (QUEST), which began in spring 2003, atmospheric aerosol particles were collected in a Finnish Scots pine forest using a high-volume sampler. The organic compounds in the filter samples were then analysed by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry (SFE-LC-GC-MS). The sample was first extracted by SFE. During LC the extracts were fractionated into three fractions according to polarity. The final separation was carried out by GC-MS. A fraction volume as high as 840 {mu}L was transferred to the GC, using the partial concurrent eluent evaporation technique. The same instrumentation, with an in-situ SFE derivatisation method, was used to analyse organic acids. Major compounds such as n-alkanes and PAH were analysed quantitatively. Their concentrations were lower than those usually observed in urban areas or in other forest areas in Europe. The wind direction was one of the most important factors affecting changes in the daily concentrations of these compounds. Scots pine needles were analysed with the same system to obtain reference data for identification of biogenic compounds in aerosol particles. Other organic compounds found in this study included hopanes, steranes, n-alkanals, n-alkan-2-ones, oxy-PAH, and alkyl-PAH; some biogenic products, including oxidation products of monoterpenes, were also identified. (orig.)

Production of extracts from preserved olives using supercritical CO2 and preliminary evaluation of its polyphenol content

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Maria João Cebola

2014-06-01

Full Text Available The supercritical fluid extraction (SFE technique was used to obtain extracts from a sample simulating an olive pomace, obtained from preserved olives. The objective was to achieve the extraction of polyphenolic components from this matrix which is considered a hazardous waste from the production of olive oil. The supercritical fluid used was carbon dioxide and the SFE studies were conducted in two stages, the first at a pressure of 200 bar and 40 ºC and the second stage at 300 bar, 45 ºC and using ethanol as co-solvent. In both cases the SFE was performed for 3 hours. The first stage was carried out to obtain a cleaner matrix and the second step was aimed at the components of interest. The overall mass yield obtained was 5.5 %. Preliminary HPLC screening of the samples obtained and also of the water in which the olives were preserved showed that the polyphenol compounds were mostly in the latter.

Supercritical Carbon Dioxide and Microwave-Assisted Extraction of Functional Lipophilic Compounds from Arthrospira platensis

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Diego A. Esquivel-Hernández

2016-05-01

Full Text Available Arthrospira platensis biomass was used in order to obtain functional lipophilic compounds through green extraction technologies such as supercritical carbon dioxide fluid extraction (SFE and microwave-assisted extraction (MAE. The temperature (T factor was evaluated for MAE, while for SFE, pressure (P, temperature (T, and co-solvent (ethanol (CS were evaluated. The maximum extraction yield of the obtained oleoresin was (4.07% ± 0.14% and (4.27% ± 0.10% for SFE and MAE, respectively. Extracts were characterized by gas chromatography mass spectrometry (GC-MS and gas chromatography flame ionization detector (GC-FID. The maximum contents of functional lipophilic compounds in the SFE and MAE extracts were: for carotenoids 283 ± 0.10 μg/g and 629 ± 0.13 μg/g, respectively; for tocopherols 5.01 ± 0.05 μg/g and 2.46 ± 0.09 μg/g, respectively; and for fatty acids 34.76 ± 0.08 mg/g and 15.88 ± 0.06 mg/g, respectively. In conclusion, the SFE process at P 450 bar, T 60 °C and CS 53.33% of CO2 produced the highest yield of tocopherols, carotenoids and fatty acids. The MAE process at 400 W and 50 °C gives the best extracts in terms of tocopherols and carotenoids. For yield and fatty acids, the MAE process at 400 W and 70 °C produced the highest values. Both SFE and MAE showed to be suitable green extraction technologies for obtaining functional lipophilic compounds from Arthrospira platensis.

Use of on-line supercritical fluid extraction-supercritical fluid chromatography/tandem mass spectrometry to analyze disease biomarkers in dried serum spots compared with serum analysis using liquid chromatography/tandem mass spectrometry.

Science.gov (United States)

Suzuki, Makoto; Nishiumi, Shin; Kobayashi, Takashi; Sakai, Arata; Iwata, Yosuke; Uchikata, Takato; Izumi, Yoshihiro; Azuma, Takeshi; Bamba, Takeshi; Yoshida, Masaru

2017-05-30

The analytical stability and throughput of biomarker assays based on dried serum spots (DSS) are strongly dependent on the extraction process and determination method. In the present study, an on-line system based on supercritical fluid extraction-supercritical fluid chromatography coupled with tandem mass spectrometry (SFE-SFC/MS/MS) was established for analyzing the levels of disease biomarkers in DSS. The chromatographic conditions were investigated using the ODS-EP, diol, and SIL-100A columns. Then, we optimized the SFE-SFC/MS/MS method using the diol column, focusing on candidate biomarkers of oral, colorectal, and pancreatic cancer that were identified using liquid chromatography (LC)/MS/MS. By using this system, four hydrophilic metabolites and 17 hydrophobic metabolites were simultaneously detected within 15 min. In an experiment involving clinical samples, PC 16:0-18:2/16:1-18:1 exhibited 93.8% sensitivity and 64.3% specificity, whereas PC 17:1-18:1/17:0-18:2 showed 81.3% sensitivity and 92.9% specificity for detecting oral cancer. In addition, assessments of the creatine levels demonstrated 92.3% sensitivity and 78.6% specificity for detecting colorectal cancer. The results of this study indicate that our method has great potential for clinical diagnosis and would be suitable for large-scale screening. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Fatty acid profile and elemental content of avocado (Persea americana Mill.) oil--effect of extraction methods.

Science.gov (United States)

Reddy, Mageshni; Moodley, Roshila; Jonnalagadda, Sreekanth B

2012-01-01

Interest in vegetable oil extracted from idioblast cells of avocado fruit is growing. In this study, five extraction methods to produce avocado oil have been compared: traditional solvent extraction using a Soxhlet or ultrasound, Soxhlet extraction combined with microwave or ultra-turrax treatment and supercritical fluid extraction (SFE). Traditional Soxhlet extraction produced the most reproducible results, 64.76 ± 0.24 g oil/100 g dry weight (DW) and 63.67 ± 0.20 g oil/100 g DW for Hass and Fuerte varieties, respectively. Microwave extraction gave the highest yield of oil (69.94%) from the Hass variety. Oils from microwave extraction had the highest fatty acid content; oils from SFE had wider range of fatty acids. Oils from Fuerte variety had a higher monounsaturated: saturated FA ratio (3.45-3.70). SFE and microwave extraction produced the best quality oil, better than traditional Soxhlet extraction, with the least amount of oxidizing metals present. Copyright © Taylor & Francis Group, LLC

Dicty_cDB: SFE484 [Dicty_cDB

Lifescience Database Archive (English)

Full Text Available AAAAACTAGTAATTTAAAAAAAAA AAAAACCAAAAAAAAAAXXXXXXXXXXATGATGTCGAATGTCCANATTTCCATANA...seq. 137 3' end seq. ID SFE484Z 3' end seq. >SFE484Z.Seq ----------ATGATGTCGAATGTCCANATTTCCATANATGTGTTTAAANA...AACTAGTAATTTAAAAAAAAA AAAAACCAAAAAAAAAA----------ATGATGTCGAATGTCCANATTTCCATANATGTG TTTAAANACGTGGNGGNATCTTAAG

Construction of a supercritical fluid extraction (SFE equipment: validation using annatto and fennel and extract analysis by thin layer chromatography coupled to image

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Júlio Cezar Flores JOHNER

2016-01-01

Full Text Available Abstract The present work describes setting up a laboratory unit for supercritical fluid extraction. In addition to its construction, a survey of cost was done to compare the cost of the homemade unit with that of commercial units. The equipment was validated using an extraction of annatto seeds’ oil, and the extraction and fractionation of fennel oil were used to validate the two separators; for both systems, the solvent was carbon dioxide. The chemical profiles of annatto and fennel extracts were assessed using thin layer chromatography; the images of the chromatographic plates were processed using the free ImageJ software. The cost survey showed that the homemade equipment has a very low cost (~US$ 16,000 compared to commercial equipment. The extraction curves of annatto were similar to those obtained in the literature (yield of 3.8% oil. The separators were validated, producing both a 2.5% fraction of fennel seed extract rich in essential oils and another extract fraction composed mainly of oleoresins. The ImageJ software proved to be a low-cost tool for obtaining an initial evaluation of the chemical profile of the extracts.

Online recovery of radiocesium from soil, tissue paper and plant samples by supercritical fluid extraction

International Nuclear Information System (INIS)

Kanekar, A.S.; Pathak, P.N.; Mohapatra, P.K.

2014-01-01

The feasibility of recovery of radio-cesium from soil, tissue papers, and plant samples has been evaluated by supercritical fluid extraction (SFE) route employing calix(4)arene-mono(crown-6) (CC) dissolved in acetonitrile. These studies showed that quantitative recovery of 137 Cs from soil samples was difficult under the conditions of these studies. However, experiments performed on tissue papers (cellulose matrix) showed quantitative recovery of 137 Cs. On the other hand, 137 Cs recovery from plant samples varied between ∼50 % (for stems) and ∼67.2 % (for leaves) employing 1x10 -3 M CC + 4 M HNO 3 dissolved in acetonitrile. (author)

Wheat germ oil extracted by supercritical carbon dioxide with ethanol: Fatty acid composition

International Nuclear Information System (INIS)

Parczewska-Plesnar, B.; Brzozowski, R.; Gwardiak, H.; Białecka-Florjańczyk, E.; Bujnowski, Z.

2016-01-01

In this work, supercritical fluid extraction (SFE) using CO2 with ethanol as entrainer was performed at a temperature of 40 o C under a pressure of 21 MPa. For comparison, a similar extraction without the entrainer was carried out. The extraction yield of wheat germ using supercritical CO2 with ethanol was slightly higher (10.7 wt%) than that of extraction without the entrainer (9.9 wt%). Fractions of SFE extracts were collected separately during the experiments and the composition of fatty acids in each fraction was analyzed. The SFE extracted oils were rich (63.4-71.3%) in the most valuable polyunsaturated fatty acids (PUFA) and their content in all collected fractions was approximately constant. Similar PUFA contents were found in the reference samples of oils extracted by n-hexane (66.2-67.0%), while the commercial cold-pressed oil contained significantly less PUFA (60.2%). These results show a higher nutritional value of the oil obtained by extraction with supercritical CO2 than cold pressed oil which is generally considered to be very valuable. [es

Supercritical fluid extraction of volatile and non-volatile compounds from Schinus molle L.

Directory of Open Access Journals (Sweden)

M. S. T. Barroso

2011-06-01

Full Text Available Schinus molle L., also known as pepper tree, has been reported to have antimicrobial, antifungal, anti-inflammatory, antispasmodic, antipyretic, antitumoural and cicatrizing properties. This work studies supercritical fluid extraction (SFE to obtain volatile and non-volatile compounds from the aerial parts of Schinus molle L. and the influence of the process on the composition of the extracts. Experiments were performed in a pilot-scale extractor with a capacity of 1 L at pressures of 9, 10, 12, 15 and 20 MPa at 323.15 K. The volatile compounds were obtained by CO2 supercritical extraction with moderate pressure (9 MPa, whereas the non-volatile compounds were extracted at higher pressure (12 to 20 MPa. The analysis of the essential oil was carried out by GC-MS and the main compounds identified were sabinene, limonene, D-germacrene, bicyclogermacrene, and spathulenol. For the non-volatile extracts, the total phenolic content was determined by the Folin-Ciocalteau method. Moreover, one of the goals of this study was to compare the experimental data with the simulated yields predicted by a mathematical model based on mass transfer. The model used requires three adjustable parameters to predict the experimental extraction yield curves.

Extraction of three bioactive diterpenoids from Andrographis paniculata: effect of the extraction techniques on extract composition and quantification of three andrographolides using high-performance liquid chromatography.

Science.gov (United States)

Kumar, Satyanshu; Dhanani, Tushar; Shah, Sonal

2014-10-01

Andrographis paniculata (Burm.f.) wall.ex Nees (Acanthaceae) or Kalmegh is an important medicinal plant finding uses in many Ayurvedic formulations. Diterpenoid compounds andrographolides (APs) are the main bioactive phytochemicals present in leaves and herbage of A. paniculata. The efficiency of supercritical fluid extraction (SFE) using carbon dioxide was compared with the solid-liquid extraction techniques such as solvent extraction, ultrasound-assisted solvent extraction and microwave-assisted solvent extraction with methanol, water and methanol-water as solvents. Also a rapid and validated reverse-phase high-performance liquid chromatography-diode array detection method was developed for the simultaneous determination of the three biologically active compounds, AP, neoandrographolide and andrograpanin, in the extracts of A. paniculata. Under the best SFE conditions tested for diterpenoids, which involved extraction at 60°C and 100 bar, the extractive efficiencies were 132 and 22 µg/g for AP and neoandrographolide, respectively. The modifier percentage significantly affected the extraction efficiency. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Analytical method for Dioxin and Organo-Chlorinated Compounds:(II) Comparison of Extraction Methods of Dioxins from XAD-2 Adsorbent

International Nuclear Information System (INIS)

Yang, Jeong Soo; Lee, Sung Kwang; Park, Young Hun; Lee, Dai Woon

1999-01-01

Supercritical fluid extraction (SFE), ultrasonic extraction (USE), and accelerated solvent extraction (ASE) were compared with the well known Soxhlet extraction for the extraction of polychlorinated biphenyls (PCB s ) and polychlorinated dibenzo-p-dioxins (PCDD s ) from the XAD-2 resin which was used to adsorb PCDD s in the atmosphere. XAD-2 resin spiked with five PCDD s was chosen as a sample. The optimum conditions for the extraction of PCDD s by SFE were turned out to be the use of CO 2 modified with 10% toluene at 100 .deg. C and 350 atm, with 5 min static extraction followed by 20 min dynamic extraction. SFE gave a good extraction rate with good reproducibility for PCDD s ranging from 68 to 98%. The ultrasonic extraction of PCDD s from XAD-2 was investigated and compared with other extractions. A probe type method was compared with a bath type. Two extraction solvents, toluene and acetone were compared with their mixture. The use of their mixture in probe type, with 9 minutes of extraction time, was found to be the optimum condition. The average recovery of the five PCDD s for USE was 82-93%. Accelerated solvent extraction (ASE) with a liquid solvent, a new technique for sample preparation, was performed under elevated temperatures and pressures. The effect of temperature on the efficiency of ASE was investigated. The extraction time for a 10 g sample was less than 15 min, when the organic solvent was η-hexaneacetone mixture (1 : 1, v/v). Using ASE, the average recoveries of five PCDD s ranged from 90 to 103%. SFE, USE, and ASE were faster and less laborious than Soxhlet extraction. The former three methods required less solvent than Soxhlet extraction. SFE required no concentration of the solvent extracts. SFE and ASE failed to perform simultaneous parallel extractions because of instrumental limitations

Analysis of the essential oils of Alpiniae Officinarum Hance in different extraction methods

Science.gov (United States)

Yuan, Y.; Lin, L. J.; Huang, X. B.; Li, J. H.

2017-09-01

It was developed for the analysis of the essential oils of Alpiniae Officinarum Hance extracted by steam distillation (SD), ultrasonic assisted solvent extraction (UAE) and supercritical fluid extraction (SFE) via gas chromatography mass spectrometry (GC-MS) combined with retention index (RI) method. There were multiple volatile components of the oils extracted by the three above-mention methods respectively identified; meanwhile, each one was quantified by area normalization method. The results indicated that the content of 1,8-Cineole, the index constituent, by SD was similar as SFE, and higher than UAE. Although UAE was less time consuming and consumed less energy, the oil quality was poorer due to the use of organic solvents was hard to degrade. In addition, some constituents could be obtained by SFE but could not by SD. In conclusion, essential oil of different extraction methods from the same batch of materials had been proved broadly similarly, however, there were some differences in composition and component ratio. Therefore, development and utilization of different extraction methods must be selected according to the functional requirements of products.

Supercritical fluid extraction as an on-line clean-up technique for determination of riboflavin vitamins in food samples by capillary electrophoresis with fluorimetric detection.

Science.gov (United States)

Zougagh, Mohammed; Ríos, Angel

2008-08-01

An automatic method for the separation and determination of riboflavin (RF) vitamins (RF, flavin mononucleotide and flavin adenine dinucleotide) in food samples (chicken liver, tablet and powder milk) is proposed. The method is based on the on-line coupling of a supercritical fluid extractor (SFE) with a continuous flow-CE system with guided optical fiber fluorimetric detection (CF-CE-FD). The whole SFE-CF-CE-FD arrangement allowed the automatic treatment of food samples (clean-up of the sample followed by the extraction of the analytes), and the direct introduction of a small volume of the extracted plug to the CE-FD system for the determination of RF vitamins. Fluorescence detection introduced an appropriated sensitivity and contributed to avoid interferences of nonfluorescent polar compounds coming from the matrix samples in the extracted plug. Electrophoretic responses were linear within the 0.05-1 microg/g range, whereas the detection limits of RF vitamins were in the 0.036-0.042 microg/g range. The proposed arrangement opens up interesting prospects for the direct determination of polar analytes in complex samples with a good throughput and high level of automation.

Development of Nordic Standard for analysis of oil and fat in water based on supercritical fluid extraction. Preliminary study, part 2

International Nuclear Information System (INIS)

Jenssen, L.

1994-06-01

This report describes a preliminary study of a method of determining oil in water. The method is based on solid phase extraction and supercritical fluid extraction (SPE-SFE). The oil is extracted from the water by absorption to extraction disks from which it is then desorbed by supercritical carbon dioxide and detected by means of infrared spectrophotometry or gas chromatography. The results of the study will indicate if the method is suitable as a future substitute for the present Norwegian Standard, NS 9803 (Swedish Standard, SS 02 8145). The method has been validated using water samples with addition of real oil to 1-100 ppm. The accuracy is almost 70%, and the method has good repeatability and is linear in the 1-100 ppm range. 5 refs., 6 figs., 10 tabs

The Effects of Different Extraction Methods on Antioxidant Properties, Chemical Composition, and Thermal Behavior of Black Seed (Nigella sativa L.) Oil

Science.gov (United States)

Mohammed, Nameer Khairullah; Abd Manap, Mohd Yazid; Muhialdin, Belal J.; Alhelli, Amaal M.

2016-01-01

The Nigella sativa L. popularly referred to as black seeds are widely used as a form of traditional nutrition and medicine. N. sativa seeds were used for the extraction of their oil by way of supercritical fluid extraction (SFE) and cold press (CP) to determine the physicochemical properties, antioxidant activity, and thermal behavior. The GC-MS results showed the primary constituents in the Nigella sativa oil (NSO) were Caryophyllene (17.47%) followed by thymoquinone (TQ) (11.80%), 1,4-Cyclohexadiene (7.17%), longifolene (3.5%), and carvacrol (1.82%). The concentration of TQ was found to be 6.63 mg/mL for oil extracted using SFE and 1.56 mg/mL for oil extracted by CP method. The antioxidant activity measured by DPPH and the IC50 was 1.58 mg/mL and 2.30 mg/mL for SFE oil and cold pressed oil, respectively. The ferric reducing/antioxidant power (FRAP) activity for SFE oil and CP oil was 538.67 mmol/100 mL and 329.00 mmol/100 mL, respectively. The total phenolic content (TPC) of SFE oil was 160.51 mg/100 mL and 94.40 mg/100 mL for CP oil presented as gallic acid equivalents (GAE). This research showed that a high level of natural antioxidants could be derived from NSO extracted by SFE. PMID:27642353

The Effects of Different Extraction Methods on Antioxidant Properties, Chemical Composition, and Thermal Behavior of Black Seed (Nigella sativa L. Oil

Directory of Open Access Journals (Sweden)

Nameer Khairullah Mohammed

2016-01-01

Full Text Available The Nigella sativa L. popularly referred to as black seeds are widely used as a form of traditional nutrition and medicine. N. sativa seeds were used for the extraction of their oil by way of supercritical fluid extraction (SFE and cold press (CP to determine the physicochemical properties, antioxidant activity, and thermal behavior. The GC-MS results showed the primary constituents in the Nigella sativa oil (NSO were Caryophyllene (17.47% followed by thymoquinone (TQ (11.80%, 1,4-Cyclohexadiene (7.17%, longifolene (3.5%, and carvacrol (1.82%. The concentration of TQ was found to be 6.63 mg/mL for oil extracted using SFE and 1.56 mg/mL for oil extracted by CP method. The antioxidant activity measured by DPPH and the IC50 was 1.58 mg/mL and 2.30 mg/mL for SFE oil and cold pressed oil, respectively. The ferric reducing/antioxidant power (FRAP activity for SFE oil and CP oil was 538.67 mmol/100 mL and 329.00 mmol/100 mL, respectively. The total phenolic content (TPC of SFE oil was 160.51 mg/100 mL and 94.40 mg/100 mL for CP oil presented as gallic acid equivalents (GAE. This research showed that a high level of natural antioxidants could be derived from NSO extracted by SFE.

Extraction of functional ingredients from spinach (Spinacia oleracea L.) using liquid solvent and supercritical CO₂ extraction.

Science.gov (United States)

Jaime, Laura; Vázquez, Erika; Fornari, Tiziana; López-Hazas, María del Carmen; García-Risco, Mónica R; Santoyo, Susana; Reglero, Guillermo

2015-03-15

In this work three different techniques were applied to extract dry leaves of spinach (Spinacia oleracea): solid-liquid extraction (SLE), pressurised liquid extraction (PLE) and supercritical fluid extraction (SFE) to investigate the influence of extraction solvent and technique on extracts composition and antioxidant activity. Moreover, the influence of carotenoids and phenolic compounds on the antioxidant and anti-inflammatory activities of spinach extracts was also studied. The higher concentrations of carotenoids and the lower content of phenolic compounds were observed in the supercritical CO₂ extracts; whereas water and/or ethanol PLE extracts presented low amounts of carotenoids and the higher concentrations of phenolic compounds. PLE extract with the highest content of phenolic compounds showed the highest antioxidant activity, although SFE carotenoid rich extract also showed a high antioxidant activity. Moreover, both extracts presented an important anti-inflammatory activity. PLE seems to be a good technique for the extraction of antioxidant and anti-inflammatory compounds from spinach leaves. Moreover, spinach phenolic compounds and carotenoids present a high antioxidant activity, whereas spinach carotenoids seem to show a higher anti-inflammatory activity than phenolic compounds. It is worth noting that of our knowledge this is the first time the anti-inflammatory activity of lipophilic extracts from spinach leaves is reported. © 2014 Society of Chemical Industry.

Extraction of polycyclic aromatic hydrocarbons from polluted soils with binary and ternary supercritical phases

International Nuclear Information System (INIS)

Hollender, J.; Shneine, J.; Dott, W.; Heinzel, M.; Hagemann, H.W.; Gotz, G.K.E.

1997-01-01

The paper describes how supercritical fluid extractions (SFE) using carbon dioxide and modifiers (n-hexane, cyclohexane, toluene, methyl tert-butyl ether, methoxybenzene, dichloromethane, propanone, pyridine, methanol) as well as modifier mixtures (methanol-containing diethylamide, 2-aminoethan-1-ol, acetic acid) were performed to extract polycyclic aromatic hydrocarbons (PAHs) from real environmental samples polluted to a minor extent by mineral oil products and highly contaminated by brown coal tar. Comparing the results with those from Soxhlet extraction utilizing dichloromethane and SFE using pure carbon dioxide show that acidic or basic co-solvents give the highest PAH yields. Extraction efficiency decreases with reduced polarity of the modifier used and increases at higher concentrations of co-solvent. To explain the SFE results, several mechanisms of disruption of matrix-PAH interactions are considered: the competition between the modifier molecules and the active sites of soil's organic and inorganic matter to interact with non-covalent bondings to the analytes; and the splitting of electron donor-acceptor complexes between humic substances and PAHs induced by Lewis acids or Lewis bases

High Pressure Extraction of Antioxidants from Solanum stenotomun Peel

Directory of Open Access Journals (Sweden)

Enrique J. Martínez de la Ossa

2013-03-01

Full Text Available In the work described here, two techniques for the recovery of anthocyanins from potato peel were studied and compared. One of the techniques employed was supercritical fluid extraction (SFE with pure CO2 or with CO2 and ethanol as cosolvent and the other technique was pressurized liquid extraction (PLE, where the solvent used was ethanol in water acidified to pH 2.6. The effects of pressure and temperature were studied and the anthocyanin contents obtained were statistically analyzed. In SFE the use of low pressure (100 bar and high temperature (65 °C was desirable for the anthocyanin extraction. With PLE the anthocyanin contents are increased considerably, and the best yields were obtained at 100 bar and 80 °C. This result is in correspondence with antioxidant activity index values (1.66 obtained in a DPPH antioxidant activity assay. In the extracts obtained with PLE the phenolic compounds were also determined, but the main compounds presented in the extract are anthocyanins.

Supercritical Carbon Dioxide extraction of Aloe Emodin and Barbaloin from Aloe Vera L. leaves and their in-vitro cytotoxic activity

International Nuclear Information System (INIS)

Kabbash, A.; El-Soud, K.A.; Zalat, E.; Shoeib, N.; Yagi, A.

2008-01-01

Aloe emodin and barbaloin, isolated as the active principles of the medicinal plant Aloe vera L., were extracted by supercritical fluid extraction (SFE) and analyzed by high performance liquid chromatography (HPLC). With optimized operating conditions for SFE, aloe emodin and barbaloin were quantitatively extracted from A. Vera leaves within 20 minutes at a flow rate of 0.3 ml/min, temperature and pressure at 40C and 3200 Psi respectively with the addition of 1 ml of methanol as a modifier. Separation of aloe emodin and barbaloin, in a pure form, from the SFE extract was achieved using a semi-preparative column. The cytotoxic activity of both aloe emodin and barbaloin were evaluated using the in-vitro MTT colorimetric assay. Aloe emodin showed a cytotoxic activity on two human colon cancer cells lines (DLD-1 and HD-29) with IC 8.94 and 10.78 M respectively, while barbaloin had no effect. (author)

Phenolic Extracts from Wild Olive Leaves and Their Potential as Edible Oils Antioxidants

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Theodora-Ioanna Lafka

2013-01-01

Full Text Available The kinetics solid-liquid extraction of phenolics from wild olive leaves was elaborated using different mathematical models (Peleg, second order, Elovich, and power law model. As solvents, methanol, ethanol, ethanol:water 1:1, n-propanol, isopropanol and ethyl acetate were used. The second order model best described the solvent extraction process, followed by the Elovich model. The most effective solvent was ethanol with optimum phenol extraction conditions 180 min, solvent to sample ratio 5:1 v/w and pH 2. Ethanol extract exhibited the highest antiradical activity among solvent and supercritical fluid extraction (SFE extracts, which in addition showed the highest antioxidant capacity compared to synthetic and natural food antioxidants such as BHT, ascorbyl palmitate and vitamin E. Antioxidant potential of SFE extract was quite high, although its phenolic potential was not. Leaf extracts were proven to be good protectors for olive and sunflower oils at levels of 150 ppm.

Economic Analysis of an Integrated Annatto Seeds-Sugarcane Biorefinery Using Supercritical CO2 Extraction as a First Step

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Juliana Q. Albarelli

2016-06-01

Full Text Available Recently, supercritical fluid extraction (SFE has been indicated to be utilized as part of a biorefinery, rather than as a stand-alone technology, since besides extracting added value compounds selectively it has been shown to have a positive effect on the downstream processing of biomass. To this extent, this work evaluates economically the encouraging experimental results regarding the use of SFE during annatto seeds valorization. Additionally, other features were discussed such as the benefits of enhancing the bioactive compounds concentration through physical processes and of integrating the proposed annatto seeds biorefinery to a hypothetical sugarcane biorefinery, which produces its essential inputs, e.g., CO2, ethanol, heat and electricity. For this, first, different configurations were modeled and simulated using the commercial simulator Aspen Plus® to determine the mass and energy balances. Next, each configuration was economically assessed using MATLAB. SFE proved to be decisive to the economic feasibility of the proposed annatto seeds-sugarcane biorefinery concept. SFE pretreatment associated with sequential fine particles separation process enabled higher bixin-rich extract production using low-pressure solvent extraction method employing ethanol, meanwhile tocotrienols-rich extract is obtained as a first product. Nevertheless, the economic evaluation showed that increasing tocotrienols-rich extract production has a more pronounced positive impact on the economic viability of the concept.

Enhancing Phenolic Contents and Antioxidant Potentials of Antidesma thwaitesianum by Supercritical Carbon Dioxide Extraction

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Warut Poontawee

2015-01-01

Full Text Available Supercritical fluid extraction (SFE has increasingly gained attention as an alternative technique for extraction of natural products without leaving toxic residues in extracts. Antidesma thwaitesianum Muell. Arg. (Phyllanthaceae, or ma mao, has been reported to exhibit antioxidant health benefits due to its phenolic constituents. To determine whether SFE technique could impact on phenolic contents and associated antioxidant potentials, ripe fruits of Antidesma thwaitesianum (Phyllanthaceae were extracted using supercritical carbon dioxide (SC-CO2 and conventional solvents (ethanol, water. The results showed that the SC-CO2 extract contained significantly higher yield, total phenolic, flavonoid, and proanthocyanidin contents than those obtained from ethanol and water. It also demonstrated the greatest antioxidant activities as assessed by ABTS radical cation decolorization, DPPH radical scavenging, and ferric reducing antioxidant power (FRAP assays. Further analysis using high-performance liquid chromatography with diode array and mass spectrometry detectors (HPLC-DAD/MSD revealed the presence of catechin as a major phenolic compound of Antidesma thwaitesianum (Phyllanthaceae, with the maximum amount detected in the SC-CO2 extract. These data indicate that SFE technology improves both quantity and quality of Antidesma thwaitesianum fruit extract. The findings added more reliability of using this technique to produce high added value products from this medicinal plant.

IN VIVO STUDIES AND STABILITY STUDY OF CLADOPHORA GLOMERATA EXTRACT AS A COSMETIC ACTIVE INGREDIENT.

Science.gov (United States)

Fabrowska, Joanna; Kapuscinska, Alicja; Leska, Boguslawa; Feliksik-Skrobich, Katarzyna; Nowak, Izabela

2017-03-01

Marine algae are widely used as cosmetics raw materials. Likewise, freshwater alga Cladophora glomerata may be a good source of fatty acids and others bioactive agents. The aims of this study was to find out if the addition of the extract from the freshwater C. glonerata affects the stability of prepared cosmetic emulsions and to investigate in vivo effects of the extract in cosmetic formulations on hydration and elasticity of human skin. Extract from the freshwater C. glonierata was obtained using supercritical fluid extraction (SFE). Two forms of O/W emulsions were prepared: placebo and emulsion containing 0.5% of Cladophora SFE extract. The stability of obtained emulsions was investigated by using Turbiscan Lab Expert. Emulsions were applied by .volunteers daily. Corneometer was used to evaluate skin hydration and cutometer to examine skin elasticity. Measurements were conducted at reference point (week 0) and after 1st, 2nd, 3rd and 4th week of application. The addition of Cladophora extract insignificantly affected stability of the emulsion. The extract from C. glomerata in the emulsion influenced the improvement of both skin hydration and its elasticity. Thus, freshwater C. glonierata extract prepared via SFE method may be considered as an effective cosmetic raw material used as a moisturizing and firming agent.

Supercritical fluid extraction of ginger (Zingiber Officinale Var. Amarum) : Global yield and composition study

Science.gov (United States)

Fitriady, Muhammad Arifuddin; Sulaswatty, Anny; Agustian, Egi; Salahuddin, Aditama, Deska Prayoga Fauzi

2017-11-01

An experiment to observe the effect of temperature and time process in ginger rhizome-Supercritical Fluid Extraction (SFE) using CO2 as the solvent has been conducted. The ginger rhizome (Zingiber Officinale Var. Amarum) was washed, drained, sliced, sun-dried, and then stored in a sealed bag prior to usage. The temperature and time process variables are each 35, 40, 45°C and 2, 4, 6 hours respectively with the pressure variable are 3500, 4000, and 4500 psi. It is found that the highest yield (2.9%) was achieved using temperature of 40°C and pressure of 4500 psiwith the process time of 4 hours. However, using the curve-fitting method, it is suggested to use 42°C as the temperature and 5 hours, 7 minutes, and 30 seconds (5.125 Hours) as the time process to obtain the highest yield. The temperature changes will affect both solvent and vapor pressure of diluted compounds of the ginger which will influence the global yield and the composition of the extract. The three major components of the extract are curcumene, zingiberene, and β - sesquipellandrene,

Optimization of ultrasonic-assisted extraction of pomegranate (Punica granatum L.) seed oil.

Science.gov (United States)

Tian, Yuting; Xu, Zhenbo; Zheng, Baodong; Martin Lo, Y

2013-01-01

The effectiveness of ultrasonic-assisted extraction (UAE) of pomegranate seed oil (PSO) was evaluated using a variety of solvents. Petroleum ether was the most effective for oil extraction, followed by n-hexane, ethyl acetate, diethyl ether, acetone, and isopropanol. Several variables, such as ultrasonic power, extraction temperature, extraction time, and the ratio of solvent volume and seed weight (S/S ratio) were studied for optimization using response surface methodology (RSM). The highest oil yield, 25.11% (w/w), was obtained using petroleum ether under optimal conditions for ultrasonic power, extraction temperature, extraction time, and S/S ratio at 140 W, 40 °C, 36 min, and 10 ml/g, respectively. The PSO yield extracted by UAE was significantly higher than by using Soxhlet extraction (SE; 20.50%) and supercriti cal fluid extraction (SFE; 15.72%). The fatty acid compositions were significantly different among the PSO extracted by Soxhlet extraction, SFE, and UAE, with punicic acid (>65%) being the most dominant using UAE. Copyright © 2012 Elsevier B.V. All rights reserved.

Supercritical Algal Extracts: A Source of Biologically Active Compounds from Nature

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Izabela Michalak

2015-01-01

Full Text Available The paper discusses the potential applicability of the process of supercritical fluid extraction (SFE in the production of algal extracts with the consideration of the process conditions and yields. State of the art in the research on solvent-free isolation of biologically active compounds from the biomass of algae was presented. Various aspects related with the properties of useful compounds found in cells of microalgae and macroalgae were discussed, including their potential applications as the natural components of plant protection products (biostimulants and bioregulators, dietary feed and food supplements, and pharmaceuticals. Analytical methods of determination of the natural compounds derived from algae were discussed. Algal extracts produced by SFE process enable obtaining a solvent-free concentrate of biologically active compounds; however, detailed economic analysis, as well as elaboration of products standardization procedures, is required in order to implement the products in the market.

Quality of Cosmetic Argan Oil Extracted by Supercritical Fluid Extraction from Argania spinosa L.

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Chouaa Taribak

2013-01-01

Full Text Available Argan oil has been extracted using supercritical CO2. The influence of the variables pressure (100, 200, 300, and 400 bar and temperature (35, 45, 55°C was investigated. The best extraction yields were achieved at a temperature of 45°C and a pressure of 400 bar. The argan oil extracts were characterized in terms of acid, peroxide and iodine values, total tocopherol, carotene, and fatty acids content. Significant compositional differences were not observed between the oil samples obtained using different pressures and temperatures. The antioxidant capacity of the argan oil samples was high in comparison to those of walnut, almond, hazelnut, and peanut oils and comparable to that of pistachio oil. The physicochemical parameters of the extracted oils obtained by SFE, Soxhlet, and traditional methods are comparable. The technique used for oil processing does not therefore markedly alter the quality of argan oil.

Chemical Composition and Biological Activity of Volatile Extracts from Leaves and Fruits of Schinusterebinthifolius Raddi from Tunisia

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Alessandra Piras

2017-01-01

Full Text Available Volatile oils composition from leaves and ripe fruits of pink pepper (Schinus terebinthifolius Raddi growing in Tunisia were investigated using GC-FID and GC-MS techniques. Volatile oil extraction was achieved by hydrodistillation (HD using a Clevenger apparatus and by supercritical fluid extraction (SFE using carbon dioxide. All plant organs, gave SFE extracts chiefly composed by a -pinene, a -phellandrene, b -phellandrene, germacrene D and bicyclogermacrene. In the case of the fruits, both extraction techniques gave volatile oils of similar composition; whereas the comparison between the HD and SFE leave oils revealed important differences in the content of a -pinene (6.1 % vs traces, a -phellandrene (22.7 % vs 0.8 % and b -phellandrene (14.6 % vs 1.2 %. All volatile samples were evaluated against yeasts and dermatophyte strains, being more active against Cryptococcus neoformans, particularly the volatile oil from the fruits, with MIC values of (0.32-0.64 mg/mL.Moreover, this oil revealed an inhibitory effect on germ tube formation in C. albicans at sub-inhibitory concentration. At the concentration of MIC/8 the inhibition of filamentation was more than 70 %.

Integrated intelligent instruments using supercritical fluid technology for soil analysis

International Nuclear Information System (INIS)

Liebman, S.A.; Phillips, C.; Fitzgerald, W.; Levy, E.J.

1994-01-01

Contaminated soils pose a significant challenge for characterization and remediation programs that require rapid, accurate and comprehensive data in the field or laboratory. Environmental analyzers based on supercritical fluid (SF) technology have been designed and developed for meeting these global needs. The analyzers are designated the CHAMP Systems (Chemical Hazards Automated Multimedia Processors). The prototype instrumentation features SF extraction (SFE) and on-line capillary gas chromatographic (GC) analysis with chromatographic and/or spectral identification detectors, such as ultra-violet, Fourier transform infrared and mass spectrometers. Illustrations are given for a highly automated SFE-capillary GC/flame ionization (FID) configuration to provide validated screening analysis for total extractable hydrocarbons within ca. 5--10 min, as well as a full qualitative/quantitative analysis in 25--30 min. Data analysis using optional expert system and neural networks software is demonstrated for test gasoline and diesel oil mixtures in this integrated intelligent instrument approach to trace organic analysis of soils and sediments

Chemical composition and antioxidant/antimicrobial activities in supercritical carbon dioxide fluid extract of Gloiopeltis tenax.

Science.gov (United States)

Zheng, Jiaojiao; Chen, Yicun; Yao, Fen; Chen, Weizhou; Shi, Ganggang

2012-12-01

Gloiopeltis tenax (G. tenax) is widely distributed along the Chinese coastal areas and is commonly used in the treatment of diarrhea and colitis. This study aimed at investigating the bioactivities of the volatile constituents in G. tenax. We extracted the essential constituents of G. tenax by supercritical carbon dioxide extraction (CO₂-SFE), then identified and analyzed the constituents by gas chromatography-mass spectrometry (GC-MS). In total, 30 components were identified in the G. tenax extract. The components showed remarkable antioxidant activity (radical scavenging activity of 2,2-diphenyl-1-picrylhydrazyl (DPPH)), lipid peroxidation inhibition capacity (in a β-carotene/linoleic acid-coupled oxidation reaction), and hydroxyl radical-scavenging activity (by deoxyribose degradation by iron-dependent hydroxyl radical), compared to butylated hydroxytoluene. In microdilution assays, G. tenax extracts showed a moderate inhibitory effects on Staphyloccocus aureus (minimum inhibitory concentration (MIC) = 3.9 mg/mL), Enterococcus faecalis (7.8 mg/mL), Pseudomonas aeruginosa (15.6 mg/mL), and Escherichia coli (3.9 mg/mL). Antioxidant and antimicrobial activities of G. tenax were related to the active chemical composition. These results suggest that the CO₂-SFE extract from G. tenax has potential to be used as a natural antioxidant and antimicrobial agent in food processing.

Chemical Composition and Antioxidant/Antimicrobial Activities in Supercritical Carbon Dioxide Fluid Extract of Gloiopeltis tenax

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Jiaojiao Zheng

2012-11-01

Full Text Available Gloiopeltis tenax (G. tenax is widely distributed along the Chinese coastal areas and is commonly used in the treatment of diarrhea and colitis. This study aimed at investigating the bioactivities of the volatile constituents in G. tenax. We extracted the essential constituents of G. tenax by supercritical carbon dioxide extraction (CO2-SFE, then identified and analyzed the constituents by gas chromatography-mass spectrometry (GC-MS. In total, 30 components were identified in the G. tenax extract. The components showed remarkable antioxidant activity (radical scavenging activity of 2,2-diphenyl-1-picrylhydrazyl (DPPH, lipid peroxidation inhibition capacity (in a β-carotene/linoleic acid-coupled oxidation reaction, and hydroxyl radical-scavenging activity (by deoxyribose degradation by iron-dependent hydroxyl radical, compared to butylated hydroxytoluene. In microdilution assays, G. tenax extracts showed a moderate inhibitory effects on Staphyloccocus aureus (minimum inhibitory concentration (MIC = 3.9 mg/mL, Enterococcus faecalis (7.8 mg/mL, Pseudomonas aeruginosa (15.6 mg/mL, and Escherichia coli (3.9 mg/mL. Antioxidant and antimicrobial activities of G. tenax were related to the active chemical composition. These results suggest that the CO2-SFE extract from G. tenax has potential to be used as a natural antioxidant and antimicrobial agent in food processing.

KOMPARASI MODEL PEMBELAJARAN TPS DAN SFE TERHADAP KEMAMPUAN PEMAHAMAN KONSEP

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Febri Susanto

2014-03-01

Full Text Available Penelitian ini bertujuan untuk mengetahui apakah pembelajaran model Think Pair Share (TPS dan model Student Facilitator and Explaining (SFE pada siswa kelas X materi jarak pada bangun ruang dapat mencapai ketuntasan belajar dan untuk mengetahui manakah yang lebih efektif antara pembelajaran model Think Pair Share (TPS dan model Student Facilitator and Explaining (SFE. Populasi dalam penelitian ini adalah siswa kelas X SMA N 1 Kota Tegal tahun pelajaran 2012/2013 yang berada dalam sembilan kelas. Sembilan kelas tersebut kemudian dipilih dua kelas secara acak untuk dijadikan sampel dalam penelitian ini yaitu kelas X 2 sebagai kelas eksperimen 1 dan kelas X 1 sebagai kelas eksperimen 2. Uji ketuntasan belajar memberikan hasil yaitu siswa kelas eksperimen 1 dan 2 telah mencapai ketuntasan belajar. Uji kesamaan dua proporsi memberikan hasil yakni proporsi ketuntasan belajar pada aspek pemahaman konsep siswa kelas eksperimen 1 sama baiknya dibanding proporsi ketuntasan belajar pada aspek pemahaman konsep siswa kelas eksperimen 2. Hasil Penelitian menunjukkan pembelajaran model TPS dan SFE pada materi jarak pada bangun ruang telah mencapai ketuntasan belajar dan model pembelajaran TPS sama efektifnya dengan pembelajaran model SFE.

Effects of grape (vitis labrusca b.) peel and seed extracts on phenolics, antioxidants and anthocyanins in grape juice

International Nuclear Information System (INIS)

Ghafoor, K.; Juhaimi, F.; Choi, Y.H.

2011-01-01

Grape peel and seed are good sources of important bioactive components such as phenolics, anthocyanins and antioxidants. Recovery of these components and their proper utilization is important for the development of functional foods. We have utilized the extracts of grape peel and seed obtained by ultrasonic-assisted (UAE) and supercritical fluid extractions (SFE) for the enrichment of Campbell Early grape juice (CEJ). CEJ samples were analyzed for different functional compounds and it was observed that the addition of these extracts in CEJ significantly improved total phenolic compounds, antioxidants, anti radical activities and total anthocyanin contents. HPLC analysis of CEJ samples containing these extracts showed that the phenolic acids (benzoic and cinnamic acids) and catechins contents were also significantly improved with the addition of grape peel and seed extracts. Generally SFE extracts proved to be of superior quality for the functional enrichment in CEJ. The sensory evaluation revealed that the CEJ samples containing the extracts had good overall acceptability. (author)

Analysis of particulate polycyclic aromatic hydrocarbons by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry

Science.gov (United States)

Shimmo, Masahiko; Adler, Heidi; Hyötyläinen, Tuulia; Hartonen, Kari; Kulmala, Markku; Riekkola, Marja-Liisa

An on-line supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry (SFE-LC-GC-MS) method was developed for the analysis of the particulate polycyclic aromatic hydrocarbons (PAHs). The limits of detection of the system for the quantification standards were in the range of 0.25-0.57 ng, while the limits of determinations for filter samples varied from 0.02 to 0.04 ng m -3 (24 h sampling). The linearity was excellent from 5 to 300 ng ( R2>0.967). The analysis could be carried out in a closed system without tedious manual sample pretreatment and with no risk of errors by contamination or loss of the analytes. The results of the SFE-LC-GC-MS method were comparable with those for Soxhlet and shake-flask extractions with GC-MS. The new method was applied to the analysis of PAHs collected by high-volume filter in the Helsinki area to study the seasonal trend of the concentrations. The individual PAH concentrations varied from 0.015 to more than 1 ng m -3, while total PAH concentrations varied from 0.81 to 5.68 ng m -3. The concentrations were generally higher in winter than in summer. The mass percentage of the total PAHs in total suspended particulates ranged from 2.85×10 -3% in July to 15.0×10 -3% in December. Increased emissions in winter, meteorological conditions, and more serious artefacts during the sampling in summer season may explain the concentration profiles.

Design Criteria for Bagless Transfer System (BTS) Packaging System

International Nuclear Information System (INIS)

RISENMAY, H.R.

2000-01-01

This document provides the criteria for the design and installation of a Bagless Transfer System (BTS); Blend, Sieve and Balance Equipment; and Supercritical Fluid Extraction System (SFE). The project consists of 3 major modules: (1) Bagless Transfer System (BTS) Module; (2) Blend, Sieve and Balance Equipment; and (3) Supercritical Fluid Extraction (SFE) Module

Quantitative aspects of directly coupled supercritical fluid extraction-capillary gas chromatography with a conventional split/splitless injector as interface

NARCIS (Netherlands)

Lou, X.W.; Janssen, J.G.M.; Cramers, C.A.

1993-01-01

The quant. aspects of online supercrit. fluid extn.-capillary gas chromatog. (SFE-GC) with a split/splitless injector as interface were studied. Special attention was paid to the discrimination behavior and the reproducibility of the split/splitless interface. A simple exptl. set-up is proposed that

The influence of extraction methods on composition and antioxidant properties of rice bran oil

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Noppawat Pengkumsri

2015-09-01

Full Text Available AbstractThe current study was employed to assess the influence of the different extraction methods on total tocols, γ-oryzanol content, and antioxidant properties of Chiang Mai Black rice, Mali Red rice, and Suphanburi-1 Brown rice bran oil. Rice bran oil (RBO was extracted by Hexane, Hot pressed, Cold pressed, and Supercritical Fluid Extraction (SFe methods. High yield of RBO was extracted by hexane and SFe methods. Total and subgroups of tocols, and γ-oryzanol content were determined by HPLC. The hexane extracted sample accounts for high content of γ-oryzanol and tocols. Besides, all of RBO extracts contain a significantly high amount of γ-tocotrienol. In vitro antioxidant assay results indicated that superior quality of oil was recovered by hexane extraction. The temperature in the extraction process also affects the value of the oil. Superior quality of oil was recovered by hexane extraction, in terms of phytochemical contents and antioxidant properties compared to other tested extraction methods. Further, thorough study of factors compromising the quality and quantity of RBO recovery is required for the development of enhanced functional foods and other related products.

Use of Immobilised Lipase from Candida antarctica in Supercritical Fluid Extraction of Borage (Borago officinalis L. Seed Oil

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Egidijus Daukšas

2008-01-01

Full Text Available This study aims at the investigation of the possibilities to use immobilised lipase from Candida antarctica in supercritical fluid extraction (SFE of borage (Borago officinalis L. see doil. The first series of experiments was performed to measure the extract yields obtained with pure CO2 and with the added entrainer (ethanol. The yield increased more than twice after increasing the extraction pressure from 15 to 25 MPa. Further increase to 35 MPa was less effective. The effect of the entrainer was not significant in most cases. Palmitic (13.1–16.1 %, oleic (13.4–23.8 %, linoleic (33.8–48.4 % and linolenic (8.8–16.3 % acids were dominant in all extracted oils. Further experiments involved the use of enzyme. In this case the first extractor was loaded with ground borage seeds, the second one was filled with the enzyme. The total yield obtained at 15, 25 and 35 MPa was (8.8±0.2, (23.6±0.2 and (28.9±1.1 %, respectively. Thin layer chromatography (TLC of fatty acid ethyl esters showed that the content of esters was higher in the extract obtained in one extractor system at 15 MPa, compared to 35 MPa.

A Simplified Method to Estimate Sc-CO2 Extraction of Bioactive Compounds from Different Matrices: Chili Pepper vs. Tomato By-Products

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Francesca Venturi

2017-04-01

Full Text Available In the last few decades, the search for bioactive compounds or “target molecules” from natural sources or their by-products has become the most important application of the supercritical fluid extraction (SFE process. In this context, the present research had two main objectives: (i to verify the effectiveness of a two-step SFE process (namely, a preliminary Sc-CO2 extraction of carotenoids followed by the recovery of polyphenols by ethanol coupled with Sc-CO2 in order to obtain bioactive extracts from two widespread different matrices (chili pepper and tomato by-products, and (ii to test the validity of the mathematical model proposed to describe the kinetics of SFE of carotenoids from different matrices, the knowledge of which is required also for the definition of the role played in the extraction process by the characteristics of the sample matrix. On the basis of the results obtained, it was possible to introduce a simplified kinetic model that was able to describe the time evolution of the extraction of bioactive compounds (mainly carotenoids and phenols from different substrates. In particular, while both chili pepper and tomato were confirmed to be good sources of bioactive antioxidant compounds, the extraction process from chili pepper was faster than from tomato under identical operating conditions.

Supercritical fluid extraction of uranium and thorium from nitric acid medium using organophosphorous compounds

Energy Technology Data Exchange (ETDEWEB)

Pitchaiah, K.C.; Sujatha, K.; Rao, C.V.S. Brahmmananda; Subramaniam, S.; Sivaraman, N.; Rao, P.R. Vasudeva [Indira Gandhi Centre for Atomic Research, Kalpakkam (India). Chemistry Group

2015-06-01

In recent years, Supercritical Fluid Extraction (SFE) technique has been widely used for the extraction of metal ions. In the present study, extraction of uranium from nitric acid medium was investigated using supercritical carbon dioxide (Sc-CO{sub 2}) containing various organophosphorous compounds such as trialkyl phosphates e.g. tri-iso-amyl phosphate (TiAP), tri-sec-butyl phosphate (TsBP) and tri-n-butyl phosphate (TBP), dialkylalkyl phosphonates, e.g. diamylamyl phosphonate (DAAP) and dibutyl butyl phosphonate (DBBP), dialkyl hydrogen phosphonates, e.g. dioctyl hydrogen phosphonate (DOHP), dioctylphosphineoxide (DOPO), trioctyl phosphine oxide (TOPO), n-octylphenyl N,N-diisobutyl carbamoylmethylphosphine oxide (CMPO) and di-2-ethyl-hexyl phosphoric acid (HDEHP). Some of these ligands have been investigated for the first time in the supercritical phase for the extraction of uranium. The extraction efficiency of uranium was studied with TiAP, DAAP and DBBP as a function of nitric acid concentration; the kinetics of the equilibration period (static extraction) and transportation of the metal complex (dynamic extraction) was investigated. The influence of pressure and temperature on the extraction behaviour of uranium with DAAP was studied from 4 N HNO{sub 3}. The extraction efficiency of uranium from 4 N nitric acid medium was found to increase in the order of phosphates < phosphonates < HDEHP < TOPO < CMPO. In the case of phosphates and phosphonates, the maximum extraction of uranium was found to be from 4 N HNO{sub 3} medium. The acidic extractants, HDEHP and DOHP showed relatively higher extraction at lower acidities. The relative extraction of uranium and thorium from their mixture was also examined using Sc-CO{sub 2} containing phosphates, phosphonates and TOPO. The ligand, TsBP provided better fractionation between uranium and thorium compared to trialkyl phosphates, dialkyl alkyl phosphonates and TOPO.

Evaluation of Supercritical Extracts of Algae as Biostimulants of Plant Growth in Field Trials

OpenAIRE

Michalak, Izabela; Chojnacka, Katarzyna; Dmytryk, Agnieszka; Wilk, Rados?aw; Gramza, Mateusz; R?j, Edward

2016-01-01

The aim of the field trials was to determine the influence of supercritical algal extracts on the growth and development of winter wheat (variety Akteur). As a raw material for the supercritical fluid extraction (SFE), the biomass of microalga Spirulina plantensis, brown seaweed – Ascophyllum nodosum and Baltic green macroalgae was used. Forthial and Asahi SL constituted the reference products. It was found that the tested biostimulants did not influence statistically significantly the plant...

Optimization and evaluation of foxtail millet (Setaria italica bran oil by supercritical carbon dioxide extraction

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Pang, M.

2015-12-01

Full Text Available A Box-Behnken central composite design combined with the response surface methodology (RSM was used to optimize the parameters of a supercritical fluid extraction (SFE of foxtail millet bran oil (FMBO. Results showed that a maximum oil yield of 7.97% was achieved under the optimal conditions with an extracting pressure of 30.03MPa, extracting temperature of 47.93 °C; and an extraction time of 2.3 h. The quality of the oil obtained from SFE and solvent extraction (SE was evaluated by proximate analysis to include physicochemical properties, fatty acids and sterol compounds. The FBMO obtained from SFE showed a much lower phospholipid (0.188 mg/g content and a preferable color compared to the oil from SE, while it contained a higher content of total sterols, 1.55%. The thermal gravimetric analysis results showed one major regime of weight loss over a temperature range of 300–500 °C. The results show that FBMO obtained by SFE can be a promising nutritional source for food fortification and is understood to have more potentially healthy biological properties.Un diseño Box-Behnken combinado con la metodología de superficie de respuesta (RSM se usó para optimizar los parámetros de extracción mediante fluido supercrítico (SFE de aceite de salvado de mijo (FMBO. Los resultados mostraron que un rendimiento máximo de extracción de aceite del 7,97% se logró en las condiciones óptimas correspondientes a una presión de 30.03MPa, una temperatura 47.93 °C y un tiempo 2,3H. Además, se evaluó la calidad del aceite obtenido por SFE y mediante extracción con disolvente (SE a partir de un análisis proximal que incluye propiedades fisicoquímicas, ácidos grasos y esteroles. El aceite de FBMO obtenido mediante SFE mostró un contenido mucho menor de fosfolípidos (0.188 mg/g y un color mas aceptable que el aceite de la SE, mientras que contenía un mayor contenido de esteroles totales: 1,55%. El resultado del análisis térmico gravimétrico mostr

Wheat germ oil extracted by supercritical carbon dioxide with ethanol: Fatty acid composition

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Parczewska-Plesnar, B.

2016-09-01

Full Text Available In this work, supercritical fluid extraction (SFE using CO2 with ethanol as entrainer was performed at a temperature of 40 oC under a pressure of 21 MPa. For comparison, a similar extraction without the entrainer was carried out. The extraction yield of wheat germ using supercritical CO2 with ethanol was slightly higher (10.7 wt% than that of extraction without the entrainer (9.9 wt%. Fractions of SFE extracts were collected separately during the experiments and the composition of fatty acids in each fraction was analyzed. The SFE extracted oils were rich (63.4-71.3% in the most valuable polyunsaturated fatty acids (PUFA and their content in all collected fractions was approximately constant. Similar PUFA contents were found in the reference samples of oils extracted by n-hexane (66.2-67.0%, while the commercial cold-pressed oil contained significantly less PUFA (60.2%. These results show a higher nutritional value of the oil obtained by extraction with supercritical CO2 than cold pressed oil which is generally considered to be very valuable.En este trabajo, la extracción con fluidos supercríticos (SFE usando CO2 con etanol como agente de arrastre se realizó a 40 °C bajo una presión de 21 MPa. Se ha llevado a cabo la comparación con una extracción similar sin agente de arrastre. El rendimiento de la extracción de germen de trigo usando CO2 supercrítico con etanol fue ligeramente mayor (10,7% en peso que la de extracción sin agente de arrastre (9,9% en peso. Se recogieron por separado fracciones de extractos SFE durante los experimentos y se analizó la composición de ácidos grasos en cada fracción. Los aceites extraídos mediante SFE eran ricos en los ácidos grasos poliinsaturados más valiosos (63,4-71,3%, (PUFA y su contenido en todas las fracciones recogidas fue aproximadamente constante. Un contenido similar de PUFA fueron encontrados en muestras de referencia de los aceites extraídos con n-hexano (66,2-67,0%, mientras que el

Supercritical CO2 extraction of raw propolis and its dry ethanolic extract

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L. C. Paviani

2012-06-01

Full Text Available Three types of propolis extract were prepared and analyzed with respect to their global extraction yields and with respect to the concentration of the following markers: 3,5-diprenyl-4-hydroxycinnamic acid; 3-prenyl-4-hydroxycinnamic acid; 4-hydroxycinnamic acid and 4-methoxy-3,5,7-trihydroxyflavone. The extract EEP (ethanolic extract of propolis was obtained by the conventional method from raw propolis using ethanol as solvent. The extracts (SFE were obtained by supercritical solvent extraction from the raw propolis using supercritical carbon dioxide (sc-CO2, with and without the addition of ethanol as a co-solvent. The fractionated supercritical extracts (FSCE were obtained by fractionation (extract and raffinate of the dry EEP with sc-CO2. EEP yields of 39.5% were obtained and maximum global extraction yields were 7.3% for SFE with no co-solvent, 51% for SFE with 15% ethanol and 18% for the FSCE extract fraction. The concentrations of the markers in the different extracts differed as a function of the operational parameters, indicating that the addition of co-solvent and the selectivity of sc-CO2 could be manipulated so as to obtain extracts with the yields and concentrations of interest.

Identification of Bioactivity, Volatile and Fatty Acid Profile in Supercritical Fluid Extracts of Mexican arnica

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J. Saúl García-Pérez

2016-09-01

Full Text Available Supercritical fluid extraction (SFE is a sustainable technique used for the extraction of lipophilic metabolites such as pigments and fatty acids. Arnica plant is considered a potential candidate material with high antioxidant and antimicrobial activities. Therefore, in this study, a locally available Heterotheca inuloides, also known as Mexican arnica, was analyzed for the extraction of high-value compounds. Based on different pressure (P, temperature (T, and co-solvent (CoS, four treatments (T were prepared. A maximum 7.13% yield was recovered from T2 (T = 60 °C, P = 10 MPa, CoS = 8 g/min, followed by 6.69% from T4 (T = 60 °C, P = 30 MPa, CoS = 4 g/min. Some bioactive sesquiterpenoids such as 7-hydroxycadalene, caryophyllene and δ-cadinene were identified in the extracts by GC/MS. The fatty acid profile revealed that the main components were palmitic acid (C16:0, followed by linoleic acid (C18:2ω6c, α-linolenic acid (C18:3ω3 and stearic acid (C18:0 differing in percent yield per treatment. Antibacterial activities were determined by the agar diffusion method, indicating that all the treatments exerted strong antibacterial activity against S. aureus, C. albicans, and E. coli strains. The antioxidant capacity of the extracts was also measured by three in vitro assays, DPPH, TEAC and FRAP, using Trolox as a standard. Results showed high antioxidant capacity enabling pharmaceutical applications of Mexican arnica.

Qualitative comparison of active compounds between red and green Mariposa Christia Vespertillonis leaves extracts

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Osman, M. S.; Ghani, Z. A.; Ismail, N. F.; Razak, N. A. A.; Jaapar, J.; Ariff, M. A. M.

2017-09-01

At present time, Mariposa Christia Vespertillonis (MCV) leave has become popular for its anti-cancer and thus is used widely among the traditional medicine in Malaysia. There are several types of MCV plants and the one that is currently well-known for traditional medicine in Malaysia is the green MCV (GMCV). Red MCV (RMCV) is another type of MCV plant which can also be found easily in Malaysia. In this study, the active compounds for GMCV and RMCV will be compared and analyzed by using Liquid Chromatography - Mass Spectrometry (LC-MS). The active compounds will be extracted from the MCV leaves by using Supercritical Fluid Extraction (SFE). The findings of this study indicates the global yield of the MCV oils is 31 mg/g while the compound identification indicates the presence of anti-cancer, anti-inflammatory and beneficial phytochemicals. This work is an explorative study to reveal the potential of MCV to be extracted using SFE method as potential therapeutic plants for the traditional medicine in Malaysia.

Supercritical fluid extraction and ultra performance liquid chromatography of respiratory quinones for microbial community analysis in environmental and biological samples.

Science.gov (United States)

Hanif, Muhammad; Atsuta, Yoichi; Fujie, Koichi; Daimon, Hiroyuki

2012-03-05

Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE) and ultra performance liquid chromatography (UPLC) method for the analysis of bacterial respiratory quinones (RQ) in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA) detector was successfully applied to the simultaneous determination of ubiquinones (UQ) and menaquinones (MK) without tedious pretreatment. Supercritical carbon dioxide (scCO(2)) extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost) and biological samples (swine and Japanese quail feces).

Auraptene, a Major Compound of Supercritical Fluid Extract of Phalsak (Citrus Hassaku Hort ex Tanaka, Induces Apoptosis through the Suppression of mTOR Pathways in Human Gastric Cancer SNU-1 Cells

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Jeong Yong Moon

2015-01-01

Full Text Available The supercritical extraction method is a widely used process to obtain volatile and nonvolatile compounds by avoiding thermal degradation and solvent residue in the extracts. In search of phytochemicals with potential therapeutic application in gastric cancer, the supercritical fluid extract (SFE of phalsak (Citrus hassaku Hort ex Tanaka fruits was analyzed by gas chromatography-mass spectrometry (GC-MS. Compositional analysis in comparison with the antiproliferative activities of peel and flesh suggested auraptene as the most prominent anticancer compound against gastric cancer cells. SNU-1 cells were the most susceptible to auraptene-induced toxicity among the tested gastric cancer cell lines. Auraptene induced the death of SNU-1 cells through apoptosis, as evidenced by the increased cell population in the sub-G1 phase, the appearance of fragmented nuclei, the proteolytic cleavage of caspase-3 and poly(ADP-ribose polymerase (PARP protein, and depolarization of the mitochondrial membrane. Interestingly, auraptene induces an increase in the phosphorylation of Akt, which is reminiscent of the effect of rapamycin, the mTOR inhibitor that triggers a negative feedback loop on Akt/mTOR pathway. Taken together, these findings provide valuable insights into the anticancer effects of the SFE of the phalsak peel by revealing that auraptene, the major compound of it, induced apoptosis in accompanied with the inhibition of mTOR in SNU-1 cells.

Isolation of Bioactive Compounds from Sunflower Leaves (Helianthus annuus L.) Extracted with Supercritical Carbon Dioxide.

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El Marsni, Zouhir; Torres, Ascension; Varela, Rosa M; Molinillo, José M G; Casas, Lourdes; Mantell, Casimiro; Martinez de la Ossa, Enrique J; Macias, Francisco A

2015-07-22

The work described herein is a continuation of our initial studies on the supercritical fluid extraction (SFE) with CO2 of bioactive substances from Helianthus annuus L. var. Arianna. The selected SFE extract showed high activity in the wheat coleoptile bioassay, in Petri dish phytotoxicity bioassays, and in the hydroponic culture of tomato seeds. Chromatographic fractionations of the extracts and a spectroscopic analysis of the isolated compounds showed 52 substances belonging to 10 different chemical classes, which were mainly sesquiterpene lactones, diterpenes, and flavonoids. Heliannuol M (31), helivypolides K and L (36, 37), and helieudesmanolide B (38) are described for the first time in the literature. Metabolites have been tested in the etiolated wheat coleoptile bioassay with good results in a noteworthy effect on germination. The most active compounds were also tested on tomato seeds, heliannuol A (30) and leptocarpin (45) being the most active, with values similar to those of the commercial herbicide.

Effect of ultrasound on the supercritical CO2 extraction of bioactive compounds from dedo de moça pepper (Capsicum baccatum L. var. pendulum).

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Dias, Arthur Luiz Baião; Arroio Sergio, Camilla Scarelli; Santos, Philipe; Barbero, Gerardo Fernandéz; Rezende, Camila Alves; Martínez, Julian

2016-07-01

Extracts with bioactive compounds were obtained from the red pepper variety "dedo de moça" (Capsicum baccatum L. var. pendulum) through supercritical fluid extraction with carbon dioxide assisted by ultrasound (SFE-US). The process was tested at pressures of 15, 20 and 25 MPa; temperatures of 40, 50 and 60 °C, and ultrasonic powers of 200, 400 and 600 W applied during 40, 60 and 80 min of extraction. The CO2 mass flow rate was fixed at 1.7569 × 10(-4) kg/s. Global yield, phenolic content, antioxidant capacity and capsaicinoid concentration were evaluated in the extracts. The application of ultrasound raised the global extraction yield of SFE up to 45%. The phenolic content of the extract increased with the application of higher ultrasound power and radiation time. The capsaicinoid yield was also enhanced with ultrasound up to 12%. However, the antioxidant capacity did not increase with the ultrasound application. The BET-based model and the broken and intact cell model fitted well to the kinetic SFE curves. The BET-based model with three adjustable parameters resulted in the best fits to the experimental data. Field emission scanning electron microscopy (FESEM) images showed that SFE disturbed the vegetable matrix, releasing particles from the inner region of the plant cells to their surface. When the ultrasound was applied this effect was more pronounced. On the other hand, cracks, fissures or any sign of rupture were not identified on the sample surface. Copyright © 2016 Elsevier B.V. All rights reserved.

Analysis of gamma irradiated pepper constituents, 3

International Nuclear Information System (INIS)

Takagi, Kazuko; Okuyama, Tsuneo; Yamauchi, Yoshio; Saito, Muneo.

1988-01-01

The extraction of pepper perfume by use of supercritical fluid extraction (SFE) was investigated. Carbon dioxide was used as supercritical mobile phase. SFE was achieved by follow conditions, temperature was 40deg C, pressure was 200 kgf/cm 2 , 5 % methanol was added to mobile phase and the extraction time was 60 minutes. The extracted fraction by this method was yellow oily substance and was pepper perfume rich fraction, while the residue of extraction had not only perfume but also any pungency. And it seems that most part of pepper perfume was extracted by Supercritical fluid extraction. The perfume fraction was analyzed by two way method, that is, supercritical fluid chromatography (SFC) and reversed phase HPLC. SFC conditions were same as SFE. HPLC conditions were described as the first report. By both methods, about 7 peaks were detected. According to their analysis of this fraction, the main component was identified as piperine. On the chromatogram of reversed phase HPLC of extract, most peaks were eluted later than piperine. And it is thought that most perfume components have high hydrophobicity more than piperine. The change of perfume of pepper was able to be discussed based on the extraction by SFE. (author)

JV Task 92 - Alcoa/Retec SFE and SPME

Energy Technology Data Exchange (ETDEWEB)

Steven Hawthorne

2009-02-15

This report summarizes the work performed by the Energy & Environmental Research Center (EERC) under the U.S. Department of Energy Jointly Sponsored Research Program JV Task 92, which is a continuation of JV9. Successful studies performed in 1999 through the end of 2008 demonstrated the potential for using selective supercritical fluid extraction (SFE) and a solid-phase microextraction (SPME) method for measuring sediment pore water polycyclic aromatic hydrocarbons (PAHs) to mimic the bioavailability of PAHs from manufactured gas plant and aluminum smelter soils and sediments both in freshwater and saltwater locations. The studies that the EERC has performed with the commercial partners have continued to generate increased interest in both the regulatory communities and in the industries that have historically produced or utilized coal tar products. Both ASTM International and the U.S. Environmental Protection Agency (EPA) have accepted the pore water method developed at the EERC as standard methods. The studies have demonstrated the effectiveness of our techniques in predicting bioavailability of PAHs from ca. 250 impacted and background field sediments and soils. The field demonstrations from the final years of the project continued to build the foundation data for acceptance of our methods by the regulatory communities. The JV92 studies provide the single largest database in the world that includes measures of PAH bioavailability along with biological end points. These studies clearly demonstrated that present regulatory paradigms based on equilibrium partitioning greatly overpredict bioavailability. These investigations also laid the foundation for present (non-JV) studies being applied to PAHs and polychlorinated biphenyls (PCBs) at EPA Superfund sites, investigations into PAH and PCB bioavailability at U.S Department of Defense sites, and the application of the techniques to investigating the bioavailability of chlorinated dioxins and furans from impacted

Aqueous CO2 vs. aqueous extraction of soils as a preparative procedure for acute toxicity testing

International Nuclear Information System (INIS)

Yates, G.W.; Burks, S.L.

1994-01-01

This study was to determine if contaminated soils extracted with supercritical CO 2 (SFE) would yield different results from soils extracted with an aqueous media. Soil samples from an abandoned oil refinery were subjected to aqueous and SFE extraction. Uncontaminated control sites were compared with contaminated sites. Each extract was analyzed for 48 hour acute Ceriodaphnia LC50s and Microtox reg-sign EC50s. Comparisons were then made between the aqueous extracts and the SFE extracts. An additional study was made with HPLC chromatographs of the SFE contaminated site extracts to determine if there was a correlation between LC50 results and peak area of different sections of the chromatograph. The 48 hour Ceriodaphnia LC50 of one contaminated site showed a significant increase in toxicity with the supercritical extract compared to the aqueous extract. All contaminated sites gave toxic responses with the supercritical procedure. The Microtox reg-sign assay showed a toxic response with 2 of the 3 contaminated sites for both aqueous and SFE extracts. Results indicate that the Ceriodaphnia assays were more sensitive than Microtox reg-sign to contaminants found in the refinery soil. SFE controls did not show adverse effects with the Ceriodaphnia, but did have a slight effect with Microtox reg-sign. The best correlation (r 2 > 0.90) between the Ceriodaphnia LC50s and the peak areas of the chromatographs was obtained for sections with an estimated log K ow of 1 to 5. SFE extraction provided a fast, efficient and inexpensive method of collecting and testing moderately non-polar to strongly non-polar organic contaminants from contaminated soils

Pesticide residues in canned foods, fruits, and vegetables: the application of Supercritical Fluid Extraction and chromatographic techniques in the analysis.

Science.gov (United States)

El-Saeid, Mohamed H

2003-12-11

Multiple pesticide residues have been observed in some samples of canned foods, frozen vegetables, and fruit jam, which put the health of the consumers at risk of adverse effects. It is quite apparent that such a state of affairs calls for the need of more accurate, cost-effective, and rapid analytical techniques capable of detecting the minimum concentrations of the multiple pesticide residues. The aims of this paper were first, to determine the effectiveness of the use of Supercritical Fluid Extraction (SFE) and Supercritical Fluid Chromatography (SFC) techniques in the analysis of the levels of pesticide residues in canned foods, vegetables, and fruits; and second, to contribute to the promotion of consumer safety by excluding pesticide residue contamination from markets. Fifteen different types of imported canned and frozen fruits and vegetables samples obtained from the Houston local food markets were investigated. The major types of pesticides tested were pyrethroids, herbicides, fungicides, and carbamates. By using these techniques, the overall data showed 60.82% of the food samples had no detection of any pesticide residues under this investigation. On the other hand, 39.15% different food samples were contaminated by four different pyrethroid residues +/- RSD% ranging from 0.03 +/- 0.005 to 0.05 +/- 0.03 ppm, of which most of the pyrethroid residues were detected in frozen vegetables and strawberry jam. Herbicide residues in test samples ranged from 0.03 +/- 0.005 to 0.8 +/- 0.01 ppm. Five different fungicides, ranging from 0.05 +/- 0.02 to 0.8 +/- 0.1 ppm, were found in five different frozen vegetable samples. Carbamate residues were not detected in 60% of investigated food samples. It was concluded that SFE and SFC techniques were accurate, reliable, less time consuming, and cost effective in the analysis of imported canned foods, fruits, and vegetables and are recommended for the monitoring of pesticide contaminations.

Supercritical Fluid Chromatography/Fourier Transform Infrared Spectroscopy Of Food Components

Science.gov (United States)

Calvey, Elizabeth M.; Page, Samuel W.; Taylor, Larry T.

1989-12-01

Supercritical fluid (SF) technologies are being investigated extensively for applications in food processing. The number of SF-related patents issued testifies to the level of interest. Among the properties of materials at temperatures and pressures above their critical points (supercritical fluids) is density-dependent solvating power. Supercritical CO2 is of particular interest to the food industry because of its low critical temperature (31.3°C) and low toxicity. Many of the components in food matrices react or degrade at elevated temperatures and may be adversely affected by high temperature extractions. Likewise, these components may not be amenable to GC analyses. Our SF research has been in the development of methods employing supercritical fluid chromatography (SFC) and extraction (SFE) coupled to a Fourier transform infrared (FT-IR) spectrometer to investigate food composition. The effects of processing techniques on the isomeric fatty acid content of edible oils and the analysis of lipid oxidation products using SFC/FT-IR with a flow-cell interface are described.

Optimisation of supercritical carbon dioxide extraction of essential oil of flowers of tea (Camellia sinensis L.) plants and its antioxidative activity.

Science.gov (United States)

Chen, Zhenchun; Mei, Xin; Jin, Yuxia; Kim, Eun-Hye; Yang, Ziyin; Tu, Youying

2014-01-30

To extract natural volatile compounds from tea (Camellia sinensis) flowers without thermal degradation and residue of organic solvents, supercritical fluid extraction (SFE) using carbon dioxide was employed to prepare essential oil of tea flowers in the present study. Four important parameters--pressure, temperature, static extraction time, and dynamic extraction time--were selected as independent variables in the SFE. The optimum extraction conditions were the pressure of 30 MPa, temperature of 50°C, static time of 10 min, and dynamic time of 90 min. Based on gas chromatography-mass spectrometry analysis, 59 compounds, including alkanes (45.4%), esters (10.5%), ketones (7.1%), aldehydes (3.7%), terpenes (3.7%), acids (2.1%), alcohols (1.6%), ethers (1.3%) and others (10.3%) were identified in the essential oil of tea flowers. Moreover, the essential oil of tea flowers showed relatively stronger DPPH radical scavenging activity than essential oils of geranium and peppermint, although its antioxidative activity was weaker than those of essential oil of clove, ascorbic acid, tert-butylhydroquinone, and butylated hydroxyanisole. Essential oil of tea flowers using SFE contained many types of volatile compounds and showed considerable DPPH scavenging activity. The information will contribute to the future application of tea flowers as raw materials in health-care food and food flavour industries. © 2013 Society of Chemical Industry.

Supercritical Fluid Extraction and Ultra Performance Liquid Chromatography of Respiratory Quinones for Microbial Community Analysis in Environmental and Biological Samples

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Koichi Fujie

2012-03-01

Full Text Available Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE and ultra performance liquid chromatography (UPLC method for the analysis of bacterial respiratory quinones (RQ in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA detector was successfully applied to the simultaneous determination of ubiquinones (UQ and menaquinones (MK without tedious pretreatment. Supercritical carbon dioxide (scCO2 extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost and biological samples (swine and Japanese quail feces.

Vaccinium meridionale Swartz Supercritical CO2 Extraction: Effect of Process Conditions and Scaling Up

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Alexis López-Padilla

2016-06-01

Full Text Available Vaccinium meridionale Swartz (Mortiño or Colombian blueberry is one of the Vaccinium species abundantly found across the Colombian mountains, which are characterized by high contents of polyphenolic compounds (anthocyanins and flavonoids. The supercritical fluid extraction (SFE of Vaccinium species has mainly focused on the study of V. myrtillus L. (blueberry. In this work, the SFE of Mortiño fruit from Colombia was studied in a small-scale extraction cell (273 cm3 and different extraction pressures (20 and 30 MPa and temperatures (313 and 343 K were investigated. Then, process scaling-up to a larger extraction cell (1350 cm3 was analyzed using well-known semi-empirical engineering approaches. The Broken and Intact Cell (BIC model was adjusted to represent the kinetic behavior of the low-scale extraction and to simulate the large-scale conditions. Extraction yields obtained were in the range 0.1%–3.2%. Most of the Mortiño solutes are readily accessible and, thus, 92% of the extractable material was recovered in around 30 min. The constant CO2 residence time criterion produced excellent results regarding the small-scale kinetic curve according to the BIC model, and this conclusion was experimentally validated in large-scale kinetic experiments.

Vaccinium meridionale Swartz Supercritical CO2 Extraction: Effect of Process Conditions and Scaling Up

Science.gov (United States)

López-Padilla, Alexis; Ruiz-Rodriguez, Alejandro; Restrepo Flórez, Claudia Estela; Rivero Barrios, Diana Marsela; Reglero, Guillermo; Fornari, Tiziana

2016-01-01

Vaccinium meridionale Swartz (Mortiño or Colombian blueberry) is one of the Vaccinium species abundantly found across the Colombian mountains, which are characterized by high contents of polyphenolic compounds (anthocyanins and flavonoids). The supercritical fluid extraction (SFE) of Vaccinium species has mainly focused on the study of V. myrtillus L. (blueberry). In this work, the SFE of Mortiño fruit from Colombia was studied in a small-scale extraction cell (273 cm3) and different extraction pressures (20 and 30 MPa) and temperatures (313 and 343 K) were investigated. Then, process scaling-up to a larger extraction cell (1350 cm3) was analyzed using well-known semi-empirical engineering approaches. The Broken and Intact Cell (BIC) model was adjusted to represent the kinetic behavior of the low-scale extraction and to simulate the large-scale conditions. Extraction yields obtained were in the range 0.1%–3.2%. Most of the Mortiño solutes are readily accessible and, thus, 92% of the extractable material was recovered in around 30 min. The constant CO2 residence time criterion produced excellent results regarding the small-scale kinetic curve according to the BIC model, and this conclusion was experimentally validated in large-scale kinetic experiments. PMID:28773640

The Study on the Composition of Yongdamsagan-tang(龍膽瀉肝湯’s Essential Oil Obtained by Supercritical Carbon Dioxide Extraction

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Shin Min-Seop

2008-03-01

Full Text Available Objectives : This study was performed to analyze the effective components of essential oil obtained from Yongdamsagan-tang, which has been efficacious against leukorrhea in gynecologic diseases. Methods : I obtained the essential oils of Yongdamsagan-tang by hydrodistillation extraction method and supercritical fluid extraction(SFE method, and then I analyzed those by GC/MS(Gas Chromatography/Mass Spectrum. Results : 1. The optimum SFE(Supercritical Fluid Extraction condition was obtained in the following experiment conditions: pressure 200atm, temperature 45℃, duration of extraction 25minutes. 2. With GC(Gas Chromatography and GC/MS(Gas Chromato- graphy/Mass Spectrum analysis, I identified 37 compounds in the Yongdamsagan-tang's essential oil obtained through the SFE method. The main compounds were as follows : 3-Methyl-but-2-enoic acid,2,2-dimethyl-8-oxo-3,4-dihydro-2H,8H -pyrano[3,2-g]chromen-3-yl ester(49.81 %, (Z-6-Pentadecen-1 -ol(3.19%, (--Spathulenol(2.40%. 3. I identified 4 compounds in the Yongdamsagan-tang's essential oil obtained through the hydrodistillation method. The main compounds were as follows : 3-Methyl-but-2-enoic acid, 2,2-dimethyl-8-oxo-3,4-dihydro-2H,8H-pyrano[3,2-g]chromen-3-yl ester(2.61%. 4. 3 - Methy l - but - 2 - enoic acid, 2, 2 - dimethyl - 8 - oxo - 3, 4 - dihydro - 2H, 8H - pyrano[3, 2 - g] chromen - 3 - yl ester, all were identified in both the SFE method and the hydrodistillation method, but the others were not identified in common. 5. I also conducted an additional test in order to examine the essential oil's antimicrobial action against bacteria. Both MIC(Minimum Inhibitory Concentrations and MBC(Minimum Bactericidal Concentrations were 0.125㎎/㎖ against N. meningitidis, however MIC and MBC were 1.0㎎/㎖ in antimicrobial action against 12 different genera of bacteria.

Extraction of pesticides in soil using supercritical carbon dioxide co-solvents

International Nuclear Information System (INIS)

Forero, Jose R; Castro, Henry I; Guerrero, Jairo A.

2009-01-01

In this study, three organic solvents (ethyl acetate, methanol and acetone) were used as co solvent in supercritical fluid extraction (SFE) of a mixture of pesticides with different physical and chemical properties present in soil. These pesticides were determined by gas chromatography with electronic micro capture detector μECD and nitrogen-phosphorus detector (NPD), coupled in parallel. The extractions were performed on spiked soil samples using supercritical carbon dioxide (CO 2 SC) as the extracting phase to 35 celsius degrade and 14 MPa, using 10 mL of each co solvent and it was found that methanol offers the greatest efficiency in the extraction process obtaining recovery values between 51.24 and 123.50%.

The Use of a Box-Behnken Design to Optimize the Extraction Technology of Phyllanthus Embica L. Polyphenols and Simultaneous Compositional Analysis using HPLC with Fluorescence Detection

International Nuclear Information System (INIS)

Pan, H.; Zhu, B.; Gong, Y.; He, L.; Wang, M.

2015-01-01

Extractions of polyphenols from Phyllanthus emblica L. were performed by supercritical CO/sub 2/ fluid extraction (SFE). A three-level Box-Behnken factorial design using response surface methodology was applied to optimize the main extraction conditions, including the ratio of the solvent to raw material, pressure, extraction temperature and extraction time on the PEP yields. The results showed that the optimal conditions of the CO/sub 2/ flow rate was 35.9 l/h, pressure was 90.1 MPa, the extraction temperature was 55 degree C and the extraction time was 1.1 h. Under optimum conditions, PEP yields of 84.19±0.51 mg GAE/100 g were obtained, which closely matches the predicted value of the yield. Simultaneous determination of nine polyphenol compounds in polyphenols using HPLC with fluorescence detection has been successfully achieved. HPLC analysis indicated that the major polyphenols in the SFE extracts consisted of chlorogenic acid, caffeic acid, syrigin, procyanidin B2, (-)-epicatechin, cinnamic acid, coumaric acid, phlorizin and quercetin, of which procyanidin B2 had the highest content of 231.77 mg/kg. (author)

Removal of common organic solvents from aqueous waste streams via supercritical C02 extraction: a potential green approach to sustainable waste management in the pharmaceutical industry.

Science.gov (United States)

Leazer, Johnnie L; Gant, Sean; Houck, Anthony; Leonard, William; Welch, Christopher J

2009-03-15

Supercritical CO2 extraction of aqueous streams is a convenient and effective method to remove commonly used solvents of varying polarities from aqueous waste streams. The resulting aqueous layers can potentially be sewered; whereas the organic layer can be recovered for potential reuse. Supercritical fluid extraction (SFE) is a technology that is increasingly being used in commercial processes (1). Supercritical fluids are well suited for extraction of a variety of media, including solids, natural products, and liquid products. Many supercritical fluids have low critical temperatures, allowing for extractions to be done at modestly low temperatures, thus avoiding any potential thermal decomposition of the solutes under study (2). Furthermore, the CO2 solvent strength is easily tuned by adjusting the density of the supercritical fluid (The density is proportional to the pressure of the extraction process). Since many supercritical fluids are gases at ambient temperature, the extract can be concentrated by simply venting the reaction mixture to a cyclone collection vessel, using appropriate safety protocols.

Phase equilibrium of binary system carbon dioxide - methanol at high pressure using artificial neural network

International Nuclear Information System (INIS)

Nasri, F.; Hatami, T.

2012-01-01

Interest in supercritical fluids extraction (SFE ) is increasing throughout many scientific and industrial fields. The common solvent for use in SFE is carbon dioxide. However, pure carbon dioxide frequently fails to efficiently extract the essential oil from a sample matrix, and modifier fluids such as methanol should be used to enhance extraction yield. A more efficient use of SFE requires quantitative prediction of phase equilibrium of this binary system, carbon dioxide - methanol. The purpose of the current research is modeling carbon dioxide - methanol system using artificial neural network (ANN). Results of ANN modeling has been compared with experimental data as well as thermodynamic equations of state. The comparison shows that the ANN modeling has a higher accuracy than thermodynamic models. (author)

Influence of Nonpolar Substances on the Extraction Efficiency of Six Alkaloids in Zoagumhwan Investigated by Ultra Performance Liquid Chromatography and Photodiode Array Detection

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Shijing Liu

2012-11-01

Full Text Available A reverse phase ultra performance liquid chromatography and photodiode array (UPLC-PDA detection method was established for the determination of six alkaloids in Zoagumhwan (ZGW, and further for investigating the influence of nonpolar substances on the extraction efficiency of these alkaloids. The method was based on a BEH C18 (50 mm × 2.1 mm, 1.7 μm column and mobile phase of aqueous phosphoric acid and acetonitrile including 0.05% buffer solution under gradient elution. ZGW samples of ZGW I, II, III and IV were obtained and prepared by pre-processing the crude materials of Coptidis rhizoma and Evodiae fructus using four technologies, namely direct water decoction, removal of nonpolar substances in Evodiae fructus by supercritical fluid extraction (SFE, removal of nonpolar substances in ZGW by SFE and removal of nonpolar substances in ZGW by steam distillation. The developed and validated UPLC-PDA method was precise, accurate and sensitive enough based on the facts that the six alkaloids showed good regression (r > 0.9998, the limit of detections and quantifications for six alkaloids were less than 28.8 and 94.5 ng/mL, respectively, and the recovery was in the range of 98.56%–103.24%. The sequence of the total contents of six alkaloids in these samples was ZGW II > ZGW IV > ZGW III > ZGW I. ZGW II, in which nonpolar substances, including essential oils, were firstly removed from Evodiae fructus by SFE, had the highest content of the total alkaloids, indicating that extraction efficiency of the total alkaloids could be remarkably increased after Evodiae fructus being extracted by SFE.

Theoretical models for supercritical fluid extraction.

Science.gov (United States)

Huang, Zhen; Shi, Xiao-Han; Jiang, Wei-Juan

2012-08-10

For the proper design of supercritical fluid extraction processes, it is essential to have a sound knowledge of the mass transfer mechanism of the extraction process and the appropriate mathematical representation. In this paper, the advances and applications of kinetic models for describing supercritical fluid extraction from various solid matrices have been presented. The theoretical models overviewed here include the hot ball diffusion, broken and intact cell, shrinking core and some relatively simple models. Mathematical representations of these models have been in detail interpreted as well as their assumptions, parameter identifications and application examples. Extraction process of the analyte solute from the solid matrix by means of supercritical fluid includes the dissolution of the analyte from the solid, the analyte diffusion in the matrix and its transport to the bulk supercritical fluid. Mechanisms involved in a mass transfer model are discussed in terms of external mass transfer resistance, internal mass transfer resistance, solute-solid interactions and axial dispersion. The correlations of the external mass transfer coefficient and axial dispersion coefficient with certain dimensionless numbers are also discussed. Among these models, the broken and intact cell model seems to be the most relevant mathematical model as it is able to provide realistic description of the plant material structure for better understanding the mass-transfer kinetics and thus it has been widely employed for modeling supercritical fluid extraction of natural matters. Copyright © 2012 Elsevier B.V. All rights reserved.

Extraction fatty acid as a source to produce biofuel in microalgae Chlorella sp. and Spirulina sp. using supercritical carbon dioxide

Science.gov (United States)

Tai, Do Chiem; Hai, Dam Thi Thanh; Vinh, Nguyen Hanh; Phung, Le Thi Kim

2016-06-01

In this research, the fatty acids of isolated microalgae were extracted by some technologies such as maceration, Soxhlet, ultrasonic-assisted extraction and supercritical fluid extraction; and analyzed for biodiesel production using GC-MS. This work deals with the extraction of microalgae oil from dry biomass by using supercritical fluid extraction method. A complete study at laboratory of the influence of some parameters on the extraction kinetics and yields and on the composition of the oil in terms of lipid classes and profiles is proposed. Two types of microalgae were studied: Chlorella sp. and Spirulina sp. For the extraction of oil from microalgae, supercritical CO2 (SC-CO2) is regarded with interest, being safer than n-hexane and offering a negligible environmental impact, a short extraction time and a high-quality final product. Whilst some experimental papers are available on the supercritical fluid extraction (SFE) of oil from microalgae, only limited information exists on the kinetics of the process. These results demonstrate that supercritical CO2 extraction is an efficient method for the complete recovery of the neutral lipid phase.

Quantification of active principles and pigments in leaf extracts of Isatis tinctoria by HPLC/UV/MS.

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Mohn, Tobias; Potterat, Olivier; Hamburger, Matthias

2007-02-01

An HPLC method has been developed and validated for the quantification of the pharmacologically active principles tryptanthrin (1), 1,3-dihydro-3-[(4-hydroxy-3,5-dimethoxyphenyl)methylene]-2 H-indol-2-one (indolinone) (3), indirubin (4), alpha-linolenic acid (2), and indigo (5), an isomer of indirubin, in extracts from the traditional anti-inflammatory plant Isatis tinctoria (woad). The chromatographic separation was performed on a C-18 column with a linear gradient of acetonitrile in water containing 0.1% formic acid. The method combines UV and electrospray MS detection in the positive ion mode for the detection of the alkaloids, with a switch to the negative mode for the analysis of alpha-linolenic acid. The method was applied to the analysis of woad extracts obtained by supercritical fluid (SFE) CO2 extraction, and by pressurized liquid extraction (PLE) with dichloromethane and methanol, respectively. While the highest concentration of alpha-linolenic acid was found in the SFE extract (7.43%), the concentrations of tryptanthrin , indolinone, indirubin and indigo were the highest in the dichloromethane extract (0.30, 0.035, 2.48 and 0.84%, respectively). Compound 3 was not detected in the methanolic extract and only traces of compounds 1, 4 and 5 and low amount of alpha-linolenic acid (0.39%) were present in this extract.

Pesticide Residues in Canned Foods, Fruits, and Vegetables: The Application of Supercritical Fluid Extraction and Chromatographic Techniques in the Analysis

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Mohamed H. EL-Saeid

2003-01-01

Full Text Available Multiple pesticide residues have been observed in some samples of canned foods, frozen vegetables, and fruit jam, which put the health of the consumers at risk of adverse effects. It is quite apparent that such a state of affairs calls for the need of more accurate, cost-effective, and rapid analytical techniques capable of detecting the minimum concentrations of the multiple pesticide residues. The aims of this paper were first, to determine the effectiveness of the use of Supercritical Fluid Extraction (SFE and Supercritical Fluid Chromatography (SFC techniques in the analysis of the levels of pesticide residues in canned foods, vegetables, and fruits; and second, to contribute to the promotion of consumer safety by excluding pesticide residue contamination from markets. Fifteen different types of imported canned and frozen fruits and vegetables samples obtained from the Houston local food markets were investigated. The major types of pesticides tested were pyrethroids, herbicides, fungicides, and carbamates.By using these techniques, the overall data showed 60.82% of the food samples had no detection of any pesticide residues under this investigation. On the other hand, 39.15% different food samples were contaminated by four different pyrethroid residues ± RSD% ranging from 0.03 ± 0.005 to 0.05 ± 0.03 ppm, of which most of the pyrethroid residues were detected in frozen vegetables and strawberry jam. Herbicide residues in test samples ranged from 0.03 ± 0.005 to 0.8 ± 0.01 ppm. Five different fungicides, ranging from 0.05 ± 0.02 to 0.8 ±0.1 ppm, were found in five different frozen vegetable samples. Carbamate residues were not detected in 60% of investigated food samples. It was concluded that SFE and SFC techniques were accurate, reliable, less time consuming, and cost effective in the analysis of imported canned foods, fruits, and vegetables and are recommended for the monitoring of pesticide contaminations.

Development of an analysis method for determining chlorinated hydrocarbons in marine sediments and suspended matter giving particular consideration to supercritical fluid extraction; Entwicklung eines Analysenverfahrens zur Bestimmung von chlorierten Kohlenwasserstoffen in marinen Sedimenten und Schwebstoffen unter besonderer Beruecksichtigung der ueberkritischen Fluidextraktion

Energy Technology Data Exchange (ETDEWEB)

Sterzenbach, D.

1997-11-01

The purpose of the present study was to develop an analysis method for chlorinate hydrocarbons in marine environments using supercritical fluid extraction (SFE) instead of conventional approaches. In order to apply this extraction method the available SFE device had to be extended and all the individual steps of the analysis method had to be optimised and adapted. As chlorinated hydrocarbons only occur at very low concentrations in marine environments (ppm to ppt range) the analysis method had to be extremely sensitive. High sensitivity, in town, is generally associated with a high susceptibility of an analysis method to faults through contamination or losses. This meant that the entire method and all its individual steps had to scrutinised for such weak points and improved where necessary. A method for sampling suspended matter in marine environments had to be developed which permits efficient separation of the smallest possible particles from seawater. The designated purpose of the developed analysis method is to deal with topical aspects of marine chemistry relating to sources, transport, distribution, and the fate of chlorinated hydrocarbons in marine environments. (orig.) [Deutsch] Ziel der vorliegenden Arbeit ist, ein Analysenverfahren fuer chlorierte Kohlenwasserstoffe in der marinen Umwelt zu entwickeln. Dabei soll die ueberkritische Fluidextraktion (SFE) anstelle herkoemmlicher Verfahren eingesetzt werden. Fuer die Anwendung dieser Extraktionsmethode ist es erforderlich, das zur Verfuegung stehende SFE-Geraet zu erweitern und saemtliche Teilschritte des Analysenverfahrens zu optimieren und auf diese Methode abzustimmen. Der Umstand, dass die chlorierten Kohlenwasserstoffe nur in sehr geringen Konzentrationen in der marinen Umwelt vorkommen (ppm- bis ppt-Bereich), erfordert eine sehr hohe Empfindlichkeit des Analysenverfahrens. Eine hohe Empfindlichkeit bedingt eine grosse Stoeranfaelligkeit des Analysenverfahrens durch Kontaminationen oder Verluste. Aus

Optimization and evaluation of wheat germ oil extracted by supercritical CO2

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Niu, LiYa

2011-06-01

Full Text Available Box-Behnken design combined with response surface methodology (RSM was used to optimize the parameters of supercritical CO2 extraction (SFE of wheat germ oil. The quality of the oil and residual meal obtained by SFE and solvent extraction (SE were evaluated from proximate analysis, fatty acid composition and antioxidant activity. A maximum oil yield of 10.46% was achieved under the optimal conditions of wheat germ particle size 60-80 mesh; water content 4.37%; pressure 30MPa; temperature 40°C extraction time 1.7h. The oil obtained by SFE showed stronger DPPH radical scavenging ability than SE oil at the same concentration. The fatty acid composition of SFE oil was similar to SE oil. Higher contents of protein (34.3% and lysine (2.47g/100g were found in the residual meal obtained by SFE. The results show that oil and defatted meal obtained by SFE can be promising nutritional sources for food.Un diseño Box-Behnken combinado con metodología de superficie de respuesta (RSM fue usado para optimizar los parámetros de extracción con fluido supercrítico (SFE del aceite de germen de trigo. La calidad del aceite y de la harina residual obtenida por SFE y por extracción con solvente (SE fue evaluada mediante su análisis porcentual, composición de ácidos grasos y actividad antioxidante. Un máximo rendimiento de aceite del 10.46% fue obtenido con las condiciones óptimas de 60-80 mesh de tamaño de partícula del germen de trigo; 4.37% contenido de agua; 30MPa de presión; 40°C de temperatura y 1.7 h de tiempo de extracción. El aceite obtenido por SFE mostró una capacidad atrapadora de radicales libres mucho mayor que el aceite obtenido por SE a la misma concentración. La composición de ácidos grasos del aceite SFE fue similar al aceite SE. El mayor contenido de proteínas (34% y de lisina (2.47g/100g fue encontrado en las harinas residuales obtenidas por SFE. Los resultados muestran que el aceite y la harina desengrasada obtenidas por SFE

Environmental application of millimeter-scale sponge iron (s-Fe(0)) particles (II): the effect of surface copper.

Science.gov (United States)

Ju, Yongming; Liu, Xiaowen; Liu, Runlong; Li, Guohua; Wang, Xiaoyan; Yang, Yanyan; Wei, Dongyang; Fang, Jiande; Dionysiou, Dionysios D

2015-04-28

To enhance the catalytic reactivity of millimeter-scale particles of sponge iron (s-Fe(0)), Cu(2+) ions were deposited on the surface of s-Fe(0) using a simple direct reduction reaction, and the catalytic properties of the bimetallic system was tested for removal of rhodamine B (RhB) from an aqueous solution. The influence of Cu(0) loading, catalyst dosage, particle size, initial RhB concentration, and initial pH were investigated, and the recyclability of the catalyst was also assessed. The results demonstrate that the 3∼5 millimeter s-Fe(0) particles (s-Fe(0)(3∼5mm)) with 5wt% Cu loading gave the best results. The removal of RhB followed two-step, pseudo-first-order reaction kinetics. Cu(0)-s-Fe(0) showed excellent stability after five reuse cycles. Cu(0)-s-Fe(0) possesses great advantages compared to nanoscale zero-valent iron, iron power, and iron flakes as well as its bimetals. The surface Cu(0) apparently catalyzes the production of reactive hydrogen atoms for indirect reaction and generates Fe-Cu galvanic cells that enhance electron transfer for direct reaction. This bimetallic catalyst shows great potential for the pre-treatment of recalcitrant wastewaters. Additionally, some oxides containing iron element are selected to simulate the adsorption process. The results prove that the adsorption process of FeOOH, Fe2O3 and Fe3O4 played minor role for the removal of RhB. Copyright © 2015 Elsevier B.V. All rights reserved.

Investigation of cultivated lavender (Lavandula officinalis L. extraction and its extracts

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Nađalin Vesna

2014-01-01

Full Text Available In this study essential oil content was determined in lavender flowers and leaves by hydrodistillation. Physical and chemical characteristics of the isolated oils were determined. By using CO2 in supercritical state the extraction of lavender flowers was performed with a selected solvent flow under isothermal and isobaric conditions. By the usage of gas chromatography in combination with mass spectrometry (GC/MS and gas chromatography with flame ionisation detector (GC/FID the qualitative and quantitative analysis of the obtained essential oil and supercritical extracts (SFE was carried out. Also, the analysis of individual SFE extracts obtained during different extraction times was performed. It turned out that the main components of the analysed samples were linalool, linalool acetate, lavandulol, caryophyllene oxide, lavandulyl acetate, terpinen-4-ol and others. Two proposed models were used for modelling the extraction system lavender flower - supercritical CO2 on the basis of experimental results obtained by examining the extraction kinetics of this system. The applied models fitted well with the experimental results.

Clinical Outcome And Arginine Serum of Acute Ischemic Stroke Patients Supplemented by Snakehead Fish Extract

Science.gov (United States)

Pudjonarko, Dwi; Retnaningsih; Abidin, Zainal

2018-02-01

Background: Levels of arginine associated with clinical outcome in acute ischemic stroke (AIS). Arginine is a protein needed to synthesis nitric oxide (NO), a potential vasodilator and antioxidant. Snakehead fish is a source of protein which has antioxidant activity. Snakehead fish contains mineral, vitamin, and amino acids. One of the amino acids that were found quite high in snakehead fish extract is arginine. The aim of this study was done to determine the effect of snakehead fish extracts (SFE) on serum arginin levels and clinical outcome of AIS patients. Methods: It was double-blind randomized pretest-posttest control group design, with. AIS patients were divided into two groups i.e. snakehead fish extracts (SFE) and control. SFE group were administered 15 grams SFE for 7 days . Arginine serum levels and clinical outcome (measured by National Institute of Health Stroke Scale = NIHSS) were measured before and after treatment, other related factors were also analyzed in Logistic regression. Results: A total of 42 subjects who were performed random allocation as SFE or control group. There was no differences in subject characteristics between the two groups. There was a differences Δ arginine serum levels between SFE and control (33.6±19.95 μmol/L 0.3±2.51 μmol/L pgender factor that affected on improvement of NIHSS (OR=7; p=0,01). Conclusion: There is Clinical outcome improvement and enhancement of arginine serum levels in AIS patient with snakehead fish extract supplementation.

Influence of different extraction methods on the yield and linalool content of the extracts of Eugenia uniflora L.

Science.gov (United States)

Galhiane, Mário S; Rissato, Sandra R; Chierice, Gilberto O; Almeida, Marcos V; Silva, Letícia C

2006-09-15

This work has been developed using a sylvestral fruit tree, native to the Brazilian forest, the Eugenia uniflora L., one of the Mirtaceae family. The main goal of the analytical study was focused on extraction methods themselves. The method development pointed to the Clevenger extraction as the best yield in relation to SFE and Soxhlet. The SFE method presented a good yield but showed a big amount of components in the final extract, demonstrating low selectivity. The essential oil extracted was analyzed by GC/FID showing a large range of polarity and boiling point compounds, where linalool, a widely used compound, was identified. Furthermore, an analytical solid phase extraction method was used to clean it up and obtain separated classes of compounds that were fractionated and studied by GC/FID and GC/MS.

Supercritical carbon dioxide hop extraction

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Pfaf-Šovljanski Ivana I.

2005-01-01

Full Text Available The hop of Magnum cultivar was extracted using supercritical carbon dioxide (SFE-as extractant. Extraction was carried out in the two steps: the first one being carried out at 150 bar and 40°C for 2.5 h (Extract A, and the second was the extraction of the same hop sample at 300 bar and 40°C for 2.5 h (Extract B. Extraction kinetics of the system hop-SFE-CO2 was investigated. Two of four most common compounds of hop aroma (α-humulene and β-caryophyllene were detected in Extract A. Isomerised α-acids and β-acids were detected too. a-Acid content in Extract B was high (that means it is a bitter variety of hop. Mathematical modeling using empirical model characteristic time model and simple single sphere model has been performed on Magnum cultivar extraction experimental results. Characteristic time model equations, best fitted experimental results. Empirical model equation, fitted results well, while simple single sphere model equation poorly approximated the results.

Memory-enhancing effect of a supercritical carbon dioxide fluid extract of the needles of Abies koreana on scopolamine-induced amnesia in mice.

Science.gov (United States)

Kim, Kanghyun; Bu, Youngmin; Jeong, Seungil; Lim, Jongpil; Kwon, Youngan; Cha, Dong Seok; Kim, Jinmo; Jeon, Sora; Eun, Jaesoon; Jeon, Hoon

2006-08-01

Abies koreana Wilson (A. koreana) is a shrub or broadly pyramidal evergreen tree endemic in the mountainous regions of South Korea. We obtained the essential oil (EO) from alpine needle leaves of A. koreana by the supercritical fluid extraction (SFE) method. EO was analyzed by gas chromatography-mass spectrometry (GC-MS), and 68 compounds were identified constituting 95.66% of the oil. The major components were elemol (11.17%), terpinen-4-ol (9.77%), sabinene (8.86%), 10(15)-cadien-4-ol (7.16%), alpha-terpineol (6.13%), alpha-pinene (6.07%) and gamma-terpinene (4.71%). To investigate the memory-enhancing effects, we conducted a passive avoidance test using a scopolamine (1 mg/kg, ip)-induced amnesia mouse model. A peritoneal injection of EO from A. koreana (100 mg/kg) showed a memory enhancing effect of 72.7% compared with the control. These results suggest that EO of A. koreana may be a useful therapeutic agent against such amnesia-inducing diseases as Alzheimer and vascular dementia.

Microwave-Assisted Extraction of Cannabinoids in Hemp Nut Using Response Surface Methodology: Optimization and Comparative Study

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Chih-Wei Chang

2017-11-01

Full Text Available Hemp nut is commonly incorporated into several food preparations; however, most countries set regulations for hemp products according to their cannabinoid content. In this study, we have developed an efficient microwave-assisted extraction (MAE method for cannabinoids (i.e., Δ9-tetrahydrocannabinol, cannabidiol, and cannabinol in hemp nut. Optimization of the MAE procedure was conducted through single factor experiments and response surface methodology (RSM. A comparative study was also conducted to determine the differences in the extraction yields and morphology of hemp nut between MAE and reference extraction methods, namely heat reflux extraction (HRE, Soxhlet extraction (SE, supercritical fluid extraction (SFE, and ultrasound-assisted extraction (UAE. Among the independent variables in RSM, the temperature was the most significant parameter. The optimal conditions of MAE were as follows: extraction solvent of methanol, microwave power of 375 W, temperature of 109 °C, and extraction time of 30 min. Compared with reference extraction methods, MAE achieved the highest extraction yields of total cannabinoids in hemp nut (6.09 μg/g for MAE; 4.15 μg/g for HRE; 5.81 μg/g for SE; 3.61 μg/g for SFE; 3.73 μg/g for UAE with the least solvent consumption and shortest time. Morphological observations showed that substantial cell rupturing occurred in the microstructure of hemp nut after MAE, indicating enhanced dissolution of the target compounds during the extraction process. The MAE method is thus a rapid, economic, and environmentally friendly extraction method that is both effective and practical for industrial applications.

EVALUATION OF ANALYTICAL METHODS FOR DETERMINING PESTICIDES IN BABY FOOD

Science.gov (United States)

Three extraction methods and two detection techniques for determining pesticides in baby food were evaluated. The extraction techniques examined were supercritical fluid extraction (SFE), enhanced solvent extraction (ESE), and solid phase extraction (SPE). The detection techni...

Comparison of chemical composition and antibacterial activity of Nigella sativa seed essential oils obtained by different extraction methods.

Science.gov (United States)

Kokoska, L; Havlik, J; Valterova, I; Sovova, H; Sajfrtova, M; Jankovska, I

2008-12-01

Nigella sativa L. seed essential oils obtained by hydrodistillation (HD), dry steam distillation (SD), steam distillation of crude oils obtained by solvent extraction (SE-SD), and supercritical fluid extraction (SFE-SD) were tested for their antibacterial activities, using the broth microdilution method and subsequently analyzed by gas chromatography and gas chromatography-mass spectrometry. The results showed that the essential oils tested differed markedly in their chemical compositions and antimicrobial activities. The oils obtained by HD and SD were dominated by p-cymene, whereas the major constituent identified in both volatile fractions obtained by SD of extracted oils was thymoquinone (ranging between 0.36 and 0.38 g/ml, whereas in oils obtained by HD and SD, it constituted only 0.03 and 0.05 g/ml, respectively). Both oils distilled directly from seeds showed lower antimicrobial activity (MICs > or = 256 and 32 microg/ml for HD and SD, respectively) than those obtained by SE-SD and SFE-SD (MICs > or = 4 microg/ml). All oil samples were significantly more active against gram-positive than against gram-negative bacteria. Thymoquinone exhibited potent growth-inhibiting activity against gram-positive bacteria, with MICs ranging from 8 to 64 microg/ml.

Supercritical Fluid Extraction ; its application to the extraction of anabolic steroids from biological matrices

NARCIS (Netherlands)

Stolker AAM; ARO

1995-01-01

Het gebruik van superkritische vloeistof extractie (SFE) als alternatief voor de conventionle, op organische oplosmiddelen gebaseerde, extractie technieken begint langzamerhand steeds belangrijker te worden. Het probleem van het gebruik van superkritsche vloeistoffen voor de extractie van

High-performance separation and supercritical extraction of lanthanides and actinides

International Nuclear Information System (INIS)

Datta, Arpita; Sujatha, K.; Kumar, R.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R.

2010-01-01

Extensive studies were carried out at Chemistry Group, IGCAR for the rapid separation of individual lanthanides and actinides using dynamic ion-exchange chromatographic technique. The atom percent fission was determined from the concentrations of the lanthanide fission products, uranium and plutonium contents of dissolver solution. These advantages were exploited to significantly reduce analysis time, liquid waste generation as well as dose to operator. Supercritical fluid extraction (SFE) of actinides from waste matrices was studied in detail at our laboratory using modified supercritical carbon dioxide (Sc-CO 2 ). Complete extraction and recovery of uranium, plutonium and americium from various matrices was achieved using Sc-CO 2 modified with suitable ligands. The technique was demonstrated for the recovery of plutonium from actual waste received from different laboratories. (author)

Antioxidant Activity of Mulberry Fruit Extracts

Science.gov (United States)

Arfan, Muhammad; Khan, Rasool; Rybarczyk, Anna; Amarowicz, Ryszard

2012-01-01

Phenolic compounds were extracted from the fruits of Morus nigra and Morus alba using methanol and acetone. The sugar-free extracts (SFEs) were prepared using Amberlite XAD-16 column chromatography. All of the SFEs exhibited antioxidant potential as determined by ABTS (0.75–1.25 mmol Trolox/g), DPPH (2,2-diphenyl-1-picrylhydrazyl) (EC50 from 48 μg/mL to 79 μg/mL), and reducing power assays. However, a stronger activity was noted for the SFEs obtained from Morus nigra fruits. These extracts also possessed the highest contents of total phenolics: 164 mg/g (methanolic SFE) and 173 mg/g (acetonic SFE). The presence of phenolic acids and flavonoids in the extracts was confirmed using HPLC method and chlorogenic acid and rutin were found as the dominant phenolic constituents in the SFEs. PMID:22408465

Antioxidant Activity of Mulberry Fruit Extracts

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Ryszard Amarowicz

2012-02-01

Full Text Available Phenolic compounds were extracted from the fruits of Morus nigra and Morus alba using methanol and acetone. The sugar-free extracts (SFEs were prepared using Amberlite XAD-16 column chromatography. All of the SFEs exhibited antioxidant potential as determined by ABTS (0.75–1.25 mmol Trolox/g, DPPH (2,2-diphenyl-1-picrylhydrazyl (EC50 from 48 μg/mL to 79 μg/mL, and reducing power assays. However, a stronger activity was noted for the SFEs obtained from Morus nigra fruits. These extracts also possessed the highest contents of total phenolics: 164 mg/g (methanolic SFE and 173 mg/g (acetonic SFE. The presence of phenolic acids and flavonoids in the extracts was confirmed using HPLC method and chlorogenic acid and rutin were found as the dominant phenolic constituents in the SFEs.

Composition of the volatile compounds from Aniba canelilla (H. B. K. Mez. extracted by CO2 in the supercritical state

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Janete H. Y. Vilegas

Full Text Available The volatile compounds obtained by SFE-CO2 (supercritical fluid extraction utilizing CO2 from the barks of Aniba canelilla (H. B. K. Mez. (Lauraceae were analyzed by HRGC-FID (high resolution gas chromatography - flame ionization detector and HRGC-MS (high resolution gas chromatography -mass spectrometry. Phenylpropanoids and lower amounts of sesquiterpenoids, representing ca. 97% of the total oil, were identified. The main compound, 2-phenylnitroethane, corresponds to 71,12% of the total oil.

Instrument for Analysis of Organic Compounds on Other Planets

Science.gov (United States)

Daulton, Riley M.; Hintze, Paul E.

2016-01-01

The goal of this project is to develop the Instrument for Solvent Extraction and Analysis of Extraterrestrial Bodies using In Situ Resources (ISEE). Specifically, ISEE will extract and characterize organic compounds from regolith which is found on the surface of other planets or asteroids. The techniques this instrument will use are supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC). ISEE aligns with NASA's goal to expand the frontiers of knowledge, capability, and opportunities in space in addition to supporting NASA's aim to search for life elsewhere by characterizing organic compounds. The outcome of this project will be conceptual designs of 2 components of the ISEE instrument as well as the completion of proof-of-concept extraction experiments to demonstrate the capabilities of SFE. The first conceptual design is a pressure vessel to be used for the extraction of the organic compounds from the regolith. This includes a comparison of different materials, geometry's, and a proposition of how to insert the regolith into the vessel. The second conceptual design identifies commercially available fluid pumps based on the requirements needed to generate supercritical CO2. The proof-of-concept extraction results show the percent mass lost during standard solvent extractions of regolith with organic compounds. This data will be compared to SFE results to demonstrate the capabilities of ISEE's approach.

Comparative gas chromatography-mass spectroscopy, Fourier transform infrared spectroscopy, and high-performance liquid chromatography analysis of essential oils extracted using 4 methods from the leaves of Eucalyptus globulus L.

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Yasmeen Khan

2016-01-01

Full Text Available Background: Eucalyptus globulus L. (family, Myrtaceae is one of the world′s most widely planted genera. E. globulus L., commonly referred to as Tasmanian blue gum, is a fast growing, evergreen tree, native to Tasmania and South-East Australia. Apart from its extensive use in pulp industry, it is also produces Oleum Eucalypti (eucalyptus oil that is extracted on commercial scale in many countries such as China, India, South Africa, Portugal, Brazil, and Tasmania, as a raw material in perfumery, cosmetics, food beverage, aromatherapy, and phytotherapy. Materials and Methods: Traditional hydrodistillation (HD, solvent extraction (SE, ultrasonication (US, and supercritical fluid extraction (SFE were conducted for the extraction of essential oil from the leaves of E. globulus. Each oil was evaluated in terms of high-performance liquid chromatography (HPTLC and Fourier transform infrared spectroscopy (FTIR fingerprinting with qualitative and semi-quantitative composition of the isolated essential oil by gas chromatography-mass spectroscopy (GCMS, the extract yield of essential oil was 2.60%, 2.2%, 2.0%, and 3.6% v/w, respectively, for HD, SE, US, and SFE. Results: A total of 53 compounds were identified by GCMS. Comparative analysis indicated that SFE was favorable for extraction of monoterpene hydrocarbon, sesquiterpene hydrocarbon, and oxygenated sesquiterpene hydrocarbon. HD, SE, and US had certain advantages in the extraction of aliphatic saturated hydrocarbons organic acid and esters. Overlay, FTIR spectra of oil samples obtained by four extraction methods were superimposed with each other showing similar components. The maximum separation of compound seen at 254 nm and lesser at 366 nm by HPTLC fingerprinting which again showed superimposed chromatograms. Conclusion: It is concluded that different extraction method may lead to different yields of essential oils where the choice of appropriate method is very important to obtained more desired

Methods for extraction and determination of phenolic acids in medicinal plants: a review.

Science.gov (United States)

Arceusz, Agnieszka; Wesolowski, Marek; Konieczynski, Pawel

2013-12-01

Phenolic acids constitute a group of potentially immunostimulating compounds. They occur in all medicinal plants and are widely used in phytotherapy and foods of plant origin. In recent years, phenolic acids have attracted much interest owing to their biological functions. This paper reviews the extraction and determination methods of phenolic acids in medicinal plants over the last 10 years. Although Soxhlet extraction and ultrasonic assisted extraction (UAE) are commonly used for the extraction of phenolic acids from plant materials, alternative techniques such as supercritical fluid extraction (SFE), and accelerated solvent extraction (ASE) can also be used. After extraction, phenolic acids are determined usually by liquid chromatography (LC) owing to the recent developments in this technique, especially when it is coupled with mass spectrometry (MS). Also detection systems are discussed, including UV-Vis, diode array, electrochemical and fluorimetric. Other popular techniques for the analysis of this group of secondary metabolites are gas chromatography coupled with mass spectrometry (GC-MS) and capillary electrophoresis (CE).

Comparison of the Chemical Composition of “Cystoseira sedoides (Desfontaines C. Agardh” Volatile Compounds Obtained by Different Extraction Techniques

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Naima Bouzidi

2016-01-01

Full Text Available The volatile fraction of the brown alga Cystoseira sedoides (Desfontaines C.Agardh is prepared from the crude extract through the following three extraction methods: Hydrodistillation (HD, focused microwave assisted hydrodistillation (FMAHD and supercritical fluid extraction (SFE. The volatile fractions are analyzed by gas chromatography-flame ionization detector-mass spectrometry (GC-FID-MS, the chemical components are identified on the basis of the comparison of their retention indices with literature and their mass spectra with those reported in commercial databases. The chemical composition of the volatile fractions obtained by different extraction techniques fall into three major chemical classes: fatty acids and derivatives, sesquiterpenes, and hydrocarbons and derivatives. Others Compounds belonging to different chemical classes are found in that chemical composition.

Environmental management technology demonstration and commercialization. Semi-annual progress report, April 1, 1995--October 31, 1995

Energy Technology Data Exchange (ETDEWEB)

NONE

1995-11-01

Several field-portable (e.g., gas chromatrography (GC), gas chromatography-mass spectrometry (GC-MS)) instruments are available for the measurement of organic pollutants. However, solid samples such as soils, sludges, and sediments must first be extracted before analysis can be performed. Conventional extraction methods based on liquid solvent (e.g., Soxhlet extraction) are not practical in the field because of the large volumes fo solvents required as well as clumsy apparatus and glassware. However, supercritical fluid extraction (SFE) has been demonstrated in several studies by the Energy & Environmental Research Center (EERS) to extract a broad range of organic pollutants from soils and sediments successfully. Of the approximately 100 major organic pollutants identified as problems for the US Department of Energy (DOE) sites, our SFE laboratory has demonstrated efficient SFE recoveries for about half, and published literature has addressed an additional 40%. SFE in the off-line mode (i.e., collection of extracted organics in a small voluem of liquid solvent) has also been demonstrated to be easily performed in the field with only generator electrical power for support. Recent advances in flow restrictor design have virtually eliminated the mechanical problems previously associated with the performance of SFE in the field.

Wheat germ oil extracted by supercritical carbon dioxide with ethanol: Fatty acid composition; Aceite de germen de trigo obtenido mediante extracción con dióxido de carbono supercrítico con etanol: Composición en ácidos grasos

Energy Technology Data Exchange (ETDEWEB)

Parczewska-Plesnar, B.; Brzozowski, R.; Gwardiak, H.; Białecka-Florjańczyk, E.; Bujnowski, Z.

2016-07-01

In this work, supercritical fluid extraction (SFE) using CO2 with ethanol as entrainer was performed at a temperature of 40 o C under a pressure of 21 MPa. For comparison, a similar extraction without the entrainer was carried out. The extraction yield of wheat germ using supercritical CO2 with ethanol was slightly higher (10.7 wt%) than that of extraction without the entrainer (9.9 wt%). Fractions of SFE extracts were collected separately during the experiments and the composition of fatty acids in each fraction was analyzed. The SFE extracted oils were rich (63.4-71.3%) in the most valuable polyunsaturated fatty acids (PUFA) and their content in all collected fractions was approximately constant. Similar PUFA contents were found in the reference samples of oils extracted by n-hexane (66.2-67.0%), while the commercial cold-pressed oil contained significantly less PUFA (60.2%). These results show a higher nutritional value of the oil obtained by extraction with supercritical CO2 than cold pressed oil which is generally considered to be very valuable. [Spanish] En este trabajo, la extracción con fluidos supercríticos (SFE) usando CO2 con etanol como agente de arrastre se realizó a 40 °C bajo una presión de 21 MPa. Se ha llevado a cabo la comparación con una extracción similar sin agente de arrastre. El rendimiento de la extracción de germen de trigo usando CO2 supercrítico con etanol fue ligeramente mayor (10,7% en peso) que la de extracción sin agente de arrastre (9,9% en peso). Se recogieron por separado fracciones de extractos SFE durante los experimentos y se analizó la composición de ácidos grasos en cada fracció . Los aceites extraídos mediante SFE eran ricos en los ácidos grasos poliinsaturados más valiosos (63,4-71,3%), (PUFA) y su contenido en todas las fracciones recogidas fue aproximadamente constante. Un contenido similar de PUFA fueron encontrados en muestras de referencia de los aceites extraídos con n-hexano (66,2-67,0%), mientras

Green Extraction of Antioxidants from Different Varieties of Red Grape Pomace

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María José Otero-Pareja

2015-05-01

Full Text Available The extraction yield, phenolic content, anthocyanin content and antioxidant activity of extracts from different varieties of red grapes, Cabernet Sauvignon, Merlot, Petit Verdot, Syrah, Tempranillo and Tintilla, using pressurized green solvents have been analyzed. Two techniques were studied and compared: supercritical fluid extraction (SFE with CO2 + 20% ethanol and pressurized liquid extraction (PLE with either ethanol, water or an ethanol/water mixture as the extraction solvents. The Petit Verdot variety allowed the highest global and phenolic yield, and antioxidant activity. The best conditios for PLE obtained from the experimental design and kinetic study were 50% ethanol/water as the pressurized solvent at 90 bar, 120 °C, a flow rate of 5 g/min and, an extraction time of 90 min. A statistical analysis of variance has been performed and it was found that temperature is the only variable that has a statistical influence on the extraction yield. The antioxidant activity levels of the extracts are very promising and they are similar to those obtained with the antioxidant tocopherol.

Green extraction of antioxidants from different varieties of red grape pomace.

Science.gov (United States)

Otero-Pareja, María José; Casas, Lourdes; Fernández-Ponce, María Teresa; Mantell, Casimiro; Martínez de la Ossa, Enrique J

2015-05-26

The extraction yield, phenolic content, anthocyanin content and antioxidant activity of extracts from different varieties of red grapes, Cabernet Sauvignon, Merlot, Petit Verdot, Syrah, Tempranillo and Tintilla, using pressurized green solvents have been analyzed. Two techniques were studied and compared: supercritical fluid extraction (SFE) with CO2 + 20% ethanol and pressurized liquid extraction (PLE) with either ethanol, water or an ethanol/water mixture as the extraction solvents. The Petit Verdot variety allowed the highest global and phenolic yield, and antioxidant activity. The best conditios for PLE obtained from the experimental design and kinetic study were 50% ethanol/water as the pressurized solvent at 90 bar, 120 °C, a flow rate of 5 g/min and, an extraction time of 90 min. A statistical analysis of variance has been performed and it was found that temperature is the only variable that has a statistical influence on the extraction yield. The antioxidant activity levels of the extracts are very promising and they are similar to those obtained with the antioxidant tocopherol.

Design and construction of an on-line SPE-SFE-CGC system

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Pinto Jair S. S.

2001-01-01

Full Text Available The construction of an on-line SPE-SFE-CGC system is described. The home-made system is of low cost and of easy construction and maintenance, making possible the analysis of organic micropollutants in liquid samples such as water in a fraction of the time spent using traditional methods.

Treatment of oil-contaminated drill cuttings using supercritical carbon dioxide (SC CO2)

International Nuclear Information System (INIS)

Odusanya, O.O.; Guigard, S.E.

2002-01-01

New treatment technologies are currently being investigated for the treatment of oil-contaminated drill cuttings generated during drilling for oil and gas. Supercritical Fluid Extraction (SFE) is a promising technology that could effectively treat these contaminated drill cuttings. The objectives of this work were therefore to investigate the application of SFE to oil-contaminated drill cuttings treatment and to determine the optimal extraction conditions to remove the oil from these cuttings. Preliminary extractions indicate that SFE with carbon dioxide (CO 2 ) can effectively remove oil from oil-contaminated drill cuttings. Extraction efficiencies calculated based on Total Petroleum Hydrocarbon (TPH) content were greater than 76% for the cuttings and extraction conditions tested in this work. The preliminary results indicate a trend of increasing extraction efficiencies with increasing temperature and pressure although more data is required to confirm this trend. Additional work will focus on performing additional extractions to determine the optimum extraction conditions. (author)

Obtaining bixin from semi-defatted annatto seeds by a mechanical method and solvent extraction: Process integration and economic evaluation.

Science.gov (United States)

Alcázar-Alay, Sylvia C; Osorio-Tobón, J Felipe; Forster-Carneiro, Tânia; Meireles, M Angela A

2017-09-01

This work involves the application of physical separation methods to concentrate the pigment of semi-defatted annatto seeds, a noble vegetal biomass rich in bixin pigments. Semi-defatted annatto seeds are the residue produced after the extraction of the lipid fraction from annatto seeds using supercritical fluid extraction (SFE). Semi-defatted annatto seeds are use in this work due to three important reasons: i) previous lipid extraction is necessary to recovery the tocotrienol-rich oil present in the annatto seeds, ii) an initial removal of the oil via SFE process favors bixin separation and iii) the cost of raw material is null. Physical methods including i) the mechanical fractionation method and ii) an integrated process of mechanical fractionation method and low-pressure solvent extraction (LPSE) were studied. The integrated process was proposed for processing two different semi-defatted annatto materials denoted Batches 1 and 2. The cost of manufacture (COM) was calculated for two different production scales (5 and 50L) considering the integrated process vs. only the mechanical fractionation method. The integrated process showed a significantly higher COM than mechanical fractionation method. This work suggests that mechanical fractionation method is an adequate and low-cost process to obtain a rich-pigment product from semi-defatted annatto seeds. Copyright © 2017 Elsevier Ltd. All rights reserved.

Application of microwave-assisted extraction to the analysis of PCBs and CBzs in fly ash from municipal solid waste incinerators

Energy Technology Data Exchange (ETDEWEB)

Sun, Yifei; Takaoka, Masaki; Takeda, Nobuo; Matsumoto, Tadao; Oshita, Kazuyuki [Kyoto Univ. (Japan). Dept. of Urban and Environmental Engineering

2004-09-15

The extraction step has been, in generally, the least developed aspect of most analytical procedures, including procedures for the analysis of PCBs and CBzs. Although the Soxhlet extraction (SE) method for solid samples, developed in 1879, is still employed today in many laboratories, during the past decade, several novel extraction techniques, such as supercritical fluid extraction (SFE), microwave-assisted extraction (MAE), and accelerated-solvent extraction (ASE), have been used to analyze PCBs, PAHs, and other persistent organic pollutants (POPs) from various matrixes. These newer methods are less time-consuming and use much smaller amounts of organic solvents. The efficiency of MAE has been reported to be higher than that of SFE. In the present study, MAE was used to analyze PCBs and CBzs in MSWI fly ash. Under different experimental conditions, the optimum solvent mixture, the optimum solvent volume, and the optimum irradiation time were established. Furthermore, the relative standard deviation (RSD) values were evaluated. Finally, MAE efficiencies were compared with those of SE. The main objective of the study, however, was to use water as a polar solvent in MAE. Because solvents with a high dielectric constant, such as water, have to be used in MAE to absorb the microwave energy and heat the solvent, the residual water after acid pretreatment could be used in MAE. Therefore, the air drying time, normally three days could be shortened with MAE following the required acid pretreatment.

Comparative Study of Green Sub- and Supercritical Processes to Obtain Carnosic Acid and Carnosol-Enriched Rosemary Extracts with in Vitro Anti-Proliferative Activity on Colon Cancer Cells

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Andrea del Pilar Sánchez-Camargo

2016-12-01

Full Text Available In the present work, four green processes have been compared to evaluate their potential to obtain rosemary extracts with in vitro anti-proliferative activity against two colon cancer cell lines (HT-29 and HCT116. The processes, carried out under optimal conditions, were: (1 pressurized liquid extraction (PLE, using an hydroalcoholic mixture as solvent at lab-scale; (2 Single-step supercritical fluid extraction (SFE at pilot scale; (3 Intensified two-step sequential SFE at pilot scale; (4 Integrated PLE plus supercritical antisolvent fractionation (SAF at pilot scale. Although higher extraction yields were achieved by using PLE (38.46% dry weight, this extract provided the lowest anti-proliferative activity with no observed cytotoxic effects at the assayed concentrations. On the other hand, extracts obtained using the PLE + SAF process provided the most active rosemary extracts against both colon cancer cell lines, with LC50 ranging from 11.2 to 12.4 µg/mL and from 21.8 to 31.9 µg/mL for HCT116 and HT-29, respectively. In general, active rosemary extracts were characterized by containing carnosic acid (CA and carnosol (CS at concentrations above 263.7 and 33.9 mg/g extract, respectively. Some distinct compounds have been identified in the SAF extracts (rosmaridiphenol and safficinolide, suggesting their possible role as additional contributors to the observed strong anti-proliferative activity of CA and CS in SAF extracts.

Bio-oil production from biomass via supercritical fluid extraction

Energy Technology Data Exchange (ETDEWEB)

Durak, Halil, E-mail: halildurak@yyu.edu.tr [Yuzuncu Yıl University, Vocational School of Health Services, 65080, Van (Turkey)

2016-04-18

Supercritical fluid extraction is used for producing bio-fuel from biomass. Supercritical fluid extraction process under supercritical conditions is the thermally disruption process of the lignocellulose or other organic materials at 250-400 °C temperature range under high pressure (4-5 MPa). Supercritical fluid extraction trials were performed in a cylindrical reactor (75 mL) in organic solvents (acetone, ethanol) under supercritical conditions with (calcium hydroxide, sodium carbonate) and without catalyst at the temperatures of 250, 275 and 300 °C. The produced liquids at 300 °C in supercritical liquefaction were analyzed and characterized by elemental, GC-MS and FT-IR. 36 and 37 different types of compounds were identified by GC-MS obtained in acetone and ethanol respectively.

Bio-oil production from biomass via supercritical fluid extraction

International Nuclear Information System (INIS)

Durak, Halil

2016-01-01

Supercritical fluid extraction is used for producing bio-fuel from biomass. Supercritical fluid extraction process under supercritical conditions is the thermally disruption process of the lignocellulose or other organic materials at 250-400 °C temperature range under high pressure (4-5 MPa). Supercritical fluid extraction trials were performed in a cylindrical reactor (75 mL) in organic solvents (acetone, ethanol) under supercritical conditions with (calcium hydroxide, sodium carbonate) and without catalyst at the temperatures of 250, 275 and 300 °C. The produced liquids at 300 °C in supercritical liquefaction were analyzed and characterized by elemental, GC-MS and FT-IR. 36 and 37 different types of compounds were identified by GC-MS obtained in acetone and ethanol respectively.

Comparison of extraction fluids used with contaminated soils

International Nuclear Information System (INIS)

Erickson, D.C.; White, E.; Loehr, R.C.

1991-01-01

Five separate solutions were evaluated for use as leaching fluids with soils containing petroleum refining waste residues. The extraction fluids were: (a) water, (b) dilute hydrochloric acid, (c) 0.05 molar EDTA, (d) acetate buffer and (e) a dilute sulfuric/nitric acid mixture. The soils were collected from former refinery land treatment sites which had been used to treat petroleum refining wastes. The extractions were performed using a rotary tumbler (30 RPM, 18 hours) and the resulting solutions were analyzed for polynuclear aromatic hydrocarbons (PAHs) and metals. Concentrations of the PAHs in each of the five solutions were near or below the analytical quantitation limits. Metal concentrations were highest in the HCL and EDTA extracts, although only a small fraction of the total available metal present in the soils was extracted by the solutions evaluated

Supercritical fluid extraction of hops

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ZORAN ZEKOVIC

2007-01-01

Full Text Available Five cultivars of hop were extracted by the method of supercritical fluid extraction using carbon dioxide (SFE–CO2 as extractant. The extraction (50 g of hop sample using a CO2 flow rate of 97.725 L/h was done in the two steps: 1. extraction at 150 bar and 40°C for 2.5 h (sample of series A was obtained and, after that, the same sample of hop was extracted in the second step: 2. extraction at 300 bar and 40 °C for 2.5 h (sample of series B was obtained. The Magnum cultivar was chosen for the investigation of the extraction kinetics. For the qualitative and quantitative analysis of the obtained hop extracts, the GC-MS method was used. Two of four themost common compounds of hop aroma (a-humulene and b-caryophyllene were detected in samples of series A. In addition, isomerized a-acids and a high content of b-acids were detected. The a-acids content in the samples of series B was the highest in the extract of the Magnum cultivar (it is a bitter variety of hop. The low contents of a-acids in all the other hop samples resulted in extracts with low a-acids content, i.e., that contents were under the prescribed a-acids content.

Identification and quantification of cannabinoids in Cannabis sativa L. plants by high performance liquid chromatography-mass spectrometry

NARCIS (Netherlands)

Aizpurua-Olaizola, Oier; Omar, Jone; Navarro, Patricia; Olivares, Maitane; Etxebarria, Nestor; Usobiaga, Aresatz

2014-01-01

High performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) has been successfully applied to cannabis plant extracts in order to identify cannabinoid compounds after their quantitative isolation by means of supercritical fluid extraction (SFE). MS conditions were optimized by means

Supercritical fluid extraction of positron-emitting radioisotopes from solid target matrices

International Nuclear Information System (INIS)

Schlyer, D.

2000-01-01

Supercritical fluids are attractive as media for both chemical reactions, as well as process extraction, since their physical properties can be manipulated by small changes in pressure and temperature near the critical point of the fluid. Such changes can result in drastic effects on density-dependent properties such as solubility, refractive index, dielectric constant, viscosity and diffusivity of the fluid. This suggests that pressure tuning of a pure supercritical fluid may be a useful means to manipulate chemical reactions on the basis of a thermodynamic solvent effect. It also means that the solvation properties of the fluid can be precisely controlled to enable selective component extraction from a matrix. In recent years there has been a growing interest in applying supercritical fluid extraction to the selective removal of trace metals from solid samples. Much of the work has been done on simple systems comprised of inert matrices such as silica or cellulose. Recently, this process as been expanded to environmental samples as well. However, very little is understood about the exact mechanism of the extraction process. Of course, the widespread application of this technology is highly dependent on the ability of scientists to model and predict accurate phase equilibria in complex systems. In this project, we plan to explore the feasibility of utilizing supercritical fluids as solvents for reaction and extraction of radioisotopes produced from solid enriched targets. The reason for this work is that many of these enriched target materials used for radioisotope production are expensive

Determination of major aromatic constituents in vanilla using an on-line supercritical fluid extraction coupled with supercritical fluid chromatography.

Science.gov (United States)

Liang, Yanshan; Liu, Jiaqi; Zhong, Qisheng; Shen, Lingling; Yao, Jinting; Huang, Taohong; Zhou, Ting

2018-04-01

An on-line supercritical fluid extraction coupled with supercritical fluid chromatography method was developed for the determination of four major aromatic constituents in vanilla. The parameters of supercritical fluid extraction were systematically investigated using single factor optimization experiments and response surface methodology by a Box-Behnken design. The modifier ratio, split ratio, and the extraction temperature and pressure were the major parameters which have significant effects on the extraction. While the static extraction time, dynamic extraction time, and recycle time had little influence on the compounds with low polarity. Under the optimized conditions, the relative extraction efficiencies of all the constituents reached 89.0-95.1%. The limits of quantification were in the range of 1.123-4.747 μg. The limits of detection were in the range of 0.3368-1.424 μg. The recoveries of the four analytes were in the range of 76.1-88.9%. The relative standard deviations of intra- and interday precision ranged from 4.2 to 7.6%. Compared with other off-line methods, the present method obtained higher extraction yields for all four aromatic constituents. Finally, this method has been applied to the analysis of vanilla from different sources. On the basis of the results, the on-line supercritical fluid extraction-supercritical fluid chromatography method shows great promise in the analysis of aromatic constituents in natural products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Super/Subcritical Fluid Extractions for Preparation of the Crystalline Titania

Czech Academy of Sciences Publication Activity Database

Matějová, Lenka; Cajthaml, Tomáš; Matěj, Z.; Benada, Oldřich; Klusoň, Petr; Šolcová, Olga

2010-01-01

Roč. 52, č. 2 (2010), s. 215-221 ISSN 0896-8446 R&D Projects: GA ČR GP104/09/P290; GA ČR GA104/09/0694 Institutional research plan: CEZ:AV0Z40720504; CEZ:AV0Z50200510 Keywords : titania * supercritical fluid extraction * pressurised fluid extraction Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.986, year: 2010

Floculação de Chlorella sp. produzida em concentrado de dessalinização e estudo de método de extração de lipídeos intracelulares

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Luiz Rodrigo Ito Morioka

2014-01-01

Full Text Available Chlorella sp. was used to assess algal lipid production with concentrated desalination. In order to investigate the action of the flocculating agent calcium chloride and pH, a Box-Behnken Design and a Central Composite Design (CCD were carried out. Also, Soxhlet and Supercritical Fluid Extraction (SFE, with and without sonication lipid extraction methods, were examined. The optimal flocculation conditions were pH 10.0 and 2.0 g/L of calcium chloride concentration. The highest lipid content of Chlorella sp. was obtained using the Soxhlet extraction method. The most abundant fatty acid extracted by Soxhlet and SFE, with and without sonication, was palmitic acid, whose proportions were 57.4%, 35.3% and 25.5%, respectively.

RED WINE EXTRACT OBTAINED BY MEMBRANE-BASED SUPERCRITICAL FLUID EXTRACTION: PRELIMINARY CHARACTERIZATION OF CHEMICAL PROPERTIES.

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W. Silva

Full Text Available ABSTRACT This study aims to obtain an extract from red wine by using membrane-based supercritical fluid extraction. This technique involves the use of porous membranes as contactors during the dense gas extraction process from liquid matrices. In this work, a Cabernet Sauvignon wine extract was obtained from supercritical fluid extraction using pressurized carbon dioxide as solvent and a hollow fiber contactor as extraction setup. The process was continuously conducted at pressures between 12 and 18 MPa and temperatures ranged from 30 to 50ºC. Meanwhile, flow rates of feed wine and supercritical CO2 varied from 0.1 to 0.5 mL min-1 and from 60 to 80 mL min-1 (NCPT, respectively. From extraction assays, the highest extraction percentage value obtained from the total amount of phenolic compounds was 14% in only one extraction step at 18MPa and 35ºC. A summarized chemical characterization of the obtained extract is reported in this work; one of the main compounds in this extract could be a low molecular weight organic acid with aromatic structure and methyl and carboxyl groups. Finally, this preliminary characterization of this extract shows a remarkable ORAC value equal to 101737 ± 5324 µmol Trolox equivalents (TE per 100 g of extract.

Birch Bark Dry Extract by Supercritical Fluid Technology: Extract Characterisation and Use for Stabilisation of Semisolid Systems

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Markus Armbruster

2017-03-01

Full Text Available Triterpene compounds like betulin, betulinic acid, erythrodiol, oleanolic acid and lupeol are known for many pharmacological effects. All these substances are found in the outer bark of birch. Apart from its pharmacological effects, birch bark extract can be used to stabilise semisolid systems. Normally, birch bark extract is produced for this purpose by extraction with organic solvents. Employing supercritical fluid technology, our aim was to develop a birch bark dry extract suitable for stabilisation of lipophilic gels with improved properties while avoiding the use of toxic solvents. With supercritical carbon dioxide, three different particle formation methods from supercritical solutions have been tested. First, particle deposition was performed from a supercritical solution in an expansion chamber. Second, the Rapid Expansion of Supercritical Solutions (RESS method was used for particle generation. Third, a modified RESS-procedure, forming the particles directly into the thereby gelated liquid, was developed. All three methods gave yields from 1% to 5.8%, depending on the techniques employed. The triterpene composition of the three extracts was comparable: all three gave more stable oleogels compared to the use of an extract obtained by organic solvent extraction. Characterizing the rheological behaviour of these gels, a faster gelling effect was seen together with a lower concentration of the extract required for the gel formation with the supercritical fluid (SCF-extracts. This confirms the superiority of the supercritical fluid produced extracts with regard to the oleogel forming properties.

Steroid hormones in environmental matrices: extraction method comparison.

Science.gov (United States)

Andaluri, Gangadhar; Suri, Rominder P S; Graham, Kendon

2017-11-09

The U.S. Environmental Protection Agency (EPA) has developed methods for the analysis of steroid hormones in water, soil, sediment, and municipal biosolids by HRGC/HRMS (EPA Method 1698). Following the guidelines provided in US-EPA Method 1698, the extraction methods were validated with reagent water and applied to municipal wastewater, surface water, and municipal biosolids using GC/MS/MS for the analysis of nine most commonly detected steroid hormones. This is the first reported comparison of the separatory funnel extraction (SFE), continuous liquid-liquid extraction (CLLE), and Soxhlet extraction methods developed by the U.S. EPA. Furthermore, a solid phase extraction (SPE) method was also developed in-house for the extraction of steroid hormones from aquatic environmental samples. This study provides valuable information regarding the robustness of the different extraction methods. Statistical analysis of the data showed that SPE-based methods provided better recovery efficiencies and lower variability of the steroid hormones followed by SFE. The analytical methods developed in-house for extraction of biosolids showed a wide recovery range; however, the variability was low (≤ 7% RSD). Soxhlet extraction and CLLE are lengthy procedures and have been shown to provide highly variably recovery efficiencies. The results of this study are guidance for better sample preparation strategies in analytical methods for steroid hormone analysis, and SPE adds to the choice in environmental sample analysis.

Identification of organic sulfur compounds in coal bitumen obtained by different extraction techniques using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometric detection

Energy Technology Data Exchange (ETDEWEB)

Machado, Maria Elisabete; Cappelli Fontanive, Fernando; Bastos Caramao, Elina; Alcaraz Zini, Claudia [Universidade Federal do Rio Grande do Sul, Instituto de Quimica, Porto Alegre, RS (Brazil); Oliveira, Jose Vladimir de [URI, Universidade Regional Integrada do Alto Uruguai e das Missoes, Erechim, RS (Brazil)

2011-11-15

The determination of organic sulfur compounds (OSC) in coal is of great interest. Technically and operationally these compounds are not easily removed and promote corrosion of equipment. Environmentally, the burning of sulfur compounds leads to the emission of SO{sub x} gases, which are major contributors to acid rain. Health-wise, it is well known that these compounds have mutagenic and carcinogenic properties. Bitumen can be extracted from coal by different techniques, and use of gas chromatography coupled to mass spectrometric detection enables identification of compounds present in coal extracts. The OSC from three different bitumens were tentatively identified by use of three different extraction techniques: accelerated solvent extraction (ASE), ultrasonic extraction (UE), and supercritical-fluid extraction (SFE). Results obtained from one-dimensional gas chromatography (1D GC) coupled to quadrupole mass spectrometric detection (GC-qMS) and from two-dimensional gas chromatography with time-of-flight mass spectrometric detection (GC x GC-TOFMS) were compared. By use of 2D GC, a greater number of OSC were found in ASE bitumen than in SFE and UE bitumens. No OSC were identified with 1D GC-qMS, although some benzothiophenes and dibenzothiophenes were detected by use of EIM and SIM modes. GC x GC-TOFMS applied to investigation of OSC in bitumens resulted in analytical improvement, as more OSC classes and compounds were identified (thiols, sulfides, thiophenes, naphthothiophenes, benzothiophenes, and benzonaphthothiophenes). The roof-tile effect was observed for OSC and PAH in all bitumens. Several co-elutions among analytes and with matrix interferents were solved by use of GC x GC. (orig.)

Supercritical fluid extraction of γ-Pyrones from Ammi visnaga L. fruits

Directory of Open Access Journals (Sweden)

Mokhtar Bishr

2018-06-01

Full Text Available Extraction with supercritical fluid technique has proved to be effective in many applications including extraction and separation of various active principals from medicinal plants. It was used due to its advantages especially safety, specificity, selectivity and ease of component recovery.Ammi visnaga, L. belongs to the family Apiaceae. The fruits are used specifically for the treatment of kidney stones depending on its γ-Pyrones (mainly khellin and visnagin [2]. The supercritical fluid extraction technique of khellin and visnagin was investigated and the operating conditions for their extraction were optimized. The effect of different pressure (150, 200, 300, 400 and 500 bars, temperature (35, 40, 45, 50 and 55 °C, and particle sizes of the raw material (0.5, 1, 1.4 mm and entire fruits on the extract yield was studied under dynamic conditions for extraction for a run time of 90 min. Optimum supercritical extraction condition was found to be 200 bars at 45 °C and optimum particle size was found to be 1.4 mm. The yield is yellowish white bitter powder and measures 1.74% w/w relative to the dried weight of the fruits containing 38.414% w/w average γ-Pyrones content of which 29.4%w/w khellin, and 9.014%w/w visnagin.The obtained extracts were analyzed by reversed phase HPLC. Keywords: Ammi visnaga fruits, γ-Pyrones (khellin and visnagin, Supercritical fluid extraction and HPLC

Fluid extraction using carbon dioxide and organophosphorus chelating agents

Science.gov (United States)

Smart, Neil G.; Wai, Chien M.; Lin, Yuehe; Kwang, Yak Hwa

1998-01-01

Methods for extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical CO.sub.2, and a chelating agent are described. The chelating agent forms a chelate with the species, the chelate being soluble in the fluid to allow removal of the species from the material. In preferred embodiments the extraction solvent is supercritical CO.sub.2 and the chelating agent comprises an organophosphorous chelating agent, particularly sulfur-containing organophosphorous chelating agents, including mixtures of chelating agents. Examples of chelating agents include monothiophosphinic acid, di-thiophosphinic acid, phosphine sulfite, phosphorothioic acid, and mixtures thereof. The method provides an environmentally benign process for removing metal and metalloids from industrial waste solutions, particularly acidic solutions. Both the chelate and the supercritical fluid can be regenerated and the contaminant species recovered to provide an economic, efficient process.

Selective chelation and extraction of lanthanides and actinides with supercritical fluids

International Nuclear Information System (INIS)

Brauer, R.D.; Carleson, T.E.; Harrington, J.D.; Jean, F.; Jiang, H.; Lin, Y.; Wai, C.M.

1994-01-01

This report is made up of three independent papers: (1) Supercritical Fluid Extraction of Thorium and Uranium with Fluorinated Beta-Diketones and Tributyl Phosphate, (2) Supercritical Fluid Extraction of Lanthanides with Beta-Diketones and Mixed Ligands, and (3) A Group Contribution Method for Predicting the Solubility of Solid Organic Compounds in Supercritical Carbon Dioxide. Experimental data are presented demonstrating the successful extraction of thorium and uranium using fluorinated beta-diketones to form stable complexes that are extracted with supercritical carbon dioxide. The conditions for extracting the lanthanide ions from liquid and solid materials using supercritical carbon dioxide are presented. In addition, the Peng-Robison equation of state and thermodynamic equilibrium are used to predict the solubilities of organic solids in supercritical carbon dioxide from the sublimation pressure, critical properties, and a centric factor of the solid of interest

Fractionation and Purification of Bioactive Compounds Obtained from a Brewery Waste Stream

Directory of Open Access Journals (Sweden)

Letricia Barbosa-Pereira

2013-01-01

Full Text Available The brewery industry generates waste that could be used to yield a natural extract containing bioactive phenolic compounds. We compared two methods of purifying the crude extract—solid-phase extraction (SPE and supercritical fluid extraction (SFE—with the aim of improving the quality of the final extract for potential use as safe food additive, functional food ingredient, or nutraceutical. The predominant fractions yielded by SPE were the most active, and the fraction eluted with 30% (v/v of methanol displayed the highest antioxidant activity (0.20 g L−1, similar to that of BHA. The most active fraction yielded by SFE (EC50 of 0.23 g L−1 was obtained under the following conditions: temperature 40°C, pressure 140 bar, extraction time 30 minutes, ethanol (6% as a modifier, and modifier flow 0.2 mL min−1. Finally, we found that SFE is the most suitable procedure for purifying the crude extracts and improves the organoleptic characteristics of the product: the final extract was odourless, did not contain solvent residues, and was not strongly coloured. Therefore, natural extracts obtained from the residual stream and purified by SFE can be used as natural antioxidants with potential applications in the food, cosmetic, and pharmaceutical industries.

Supercritical fluid extraction of 2-alkylcyclobutanones formed from triglycerides by irradiation

International Nuclear Information System (INIS)

Horvatovich, P.; Farkas, J.; Hasselmann, C.; Marchioni, E.

1998-01-01

Complete text of publication follows. Radiation processing is employed to improve the microbiological safety of foodstuffs, and at the same time to suit the 'minimal processing' principle. However adequate information for consumers to enable their free choices requires specific detection methods of irradiation processes. For this purpose one of the most suitable methods is the detection of 2-alkylcyclobutanones which are formed - according to the present knowledge - only by irradiation from the fatty acid part of triglycerides. For detection of these compounds a European Norm (EN 1785) has been established. The method consists of Sohxlet extraction of fatty acids from the food sample, separation of 2-alkylcyclobutanones from other fatty components with liquid chromatography on Florisil TM , and the GC-MS analysis of the appropriate fraction with single ion monitoring (SIM) monitoring of 98 and 112 ions. But this method has a relatively high detection limit (∼1 kGy), it is time consuming and needs costly and sophisticated apparates. To improve the detection of 2-alkylcyclobutanones we replaced the Sohxlet extraction step with a supercritical fluid extraction. We optimised trapping and extraction parameters. It was found that supercritical fluid extraction is more selective than Sohxlet extraction used in the standard protocol. The extract obtained by supercritical fluid extraction contains less quantity and number of detection-disturbing components. This work is the first step towards decreasing the detection limit which will be the derivatization of 2-alkylcyclobutanones with halogen-containing reagent, and detection of derivatives with electron-capture detector (ECD)

Comparative study of modern extraction techniques for the determination of environmental samples (M14)

International Nuclear Information System (INIS)

Gfrerer, M.; Lankmayr, E.

2002-01-01

Full text: The aim of any extraction method in analytical chemistry is, to effectively separate the analytes from the matrix. The whole step should be fast and quantitative with minimal solvent and time required. The classical Soxhlet extraction usually requires large volumes (up to 200 ml) of solvent to be refluxed through the solid samples for several hours. Therefore, in the last decades, alternatives for this extraction method have been presented and investigated such as ultrasonic extraction (UE), supercritical fluid extraction (SFE), accelerated solvent extraction (ASE), microwave-assisted extraction (MAE) and fluidized-bed extraction (FBE). The actual choice for analytical application is frequently the initial capital cost, operating costs, simplicity of operation, amount of organic solvent required and sample throughput. Since sample preparation is a critical step in the analytical cycle, special care has to be taken for an accurate choice and optimization of extraction techniques and clean-up procedures. Therefore, MAE and FBE were investigated for their influential extraction parameters and these parameters were optimized for the extraction of organochlorine biocides, polychlorinated biphenyls and polycyclic aromatic hydrocarbons from environmental matrices like soil, sediment and sewage sludge. The extraction yields were compared with those obtained by Soxhlet extraction performed following DIN-methods. Finally, the optimized modern methods were validated by systematic experiments with certified reference materials. Refs. 3 (author)

Green Tea Leaves Extract: Microencapsulation, Physicochemical and Storage Stability Study

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James A. Zokti

2016-07-01

Full Text Available Green tea polyphenols have been reported to possess many biological properties. Despite the many potential benefits of green tea extracts, their sensitivity to high temperature, pH and oxygen is a major disadvantage hindering their effective utilization in the food industry. Green tea leaves from the Cameron Highlands Malaysia were extracted using supercritical fluid extraction (SFE. To improve the stability, green tea extracts were encapsulated by spray-drying using different carrier materials including maltodextrin (MD, gum arabic (GA and chitosan (CTS and their combinations at different ratios. Encapsulation efficiency, total phenolic content and antioxidant capacity were determined and were found to be in the range of 71.41%–88.04%, 19.32–24.90 (g GAE/100 g, and 29.52%–38.05% respectively. Further analysis of moisture content, water activity, hygroscopicity, bulk density and mean particles size distribution of the microparticles were carried out and the results ranged from; 2.31%–5.11%, 0.28–0.36, 3.22%–4.71%, 0.22–0.28 g/cm3 and 40.43–225.64 µm respectively. The ability of the microparticles to swell in simulated gastric fluid (SGF and simulated intestinal fluid (SIF was determined as 142.00%–188.63% and 207.55%–231.77%, respectively. Release of catechin polyphenol from microparticles in SIF was higher comparable to that of SGF. Storage stability of encapsulated catechin extracts under different temperature conditions was remarkably improved compared to non-encapsulated extract powder. This study showed that total catechin, total phenolic content (TPC and antioxidant activity did not decrease significantly (p ≥ 0.05 under 4 °C storage conditions. The half-life study results were in the range of 35–60, 34–65 and 231–288 weeks at storage temperatures of 40 °C, 25 °C and 4 °C respectively, therefore, for improved shelf-life stability we recommend that microparticles should be stored at temperatures below 25 °C.

9 CFR 319.721 - Fluid extract of meat.

Science.gov (United States)

2010-01-01

... 9 Animals and Animal Products 2 2010-01-01 2010-01-01 false Fluid extract of meat. 319.721 Section... AGENCY ORGANIZATION AND TERMINOLOGY; MANDATORY MEAT AND POULTRY PRODUCTS INSPECTION AND VOLUNTARY INSPECTION AND CERTIFICATION DEFINITIONS AND STANDARDS OF IDENTITY OR COMPOSITION Meat Soups, Soup Mixes...

SigmaPlot 2000, Version 6.00, SPSS Inc. Computer Software Test Plan

Energy Technology Data Exchange (ETDEWEB)

HURLBUT, S.T.

2000-10-24

SigmaPlot is a vendor software product used in conjunction with the supercritical fluid extraction Fourier transform infrared spectrometer (SFE-FTIR) system. This product converts the raw spectral data to useful area numbers. SigmaPlot will be used in conjunction with procedure ZA-565-301, ''Determination of Moisture by Supercritical Fluid Extraction and Infrared Detection.'' This test plan will be performed in conjunction with or prior to HNF-6936, ''HA-53 Supercritical Fluid Extraction System Acceptance Test Plan'', to perform analyses for water. The test will ensure that the software can be installed properly and will manipulate the analytical data correctly.

Comparative analysis of the oil and supercritical CO(2) extract of Schinus molle L. growing in Yemen.

Science.gov (United States)

Ali, Nasser A Awadh; Marongiu, Bruno; Piras, Alessandra; Porcedda, Silvia; Falconieri, Danilo; Al-Othman, Al-Husein M R

2011-08-01

In this study, we report the preliminary data on the chemical composition of Yemeni Schinus molle L. volatile oil obtained by supercritical extraction with carbon dioxide (40°C and 90 bar), SFE, and by hydrodistillation (HD). The composition of the volatile oil has been analysed by GC and GC-MS. The content of the major constituents in the oils from leaves varied in the following ranges: germacrene D 3.7% in SFE and 16.7% in HD; β-caryophyllene 19.1% in SFE and 13.5% in HD. The amount of monoterpenes constituted 4%, in all the analysed samples, while the number of sesquiterpenes was 44% in supercritical and 67% in HD oil. Some compounds were not identified by GC-MS and it will require further analysis using other analytical techniques.

Pressurized fluid extraction of essential oil from Lavandula hybrida using a modified supercritical fluid extractor and a central composite design for optimization.

Science.gov (United States)

Kamali, Hossein; Jalilvand, Mohammad Reza; Aminimoghadamfarouj, Noushin

2012-06-01

Essential oil components were extracted from lavandin (Lavandula hybrida) flowers using pressurized fluid extraction. A central composite design was used to optimize the effective extraction variables. The chemical composition of extracted samples was analyzed by a gas chromatograph-flame ionization detector column. For achieving 100% extraction yield, the temperature, pressure, extraction time, and the solvent flow rate were adjusted at 90.6°C, 63 bar, 30.4 min, and 0.2 mL/min, respectively. The results showed that pressurized fluid extraction is a practical technique for separation of constituents such as 1,8-cineole (8.1%), linalool (34.1%), linalyl acetate (30.5%), and camphor (7.3%) from lavandin to be applied in the food, fragrance, pharmaceutical, and natural biocides industries. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Modifier free supercritical fluid extraction of uranium from sintered UO2, soil and ore samples

International Nuclear Information System (INIS)

Kanekar, A.S.; Pathak, P.N.; Acharya, R.; Mohapatra, P.K.; Manchanda, V.K.

2011-01-01

Direct extraction of uranium from different samples viz. sintered UO 2 , soil and ores was carried out by modifier free supercritical fluid using tri-n-butyl phosphate-nitric acid (TBP-HNO 3 ) adduct as extractant. These studies showed that pre-equilibration with more concentrated nitric acid helps in better dissolution and extraction of uranium from sintered UO 2 samples. Modifier free supercritical fluid extraction appears attractive with respect to minimization of secondary wastes. This method resulted 80-100% extraction of uranium from different soil/ore samples. The results were confirmed by performing neutron activation analysis of original (before extraction) and residue (after extraction) samples. (author)

Rapid extraction of PCDD/Fs from soil and fly ash samples. Pressurized fluid extraction (PFE) and microwave-assisted extraction (MAE)

Energy Technology Data Exchange (ETDEWEB)

Sanz, P.; Fabrellas, B. [Centro de Investigaciones Energeticas Medioambientales y Tecnologicas (CIEMAT), Madrid (Spain)

2004-09-15

The main reference extraction method in the analysis of polychlorinated dibenzop- dioxins and dibenzofurans (PCDD/Fs) is still the Soxhlet extraction. But it requires long extraction times (up to 24 hs), large volumes of hazardous organic solvents (100-300 ml) and its automation is limited. Pressurized Fluid Extraction (PFE) and Microwave-Assisted Extraction (MAE) are two relatively new extraction techniques that reduce the time and the volume of solvent required for extraction. However, very different PFE extraction conditions are found for the same enviromental matrices in the literature. MAE is not a extraction technique very applied for the analysis of PCDD/Fs yet, although it is used for the determination of other organic compounds, such as PCBs and PAHs. In this study, PFE and MAE extraction conditions were optimized to determine PCDDs y PCDFs in fly ash and soil/sediment samples. Conventional Soxhlet extraction with toluene was used to compare the extraction efficiency of both techniques.

High temperature solvent extraction of oil shale and bituminous coal using binary solvent mixtures

Energy Technology Data Exchange (ETDEWEB)

Goetz, G.K.E. [Lehrstuhl fuer Geologie, Geochemie und Lagerstaetten des Erdoels und der Kohle, RWTH Aachen (Germany)

1997-12-31

A high volatile bituminous coal from the Saar Basin and an oil shale from the Messel deposit, both Germany, were extracted with binary solvent mixtures using the Advanced Solvent Extraction method (ASE). Extraction temperature and pressure were kept at 100 C, respectively 150 C, and 20,7 MPa. After the heating phase (5 min) static extractions were performed with mixtures (v:v, 1:3) of methanol with toluene, respectively trichloromethane, for further 5 min. Extract yields were the same or on a higher level compared to those from classical soxhlet extractions (3 days) using the same solvents at 60 C. Comparing the results from ASE with those from supercritical fluid extraction (SFE) the extract yields were similar. Increasing the temperature in ASE releases more soluble organic matter from geological samples, because compounds with higher molecular weight and especially more polar substances were solubilized. But also an enhanced extraction efficiency resulted for aliphatic and aromatic hydrocarbons which are used as biomarkers in Organic Geochemistry. Application of thermochemolysis with tetraethylammonium hydroxide (TEAH) using pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) on the extraction residues shows clearly that at higher extraction temperatures minor amounts of free fatty acids or their methyl esters (original or produced by ASE) were trapped inside the pore systems of the oil shale or the bituminous coal. ASE offers a rapid and very efficient extraction method for geological samples reducing analysis time and costs for solvents. (orig.)

Direct online extraction and determination by supercritical fluid extraction with chromatography and mass spectrometry of targeted carotenoids from red Habanero peppers (Capsicum chinense Jacq.).

Science.gov (United States)

Zoccali, Mariosimone; Giuffrida, Daniele; Dugo, Paola; Mondello, Luigi

2017-10-01

Recently, supercritical fluid chromatography coupled to mass spectrometry has gained attention as a fast and useful technology applied to the carotenoids analysis. However, no reports are available in the literature on the direct online extraction and determination by supercritical fluid extraction with chromatography and mass spectrometry. The aim of this research was the development of an online method coupling supercritical fluid extraction and supercritical fluid chromatography for a detailed targeted native carotenoids characterization in red habanero peppers. The online nature of the system, compared to offline approaches, improves run-to-run precision, enables the setting of batch-type applications, and reduces the risks of sample contamination. The extraction has been optimized using different temperatures, starting from 40°C up to 80°C. Multiple extractions, until depletion, were performed on the same sample to evaluate the extraction yield. The range of the first extraction yield, carried out at 80°C, which was the best extraction temperature, was 37.4-65.4%, with a %CV range of 2-12. Twenty-one targeted analytes were extracted and identified by the developed methodology in less than 17 min, including free, monoesters, and diesters carotenoids, in a very fast and efficient way. Quantification of the β-carotene was carried out by using the optimized conditions. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Investigation of extractable organic compounds in deep-sea hydrothermal vent fluids along the Mid-Atlantic Ridge

Science.gov (United States)

McCollom, Thomas M.; Seewald, Jeffrey S.; German, Christopher R.

2015-05-01

The possibility that deep-sea hydrothermal vents may contain organic compounds produced by abiotic synthesis or by microbial communities living deep beneath the surface has led to numerous studies of the organic composition of vent fluids. Most of these studies have focused on methane and other light hydrocarbons, while the possible occurrence of more complex organic compounds in the fluids has remained largely unstudied. To address this issue, the presence of higher molecular weight organic compounds in deep-sea hydrothermal fluids was assessed at three sites along the Mid-Atlantic Ridge that span a range of temperatures (51 to >360 °C), fluid compositions, and host-rock lithologies (mafic to ultramafic). Samples were obtained at several sites within the Lucky Strike, Rainbow, and Lost City hydrothermal fields. Three methods were employed to extract organic compounds for analysis, including liquid:liquid extraction, cold trapping on the walls of a coil of titanium tubing, and pumping fluids through cartridges filled with solid phase extraction (SPE) sorbents. The only samples to consistently yield high amounts of extractable organic compounds were the warm (51-91 °C), highly alkaline fluids from Lost City, which contained elevated concentrations of C8, C10, and C12n-alkanoic acids and, in some cases, trithiolane, hexadecanol, squalene, and cholesterol. Collectively, the C8-C12 acids can account for about 15% of the total dissolved organic carbon in the Lost City fluids. The even-carbon-number predominance of the alkanoic acids indicates a biological origin, but it is unclear whether these compounds are derived from microbial activity occurring within the hydrothermal chimney proximal to the site of fluid discharge or are transported from deeper within the system. Hydrothermal fluids from the Lucky Strike and Rainbow fields were characterized by an overall scarcity of extractable dissolved organic compounds. Trace amounts of aromatic hydrocarbons including

Determination of As concentration in earthworm coelomic fluid extracts by total-reflection X-ray fluorescence spectrometry

Science.gov (United States)

Allegretta, Ignazio; Porfido, Carlo; Panzarino, Onofrio; Fontanella, Maria Chiara; Beone, Gian Maria; Spagnuolo, Matteo; Terzano, Roberto

2017-04-01

Earthworms are often used as sentinel organisms to study As bioavailability in polluted soils. Arsenic in earthworms is mainly sequestrated in the coelomic fluids whose As content can therefore be used to asses As bioavalability. In this work, a method for determining As concentration in coelomic fluid extracts using total-reflection X-ray fluorescence spectrometry (TXRF) is presented. For this purpose coelomic fluid extracts from earthworms living in three polluted soils and one non-polluted (control) soil have been collected and analysed. A very simple sample preparation was implemented, consisting of a dilution of the extracts with polyvinyl alcohol (PVA) using a 1:8 ratio and dropwise deposition of the sample on the reflector. A detection limit of 0.2 μg/l and quantification limit of 0.6 μg/l was obtained in the diluted samples, corresponding to 2 μg/l and 6 μg/l in the coelomic fluid extracts, respectively. This allowed to quantify As concentration in coelomic fluids extracted from earthworms living in soils polluted with As at concentrations higher than 20 mg/kg (considered as a pollution threshold for agricultural soils). The TXRF method has been validated by comparison with As concentrations in standards and by analysing the same samples by ICP-MS, after acid digestion of the sample. The low limit of detection, the proven reliability of the method and the little sample preparation make TXRF a suitable, cost-efficient and "green" technique for the analysis of As in earthworm coelomic fluid extracts for bioavailability studies.

Anti-inflammatory and antiallergic activity in vivo of lipophilic Isatis tinctoria extracts and tryptanthrin.

Science.gov (United States)

Recio, María-Carmen; Cerdá-Nicolás, Miguel; Potterat, Olivier; Hamburger, Matthias; Ríos, José-Luis

2006-05-01

The effects of a supercritical CO2 (SFE) extract, a dichloromethane (DCM) extract from Isatis tinctoria leaf and the alkaloidal constituent tryptanthrin were studied in acute and subchronic experimental models of inflammation. The SFE and DCM extracts showed anti-inflammatory activity in the carrageenan-induced acute mouse paw oedema (ED50 values of 78 mg/kg and 165 mg/kg P. O., respectively) and in the acute tetradecanoylphorbol acetate (TPA)-induced mouse ear oedema in oral (62% and 32% oedema reduction at 100 and 125 mg/kg, respectively) and topical application (37% and 33% reduction of oedema at 0.5 mg/ear). In contrast, tryptanthrin showed no significant anti-inflammatory effect. The DCM extract inhibited oedema formation and neutrophil infiltration in subchronic inflammation in mice induced by repeated application of TPA. The extract showed activity after oral and topical administration by reducing the various parameters of the inflammatory response. The DCM extract (1 mg/ear) inhibited the delayed-type hypersensitivity (DTH) reaction induced by application of dinitrofluorobenzene (DNFB) after topical application. The response during the induction phase (24 h) was decreased by 48%, and the inflammatory phase (48 to 96 h) was reduced by 53 to 56%. The extract had no effect in this model when administered orally. The DCM extract (200 mg/kg P. O.) inhibited the acetic acid-induced writhing by 49%.

A review of extractions of seaweed hydrocolloids: Properties and applications

Directory of Open Access Journals (Sweden)

H. P. S. Abdul Khalil

2018-04-01

Full Text Available The term hydrocolloid generally refers to substances that form gels or provide viscous dispersion in the presence of water. Alginate, agar, and carrageenan are three commercially valuable hydrocolloids derived from certain brown and red seaweed and each has their distinct physicochemical properties (i.e. functional and bioactive. Various applications of these seaweed hydrocolloids as thickeners, stabilizers, coagulants and salves (in the wound and burn dressings and materials to produce bio-medical impressions in the food, pharmaceutical, and biotechnology industries are highlighted in this review. Although the existing industrial methods of extraction for these seaweed hydrocolloids are well-established, still growing demand has exposed certain limitations of those methods, notably efficiency and product consistency. In order to achieve targeted hydrocolloids for specific purposes and functionalities, some novel and green extraction methods have also been proposed and discussed. Microwave-assisted extraction (MAE, ultrasound-assisted extraction (UAE, enzyme-assisted extraction (EAE, supercritical fluid extraction (SFE, pressurized solvent extractions (PSE, reactive extrusion and photobleaching process are selectively presented as highly promising candidates that can avoid the use of chemicals and provide novel means of access to seaweed hydrocolloids with both economic and environmental benefits. However, this review does not provide the ‘best’ method or procedure as many are still under development. Hence, the review gives ‘food for thought’as to new processes which might be adopted industrially and concluded that further research is required in order to contribute additional new knowledge and refinement to this field of study.

Extraction of metals and/or metalloids from acidic media using supercritical fluids and salts

International Nuclear Information System (INIS)

Wai, C.M.; Smart, N.G.; Lin, Y.

1998-01-01

A method is described for extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical carbon dioxide, containing a chelating agent. The chelating agent forms chelates that are soluble in the fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent comprises a trialkyl phosphate, a triaryl phosphate, a trialkylphosphine oxide, a triarylphosphine oxide, or mixtures thereof. The method provides an environmentally benign process for removing contaminants from industrial waste. The method is particularly useful for extracting actinides from acidic solutions, and the process can be aided by the addition of nitrate salts. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process. 7 figs

Extraction of metals and/or metalloids from acidic media using supercritical fluids and salts

Science.gov (United States)

Wai, Chien M.; Smart, Neil G.; Lin, Yuehe

1998-01-01

A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical carbon dioxide, containing a chelating agent is described. The chelating agent forms chelates that are soluble in the fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent comprises a trialkyl phosphate, a triaryl phosphate, a trialkylphosphine oxide, a triarylphosphine oxide, or mixtures thereof. The method provides an environmentally benign process for removing contaminants from industrial waste. The method is particularly useful for extracting actinides from acidic solutions, and the process can be aided by the addition of nitrate salts. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process.

Inhibitory Effects of Adlay Extract on Melanin Production and Cellular Oxygen Stress in B16F10 Melanoma Cells

Directory of Open Access Journals (Sweden)

Huey-Chun Huang

2014-09-01

Full Text Available The aim of this study was to determine the effects of adlay extract on melanin production and the antioxidant characteristics of the extract. The seeds were extracted by the supercritical fluid CO2 extraction (SFE method. The effect of adlay extract on melanin production was evaluated using mushroom tyrosinase activity assay, intracellular tyrosinase activity, antioxidant properties and melanin content. Those assays were performed spectrophotometrically. In addition, the expression of melanogenesis-related proteins was determined by western blotting. The results revealed that the adlay extract suppressed intracellular tyrosinase activity and decreased the amount of melanin in B16F10 cells. The adlay extract decreased the expression of microphthalmia-associated transcription factor (MITF, tyrosinase, tyrosinase related protein-1 (TRP-1 and tyrosinase related protein-2 (TRP-2. The extract also exhibited antioxidant characteristics such as free radical scavenging capacity and reducing power. It effectively decreased intracellular reactive oxygen species (ROS levels in B16F10 cells. We concluded that the adlay extract inhibits melanin production by down-regulation of MITF, tyrosinase, TRP-1 and TRP-2. The antioxidant properties of the extract may also contribute to the inhibition of melanogenesis. The adlay extract can therefore be applied as an inhibitor of melanogenesis and could also act as a natural antioxidant in skin care products.

Supercritical carbon dioxide extraction of electrolyte from spent lithium ion batteries and its characterization by gas chromatography with chemical ionization

Science.gov (United States)

Mönnighoff, Xaver; Friesen, Alex; Konersmann, Benedikt; Horsthemke, Fabian; Grützke, Martin; Winter, Martin; Nowak, Sascha

2017-06-01

The aging products of the electrolyte from a commercially available state-of-the-art 18650-type cell were investigated. During long term cycling a huge difference in their performance and lifetime at different temperatures was observed. By interpretation of a strong capacity fading of cells cycled at 20 °C compared to cells cycled at 45 °C a temperature depending aging mechanism was determined. To investigate the influence of the electrolyte on this fading, the electrolyte was extracted by supercritical fluid extraction (SFE) and then analyzed by gas chromatography (GC) with electron impact (EI) ionization and mass selective detection. To obtain more information with regard to the identification of unknown decomposition products further analysis with positive chemical ionization (PCI) and negative chemical ionization (NCI) was performed. 17 different volatile organic aging products were detected and identified. So far, seven of them were not yet known in literature and several formation pathways were postulated taking previously published literature into account.

Subcritical Fluid Extraction of Chinese Quince Seed: Optimization and Product Characterization.

Science.gov (United States)

Wang, Li; Wu, Min; Liu, Hua-Min; Ma, Yu-Xiang; Wang, Xue-De; Qin, Guang-Yong

2017-03-25

Chinese quince seed (CQS) is an underutilized oil source and a potential source of unsaturated fatty acids and α-tocopherol-rich oil. Subcritical fluid (SCF) extraction is executed at lower pressures and temperatures than the pressures and temperatures used in supercritical fluid extraction. However, no studies on the SCF extraction of CQS oil are reported. Therefore, the objective of this study was to evaluate the use of SCF for the extraction of CQS oil and to compare the use of SCF with the classical Soxhlet (CS) and supercritical CO₂ (SC-CO₂) extraction methods. Response surface methodology (RSM) was used to investigate the extraction conditions: temperature (45-65 °C), time (30-50 min), and solvent/solid ratio (5-15 mL/g). The optimization results showed that the highest yield (27.78%) was obtained at 56.18 °C, 40.20 min, and 12.57 mL/g. The oil extracted by SCF had a higher unsaturated fatty acid content (86.37%-86.75%), higher α-tocopherol content (576.0-847.6 mg/kg), lower acid value (3.97 mg/g), and lower peroxide value (0.02 meq O₂/kg) than extractions using CS and SC-CO 2 methods. The SCF-defatted meal of oilseed exhibited the highest nitrogen solubility index (49.64%) and protein dispersibility index (50.80%), demonstrating that SCF extraction was a promising and efficient technique as an alternative to CS and SC-CO 2 methods, as very mild operating conditions and an eco-friendly solvent can be used in the process with maximum preservation of the quality of the meal.

The stability and degradation kinetics of Sulforaphene in microcapsules based on several biopolymers via spray drying.

Science.gov (United States)

Tian, Guifang; Li, Yuan; Yuan, Qipeng; Cheng, Li; Kuang, Pengqun; Tang, Pingwah

2015-05-20

Sulforaphene (SFE) was extracted from the radish seeds and the purity of SFE extracted by our laboratory was 95%. It is well known that SFE can prevent cancers. It is also known that SFE is unstable to heat. To overcome the problem, SFE microcapsules using natural biopolymers were prepared by spray drying. The results indicated that SFE microcapsules using hydroxypropyl-β-cyclodextrin (HP-β-CD), maltodextrin (MD) and isolated soybean protein (SPI) as wall materials could effectively improve its stability against heat, especially SFE-loaded HP-β-CD and MD microcapsules. The amount of SFE in the microcapsules was found 20% higher than that of the non-encapsulated SFE under 90 °C in 168 h. Our finding suggested that the rate of degradation of the non-encapsulated and encapsulated SFE with HP-β-CD, MD and SPI followed the first-order kinetics. The speed of the degradation of the encapsulated SFE in biopolymers increased from SFE with HP-β-CD, to SFE with MD, and to SFE-SPI. The non-encapsulated SFE degrades fastest. Copyright © 2015 Elsevier Ltd. All rights reserved.

Superkritická extrakce kapalin – nová progresivní metoda v pivovarské analytice. Část II. - Možnosti uplatnění superkritické extrakce kapalin při analýze senzoricky aktivních látek v pivě

Czech Academy of Sciences Publication Activity Database

Čulík, J.; Horák, T.; Čejka, P.; Jurková, M.; Kellner, V.; Karásek, Pavel; Ostrá, Elena V.

2006-01-01

Roč. 52, č. 5 (2006), s. 142-147 ISSN 0023-5830. [Pivovarsko-sladařský seminář /32./. Plzeň, 13.10.2004-14.10.2004] Institutional research plan: CEZ:AV0Z40310501 Keywords : supercritical fluid extraction * SFE of liquids * sensory active substances Subject RIV: CB - Analytical Chemistry, Separation

Ginger and turmeric starches hydrolysis using subcritical water + CO2: the effect of the SFE pre-treatment

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S. R. M. Moreschi

2006-06-01

Full Text Available In this work, the hydrolysis of fresh and dried turmeric (Curcuma longa L. and ginger (Zingiber officinale R. in the presence of subcritical water + CO2 was studied. The hydrolysis of ginger and turmeric bagasses from supercritical fluid extraction was also studied. The reactions were done using subcritical water and CO2 at 150 bar, 200 °C and reaction time of 11 minutes; the degree of reaction was monitored through the amount of starch hydrolyzed. Process yields were calculated using the amount of reducing and total sugars formed. The effects of supercritical fluid extraction in the starchy structures were observed by scanning electron microscopy. Higher degree of hydrolysis (97- 98 % were obtained for fresh materials and the highest total sugar yield (74% was established for ginger bagasse. The supercritical fluid extraction did not significantly modify the degree of hydrolysis in the tested conditions.

Extraction of gold and silver from geothermal fluid

Energy Technology Data Exchange (ETDEWEB)

Brown, K.L.; Roberts, P.J. (Geothermal Research Center, Wairakei (New Zealand); Spectrum Resources Ltd., Auckland (New Zealand))

1988-11-10

This paper describes the results of five experiments of the extraction of gold and silver from hydrothermal fluids with a experimental vessel settled up at KA35 well at the Kawerau geothermal field in New Zealand. The experimental vessel was designed to absorb the fluids from orifice plate controlled to be low pressure and had a chamber having within many collecting plates. The first experiment is a fundamental one in which a mild steel was used as metal collector plate. The rates of deposition of gold and silver on the plate were estimated. The second experiment showed that the rate on deposition of gold on the mild steel plate was controlled by the flux rate of hydrothermal fluid. The third experiment showed that a mild steel seemed to be better for the collection plate of gold and silver than copper and aluminium. The fourth experiment clarified that the activated charcoal was not suitable for the collector plate for gold and silver. The fifth experiment showed that a mild steel was better for metal collector than activated charcoal. 1 ref., 4 figs.

Coupled Hydro-Mechanical Simulations of CO2 Storage Supported by Pressure Management Demonstrate Synergy Benefits from Simultaneous Formation Fluid Extraction

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Kempka Thomas

2015-04-01

Full Text Available We assessed the synergetic benefits of simultaneous formation fluid extraction during CO2 injection for reservoir pressure management by coupled hydro-mechanical simulations at the prospective Vedsted storage site located in northern Denmark. Effectiveness of reservoir pressure management was investigated by simulation of CO2 storage without any fluid extraction as well as with 66% and 100% equivalent volume formation fluid extraction from four wells positioned for geothermal heat recovery. Simulation results demonstrate that a total pressure reduction of up to about 1.1 MPa can be achieved at the injection well. Furthermore, the areal pressure perturbation in the storage reservoir can be significantly decreased compared to the simulation scenario without any formation fluid extraction. Following a stress regime analysis, two stress regimes were considered in the coupled hydro-mechanical simulations indicating that the maximum ground surface uplift is about 0.24 m in the absence of any reservoir pressure management. However, a ground uplift mitigation of up to 37.3% (from 0.24 m to 0.15 m can be achieved at the injection well by 100% equivalent volume formation fluid extraction. Well-based adaptation of fluid extraction rates can support achieving zero displacements at the proposed formation fluid extraction wells located close to urban infrastructure. Since shear and tensile failure do not occur under both stress regimes for all investigated scenarios, it is concluded that a safe operation of CO2 injection with simultaneous formation fluid extraction for geothermal heat recovery can be implemented at the Vedsted site.

Supercritical carbon dioxide extract exhibits enhanced antioxidant and anti-inflammatory activities of Physalis peruviana.

Science.gov (United States)

Wu, S J; Tsai, J Y; Chang, S P; Lin, D L; Wang, S S; Huang, S N; Ng, L T

2006-12-06

Physalis peruviana L. (PP) is a medicinal herb widely used in folk medicine. In this study, supercritical carbon dioxide (SFE-CO2) method was employed to obtain three different PP extracts, namely SCEPP-0, SCEPP-4 and SCEPP-5. The total flavonoid and phenol concentrations, as well as antioxidant and anti-inflammatory activities of these extracts were analyzed and compared with aqueous and ethanolic PP extracts. Among all the extracts tested, SCEPP-5 demonstrated the highest total flavonoid (234.63+/-9.61 mg/g) and phenol (90.80+/-2.21 mg/g) contents. At concentrations 0.1-30 microg/ml, SCEPP-5 also demonstrated the strongest superoxide anion scavenging activity and xanthine oxidase inhibitory effect. At 30 microg/ml, SCEPP-5 significantly prevented lipopolysaccharide (LPS; 1 microg/ml)-induced cell cytotoxicity in murine macrophage (Raw 264.7) cells. At 10-50 microg/ml, it also significantly inhibited LPS-induced NO release and PGE2 formation in a dose-dependent pattern. SCEPP-5 at 30 microg/ml remarkably blocked the LPS induction of inducible nitric oxide synthase (iNOS) and cyclooxygenase-2 (COX-2) expression. Taken together, these results suggest that SCEPP-5, an extract of SFE-CO2, displayed the strongest antioxidant and anti-inflammatory activities as compared to other extracts. Its protection against LPS-induced inflammation could be through the inhibition of iNOS and COX-2 expression.

Chemical composition of the essential oil and supercritical CO2 extract of Commiphora myrrha (Nees) Engl. and of Acorus calamus L.

Science.gov (United States)

Marongiu, Bruno; Piras, Alessandra; Porcedda, Silvia; Scorciapino, Andrea

2005-10-05

Volatile concentrates from the oleo-gum resin of Commiphora myrrha (Nees) Engl. and from the rhizomes of Acorus calamus were isolated by supercritical extraction with carbon dioxide. The volatile oil of myrrh was obtained at 9.0 MPa and 50 degrees C and at a CO2 flow of 1.5 kg/h. Acorus calamus was extracted at 9.0 MPa and 45 degrees C and at a CO2 flow of 1.6 kg/h. In both cases, an oil devoid of cuticular waxes was obtained with a single depressurization stage. The SFE myrrh oil had a yield, Y, of 3.2%. Its main components, identified and quantified by GC/MS, were furanoeudesma-1,3-diene, 34.9%; lindestrene, 12.9%; curzerene, 8.5%; and germacrone, 5.8%. The essential oils from the same starting material by hydrodistillation, HD, (Y = 2.8%) and by steam distillation, SD, (Y = 0.4%) were quite similar to the SFE extract. The main components of the SFE oil of A. calamus (Y = 3.5%) were acorenone, 13.4%; iso-acorone, 11.6%; (Z)-sesquilavandulol, 11.0%; dehydroxy isocalamendiol, 7.7%; and beta-asarone, 5.5%. The comparison with hydrodistilled (Y = 1.8%) and steam distilled (Y = 1.0%) oils revealed large differences in the content of iso-acorone and crypto-acorone.

Environmental application of millimetre-scale sponge iron (s-Fe"0) particles (IV): New insights into visible light photo-Fenton-like process with optimum dosage of H_2O_2 and RhB photosensitizers

International Nuclear Information System (INIS)

Ju, Yongming; Yu, Yunjiang; Wang, Xiaoyan; Xiang, Mingdeng; Li, Liangzhong; Deng, Dongyang; Dionysiou, Dionysios D.

2017-01-01

Highlights: • Synergistic action of Rhodamine B (RhB), visible light, H_2O_2 and s-Fe"0 is essential. • The complexes of RhB and Fe"3"+ eject one electron via ligand-to-metal charge-transfer. • RhB assists the photo-Fenton-like removal of tetrabromobisphenol A (TBBPA). - Abstract: In this study, we firstly develop the photo-Fenton-like system with millimetric sponge iron (s-Fe"0), H_2O_2, visible light (vis, λ ≥ 420 nm) and rhodamine B (RhB), and present a comprehensive study concerning the mechanism. Thus, we investigate (1) the adsorption of RhB onto s-Fe"0, (2) the photo-Fenton-like removal of RhB over iron oxides generated from the corrosion of s-Fe"0, (3) the homogeneous photo-Fenton removal of RhB over Fe"2"+ or Fe"3"+, (4) the Fe"3"+-RhB complexes, and (5) the photo-Fenton-like removal of tetrabromobisphenol A (TBBPA). The results show that neither the adsorption process over s-Fe"0 nor the photo-Fenton-like process over FeOOH, Fe_3O_4 and Fe_2O_3, achieved efficient removal of RhB. For comparison, in homogeneous photo-Fenton process, the presence of Fe"3"+ ions, rather than Fe"2"+ ions, effectively eliminated RhB. Furthermore, the UV–vis spectra showing new absorbance at ∼ 285 nm indicate the complexes of RhB and Fe"3"+ ions, adopting vis photons to form excited state and further eject one electron via ligand-to-metal charge-transfer to activate H_2O_2. Additionally, efficient TBBPA removal was obtained only in the presence of RhB. Accordingly, the s-Fe"0– based photo-Fenton-like process assisted with dyestuff wastewater is promising for removing a series of persistent organic pollutants.

Squalene Extraction by Supercritical Fluids from Traditionally Puffed Amaranthus hypochondriacus Seeds

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Teresa Rosales-García

2017-01-01

Full Text Available Extraction of squalene, a potent natural antioxidant, from puffed A. hypochondriacus seeds was performed by supercritical fluid extraction (SCFE; besides, to have a blank for comparison, extraction was performed also by Soxhlet method using organic solvents (hexane. Chemical proximal composition and seed morphology were determined in raw, puffed, and SCFE-extracted seeds. Extracts were obtained with a 500 mL capacity commercial supercritical extractor and performed between 10 and 30 MPa at 313, 323, and 333 K under constant CO2 flow of 0.18 kg CO2/h during 8 h. The squalene content was determined and the fatty acids present in the extracts were identified by GC-MS. The extract obtained by SCFE from puffed amaranth seeds reached 460 ± 28.1 g/kg squalene in oily extract at 313 K/20 MPa.

Effect temperature of supercritical CO2 fluid extraction on phytochemical analysis and antioxidant activity of Zingiber officinale Roscoe

Science.gov (United States)

Sondari, Dewi; Irawadi, Tun Tedja; Setyaningsih, Dwi; Tursiloadi, Silvester

2017-11-01

Supercritical fluid extraction of Zingiber officinale Roscoe has been carried out at a pressure of 16 MPa, with temperatures between 20-40 °C, during extraction time of 6 hours and the flow rate of CO2 fluid 5.5 ml/min. The result of supercritical method was compared with the extraction maceration using a mixture of water and ethanol (70% v/v) for 24 hours. The main content in ginger that has a main role as an antioxidant is a gingerol compound that can help neutralize the damaging effects caused by free radicals in the body, as anti-coagulant, and inhibit the occurrence of blood clots. This study aims to determine the effect of temperature on chemical components contained in rough extract of Zingiber officinale Roscoe and its antioxidant activity, total phenol and total flavonoid content. To determine the chemical components contained in the crude extract of Zingiber officinale Roscoe extracted by supercritical fluid and maceration extraction, GC-MS analysis was performed. Meanwhile, the antioxidant activity of the extract was evaluated based on a 2.2-diphenyl-1-picrylhydrazyl (DPPH) free radical damping method. The results of the analysis show that the result of ginger extract by using the supercritical CO2 extraction method has high antioxidant activity than by using maceration method. The highest total phenol content and total flavonoids were obtained on ginger extraction using supercritical CO2 fluid extraction, indicating that phenol and flavonoid compounds contribute to antioxidant activity. Chromatographic analysis showed that the chemical profile of ginger extract containing oxygenated monoterpenes, monoterpene hydrocarbons, sesquiterpene hydrocarbons, oxygenated monoterpene gingerol and esters. In supercritical fluid extraction, the compounds that can be identified at a temperature of 20-40 °C contain 27 compounds, and 11 compounds from the result of maceration extract. The main component of Zingiber officinale Roscoe extracted using supercritical fluid

Effects of process parameters on peanut skins extract and CO2 diffusivity by supercritical fluid extraction

Science.gov (United States)

Putra, N. R.; Yian, L. N.; Nasir, H. M.; Idham, Z. Binti; Yunus, M. A. C.

2018-03-01

Peanut skins (Arachis hypogea) are an agricultural waste product which has received much attention because they contain high nutritional values and can be potentially utilized in difference industries. At present, only a few studies have been conducted to study the effects of parameters on the peanut skins oil extraction. Therefore, this study aimed to determine the best extraction condition in order to obtain the highest extract yield using supercritical carbon dioxide (SC-CO2) with co-solvent Ethanol as compared to Soxhlet extraction method. Diffusivity of carbon dioxide in supercritical fluid extraction was determined using Crank model. The mean particle size used in this study was 425 µm. The supercritical carbon dioxide was performed at temperature (40 – 70 °C), flow rate of co-solvent ethanol (0 - 7.5% Vethanol/Vtotal), and extraction pressure (10 – 30 MPa) were used in this studies. The results showed that the percentage of oil yields and effective diffusivity increase as the pressure, rate of co-solvent, and temperature increased.

Studies on supercritical fluid extraction behaviour of uranium and thorium nitrates using amides

International Nuclear Information System (INIS)

Sujatha, K.; Kumar, R.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R.

2007-01-01

Supercritical fluid extraction studies of uranyl nitrate and thorium nitrate in mixture were carried out using various amides such as N,N-di(2-ethylhexyl) isobutyramide (D2EHIBA),N,N-dihexyl octanamide (DHOA) and Diisooctyl Butanamide (DiOBA). These studies established a preferential extraction of uranium over thorium. Among the various amides studied, D2EHIBA offered the best rate of preferential extraction of uranium over thorium. (author)

MEASUREMENT OF PYRETHROID RESIDUES IN ENVIRONMENTAL AND FOOD SAMPLES BY ENHANCED SOLVENT EXTRACTION/SUPERCRITICAL FLUID EXTRACTION COUPLED WITH GAS CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

Science.gov (United States)

The abstract summarizes pyrethorid methods development research. It provides a summary of sample preparation and analytical techniques such as supercritical fluid extraction, enhance solvent extraction, gas chromatography and tandem mass spectrometry.

Modeling of the Kinetics of Supercritical Fluid Extraction of Lipids from Microalgae with Emphasis on Extract Desorption

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Helena Sovová

2016-05-01

Full Text Available Microalgae contain valuable biologically active lipophilic substances such as omega-3 fatty acids and carotenoids. In contrast to the recovery of vegetable oils from seeds, where the extraction with supercritical CO2 is used as a mild and selective method, economically viable application of this method on similarly soluble oils from microalgae requires, in most cases, much higher pressure. This paper presents and verifies hypothesis that this difference is caused by high adsorption capacity of microalgae. Under the pressures usually applied in supercritical fluid extraction from plants, microalgae bind a large fraction of the extracted oil, while under extremely high CO2 pressures their adsorption capacity diminishes and the extraction rate depends on oil solubility in supercritical CO2. A mathematical model for the extraction from microalgae was derived and applied to literature data on the extraction kinetics in order to determine model parameters.

Supercritical fluid extraction of silicone oil from uranate microspheres prepared by sol-gel process

International Nuclear Information System (INIS)

Kumar, R.; Venkatakrishnan, R.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R.

2005-01-01

Supercritical fluid extraction of silicone oil from urania microspheres prepared through sol-gel route was investigated. The influence of pressure, temperature, and flow rate on the extraction efficiency was studied. Experimental conditions were optimised for the complete removal of silicone oil from urania microspheres. (author)

Application of FTA technology to extraction of sperm DNA from mixed body fluids containing semen.

Science.gov (United States)

Fujita, Yoshihiko; Kubo, Shin-ichi

2006-01-01

FTA technology is a novel method designed to simplify the collection, shipment, archiving and purification of nucleic acids from a wide variety of biological sources. In this study, we report a rapid and simple method of extracting DNA from sperm when body fluids mixed with semen were collected using FTA cards. After proteinase K digestion of the sperm and body fluid mixture, the washed pellet suspension as the sperm fraction and the concentrated supernatant as the epithelial cell fraction were respectively applied to FTA cards containing DTT. The FTA cards were dried, then directly added to a polymerase chain reaction (PCR) mix and processed by PCR. The time required from separation of the mixed fluid into sperm and epithelial origin DNA extractions was only about 2.5-3h. Furthermore, the procedure was extremely simple. It is considered that our designed DNA extraction procedure using an FTA card is available for application to routine work.

Modeling the Supercritical Fluid Extraction of Essential Oils from Plant Materials

Czech Academy of Sciences Publication Activity Database

Sovová, Helena

2012-01-01

Roč. 1250, SI (2012), s. 27-33 ISSN 0021-9673 R&D Projects: GA TA ČR TA01010578 Institutional support: RVO:67985858 Keywords : supercritical fluid extraction * essential oils * model for kinetics Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 4.612, year: 2012

Supercritical Fluid Extraction of Minor Components of Vegetable Oils: beta-Sitosterol

Czech Academy of Sciences Publication Activity Database

Sovová, Helena; Galushko, A.A.; Stateva, R.P.; Rochová, Kristina; Sajfrtová, Marie; Bártlová, Milena

2010-01-01

Roč. 101, č. 2 (2010), s. 201-209 ISSN 0260-8774 R&D Projects: GA MŠk 2B06024 Institutional research plan: CEZ:AV0Z40720504 Keywords : supercritical fluid extraction * sea buckthorn oil * beta-sitosterol Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 2.168, year: 2010

Developing novel one-step processes for obtaining food-grade O/W emulsions from pressurized fluid extracts: processes description, state of the art and perspectives

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Diego Tresinari SANTOS

2015-01-01

Full Text Available AbstractIn this work, a novel on-line process for production of food-grade emulsions containing oily extracts, i.e. oil-in-water (O/W emulsions, in only one step is presented. This process has been called ESFE, Emulsions from Supercritical Fluid Extraction. With this process, emulsions containing supercritical fluid extracts can be obtained directly from plant materials. The aim in the conception of this process is to propose a new rapid way to obtain emulsions from supercritical fluid extracts. Nowadays the conventional emulsion formulation method is a two-step procedure, i.e. first supercritical fluid extraction for obtaining an extract; secondly emulsion formulation using another device. Other variation of the process was tested and successfully validated originating a new acronymed process: EPFE (Emulsions from Pressurized Fluid Extractions. Both processes exploit the supercritical CO2-essential oils miscibility, in addition, EPFE process exploits the emulsification properties of saponin-rich pressurized aqueous plant extracts. The feasibility of this latter process was demonstrated using Pfaffia glomerata roots as source of saponin-rich extract, water as extracting solvent and clove essential oil, directly extracted using supercritical CO2, as a model dispersed phase. In addition, examples of pressurized fluid-based coupled processes applied for adding value to food bioactive compounds developed in the past five years are reviewed.

Steps of Supercritical Fluid Extraction of Natural Products and Their Characteristic Times

Czech Academy of Sciences Publication Activity Database

Sovová, Helena

2012-01-01

Roč. 66, SI (2012), s. 73-79 ISSN 0896-8446 R&D Projects: GA MŠk 2B06049 Institutional support: RVO:67985858 Keywords : supercritical fluid extraction * vegetable oils * essential oils Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 2.732, year: 2012

Experimental results for the extraction of essential oil from Lippia sidoides cham. using pressurized carbon dioxide

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Sousa EMBD.

2002-01-01

Full Text Available The odoriferous species Lippia sidoides Cham. is abundant in the Brazilian Northeast. Its essential oil possesses antiseptic activity due to the presence of thymol. In this work, thermodynamic and kinetic data were experimentally determined for the CO2 + L. sidoides system. Solubility was determined using the dynamic method at pressures of 66.7 and 78.5 bar and temperatures of 283.15, 288.15, 293.15, 295.15, and 298.15 K. SFE kinetic data were obtained at 288.15 K and 66.7 bar. The composition of the multicomponent solute mixture was determined by GC-MS and compared to the composition of both the volatile oil obtained by steam distillation and the oleoresin obtained using ethanol. The SFE process yield was higher than the yield of either the steam distillation or the ethanol extraction. The solubilities were correlated using the Peng-Robinson equation of state with one binary interaction parameter for the attractive term, considering the essential oil as a pseudo-component. Sovová?s model quantitatively described the overall extraction curve.

Evaluation of supercritical extracts of algae as biostimulants of plant growth in field trials

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Izabela Michalak

2016-10-01

Full Text Available The aim of the field trials was to determine the influence of supercritical algal extracts on the growth and development of winter wheat (variety Akteur. As a raw material for the supercritical fluid extraction (SFE, the biomass of microalga Spirulina plantensis, brown seaweed – Ascophyllum nodosum and Baltic green macroalgae was used. Forthial and Asahi SL constituted the reference products. It was found that the tested biostimulants did not influence statistically significantly the plant height, length of ear and shank length. The ear number per square meter was the highest in the group where the Baltic macroalgae extract was applied in the dose 1.0 L/ha (statistically significant differences. Number of grains in ear (statistically significant differences and shank length was the highest in the group treated with Spirulina at the dose 1.5 L/ha. In the group with Ascophyllum at the dose 1.0 L/ha, the highest length of ear was observed. The yield was comparable in all the experimental groups (lack of statistically significant differences.Among the tested supercritical extracts, the best results were obtained for Spirulina (1.5 L/ha. The mass of 1000 grains was the highest for extract from Baltic macroalgae and was 3.5% higher than for Asahi, 4.0% higher than for Forthial and 18.5% higher than for the control group (statistically significant differences. Future work is needed to fully characterize the chemical composition of the applied algal extracts. A special attention should be paid to the extracts obtained from Baltic algae because they are inexpensive source of naturally occurring bioactive compounds, which can be used in sustainable agriculture and horticulture.

Optimization of conditions for supercritical fluid extraction of flavonoids from hops (Humulus lupulus L.)*

Science.gov (United States)

He, Guo-qing; Xiong, Hao-ping; Chen, Qi-he; Ruan, Hui; Wang, Zhao-yue; Traoré, Lonseny

2005-01-01

Waste hops are good sources of flavonoids. Extraction of flavonoids from waste hops (SC-CO2 extracted hops) using supercritical fluids technology was investigated. Various temperatures, pressures and concentrations of ethanol (modifier) and the ratio (w/w) of solvent to material were tested in this study. The results of single factor and orthogonal experiments showed that at 50 °C, 25 MPa, the ratio of solvent to material (50%), ethanol concentration (80%) resulted in maximum extraction yield flavonoids (7.8 mg/g). HPLC-MS analysis of the extracts indicated that flavonoids obtained were xanthohumol, the principal prenylflavonoid in hops. PMID:16187413

Immunomodulatory effects of supercritical fluid CO2 extracts from freeze-dried powder of Tenebrio molitor larvae (yellow mealworm

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QingFeng TANG

2016-01-01

Full Text Available Abstract In order to take full advantage of Tenebrio molitor larvae (yellow mealworm resources, the supercritical CO2 fluid freeze-dried powder of T. molitor larvae (fdTML extraction on the immune systems of mice was carried out. The results about the effects of supercritical CO2 fluid fdTML extraction on carbon expurgation and phagocytosis of peritoneal macrophages experiments of mice indicated that the fdTML extraction enhanced observably carbon expurgatory index, phagocytic rate and phagocytic index. The fdTML extraction could stimulate response of delayed hypersensitivity. The proliferation of ConA-induced mitogenic reponse for spleen lymphocyte was also increased. The amount of hemolytic antibody in mice serum increased compared with those of the control group mice. The half of hemolysis values in serum of treated mice increased compared to the control group. Furthermore, serum NO content in all treatment groups was higher than that of the control group whereas acid phosphatase and alkaline phosphatase activity was only significantly higher relative to the control group. Our findings suggest that supercritical CO2 fluid the fdTML extraction has potential as a health food supplement.

Influence of Stacking Fault Energy (SFE) on the deformation mode of stainless steels

International Nuclear Information System (INIS)

Li, X.; Van Renterghem, W.; Al Mazouzi, A.

2008-01-01

The sensibility to irradiation-assisted stress corrosion cracking (IASCC) of stainless steels in light water reactor (LWR) can be caused by the localisation of deformation that takes place in these materials. Dislocation channelling and twinning modes of deformation can induce localised plasticity leading to failure. Stacking fault energy (SFE) plays an important role in every process of plastic deformation behaviour, especially in twinning and dislocation channelling. In order to correlate localised deformation with stacking fault energy, this parameter has been experimentally determined by transmission electron microscope (TEM) using both dislocation node and multiple ribbons methods after compression in three different model alloys. Detailed deformation behaviour of three fabricated alloys with different stacking fault energy before and after tensile tests at temperatures from -150 deg C to 300 deg C, will be shown and discussed based on mechanical test and TEM observation. (authors)

Estrazione di composti biologicamente attivi da piante della Sardegna

OpenAIRE

Falconieri, Danilo

2012-01-01

This research work has been focused on the supercritical fluid extraction and characterization of volatile oils having interesting biological activities, possibly susceptible of therapeutic applications. A further aim of this work was to separate biologically active molecules and nutraceuticals by means of SFE at high pressure. The investigated species have been selected on the basis of ethnobotanic information regarding, in particular, species endemic of Sardinia or that can be easily cul...

A rapid supercritical fluid extraction method for the qualitative detection of 2-alkylcyclobutanones in gamma-irradiated fresh and sea water fish

International Nuclear Information System (INIS)

Tewfik, I.H.; Ismail, H.M.; Sumar, S.

1999-01-01

2-Alkylcyclobutanones are routinely used as chemical markers for irradiated foods containing lipids. However, current extraction procedures (soxhlet-Florisil chromatography) for the isolation of these markers involve a long and tedious clean-up regime prior to GC-MS identification. A simple and rapid method for the isolation of these markers using carbon dioxide as a super critical fluid is described for low lipid content fish samples (fresh and sea water) irradiated up to 8kGy. The presence of 2-dodecylcyclobutanone (2-DCB), a radiolytic marker, was confirmed in all irradiated fish samples at all doses. This was a clear indication that the fish samples had been irradiated and that both methods of isolation (florisil and supercritical fluid extraction) were capable of qualitatively extracting this marker. Supercritical fluid extraction is proposed as an alternative extraction procedure to the florisil chromatography method currently in use and has the added advantage of a considerably shorter extraction time

Identification and isolation of the cyclooxygenase-2 inhibitory principle in Isatis tinctoria.

Science.gov (United States)

Danz, H; Stoyanova, S; Wippich, P; Brattström, A; Hamburger, M

2001-07-01

Various extracts prepared from the traditional dye and medicinal plant Isatis tinctoria L. were submitted to a broad in vitro screening against 16 anti-inflammatory targets. Dichloromethane (DCM) extracts from dried leaves showed a marked cyclooxygenase (COX) inhibitory activity with a preferential effect on COX-2 catalysed prostaglandin synthesis. A supercritical fluid extraction (SFE) procedure employing CO2-modifier mixtures was developed by which the bioactivity profile and chromatographic fingerprint of the DCM extract could be reproduced. High-resolution activity directed on-line identification of the COX-2 inhibitory principle, using a combination of LC-DAD-MS with a microtitre-based bioassay, led to the identification of tryptanthrin (1) as the constituent responsible for essentially all COX-2 inhibitory activity in the crude extract. Following on-line identification, 1 was isolated at preparative scale and its structure confirmed by comparison with synthetic tryptanthrin. In an assay with lipopolysaccharide stimulated Mono Mac 6 cells, tryptanthrin (1) was of comparable potency (IC50 = 64 nM) than the preferential COX-2 inhibitors nimesulide (IC50 = 39 nM) and NS 398 (IC50 = 2 nM). The SFE extract and 1 showed no cytotoxicity in Mono Mac 6 and RAW 264.7 cells when tested at 100 microg/ml and 10 microM, respectively.

Offline combination of pressurized fluid extraction and electron paramagnetic resonance spectroscopy for antioxidant activity of grape skin extracts assessment

Czech Academy of Sciences Publication Activity Database

Polovka, M.; Šťavíková, Lenka; Hohnová, Barbora; Karásek, Pavel; Roth, Michal

2010-01-01

Roč. 1217, č. 51 (2010), s. 7990-8000 ISSN 0021-9673 R&D Projects: GA ČR GA203/08/1536; GA MŠk LC06023 Institutional research plan: CEZ:AV0Z40310501 Keywords : pressurized fluid extraction * electron paramagnetic resonance spectroscopy * antioxidant activity Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.194, year: 2010

Developing novel one-step processes for obtaining food-grade O/W emulsions from pressurized fluid extracts: processes description, state of the art and perspectives

OpenAIRE

SANTOS, Diego Tresinari; MEIRELES, Maria Angela de Almeida

2015-01-01

Abstract In this work, a novel on-line process for production of food-grade emulsions containing oily extracts, i.e. oil-in-water (O/W) emulsions, in only one step is presented. This process has been called ESFE, Emulsions from Supercritical Fluid Extraction. With this process, emulsions containing supercritical fluid extracts can be obtained directly from plant materials. The aim in the conception of this process is to propose a new rapid way to obtain emulsions from supercritical fluid extr...

Ancient microbes from halite fluid inclusions: optimized surface sterilization and DNA extraction.

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Krithivasan Sankaranarayanan

Full Text Available Fluid inclusions in evaporite minerals (halite, gypsum, etc. potentially preserve genetic records of microbial diversity and changing environmental conditions of Earth's hydrosphere for nearly one billion years. Here we describe a robust protocol for surface sterilization and retrieval of DNA from fluid inclusions in halite that, unlike previously published methods, guarantees removal of potentially contaminating surface-bound DNA. The protocol involves microscopic visualization of cell structures, deliberate surface contamination followed by surface sterilization with acid and bleach washes, and DNA extraction using Amicon centrifugal filters. Methods were verified on halite crystals of four different ages from Saline Valley, California (modern, 36 ka, 64 ka, and 150 ka, with retrieval of algal and archaeal DNA, and characterization of the algal community using ITS1 sequences. The protocol we developed opens up new avenues for study of ancient microbial ecosystems in fluid inclusions, understanding microbial evolution across geological time, and investigating the antiquity of life on earth and other parts of the solar system.

Ancient microbes from halite fluid inclusions: optimized surface sterilization and DNA extraction.

Science.gov (United States)

Sankaranarayanan, Krithivasan; Timofeeff, Michael N; Spathis, Rita; Lowenstein, Tim K; Lum, J Koji

2011-01-01

Fluid inclusions in evaporite minerals (halite, gypsum, etc.) potentially preserve genetic records of microbial diversity and changing environmental conditions of Earth's hydrosphere for nearly one billion years. Here we describe a robust protocol for surface sterilization and retrieval of DNA from fluid inclusions in halite that, unlike previously published methods, guarantees removal of potentially contaminating surface-bound DNA. The protocol involves microscopic visualization of cell structures, deliberate surface contamination followed by surface sterilization with acid and bleach washes, and DNA extraction using Amicon centrifugal filters. Methods were verified on halite crystals of four different ages from Saline Valley, California (modern, 36 ka, 64 ka, and 150 ka), with retrieval of algal and archaeal DNA, and characterization of the algal community using ITS1 sequences. The protocol we developed opens up new avenues for study of ancient microbial ecosystems in fluid inclusions, understanding microbial evolution across geological time, and investigating the antiquity of life on earth and other parts of the solar system.

Determination of lycopene in food by on-line SFE-LC eliminating its degradation during the analytical procedure

Czech Academy of Sciences Publication Activity Database

Pól, Jaroslav; Hyötyläinen, T.; Ranta-Aho, O.; Riekkola, M. L.

2005-01-01

Roč. 99, S (2005), s251 ISSN 0009-2770. [Meeting on Chemistry and Life /3./. 20.09.2005-22.09.2005, Brno] R&D Projects: GA AV ČR KJB4031405 Keywords : liquid chromatography * supercritical fluid extraction * antioxidant Subject RIV: CB - Analytical Chemistry, Separation

Detection of some irradiated foods

International Nuclear Information System (INIS)

NASR, E.H.A

2009-01-01

This study was performed to investigate the possibility of using two rapid methods namely Supercritical Fluid Extraction (SFE) and Direct Solvent Extraction (DSE) methods for extraction and isolation of 2-dodecylcyclobutanone (2-DCB) followed by detecting this chemical marker by Gas chromatography technique and used this marker for identification of irradiated some foods containing fat (beef meat, chicken, camembert cheese and avocado) post irradiation, during cold and frozen storage. Consequently, this investigation was designed to study the following main points:- 1- The possibility of applying SFE-GC and DSE-GC rapid methods for the detection of 2-DCB from irradiated food containing fat (beef meat, chicken, camembert cheese and avocado fruits) under investigation.2-Studies the effect of gamma irradiation doses on the concentration of 2-DCB chemical marker post irradiation and during frozen storage at -18 degree C of chicken and beef meats for 12 months.3-Studies the effect of gamma irradiation doses on the concentration of 2-DCB chemical marker post irradiation and during cold storage at 4±1 degree C of camembert cheese and avocado fruits for 20 days.

Broken-and-Intact Cell Model for Supercritical Fluid Extraction: Its Origin and Limits.

Czech Academy of Sciences Publication Activity Database

Sovová, Helena

2017-01-01

Roč. 129, SI (2017), s. 3-8 ISSN 0896-8446. [Iberoamerican Conference on Supercritical Fluid s ProSCiba 2016 /4./. Vina del Mar, 28.03.2016-01.04.2016] Institutional support: RVO:67985858 Keywords : modelling * extraction kinetics * supercritical CO2 Subject RIV: CI - Industrial Chemistry, Chemical Engineering OBOR OECD: Chemical process engineering Impact factor: 2.991, year: 2016

Broken-and-Intact Cell Model for Supercritical Fluid Extraction: Its Origin and Limits.

Czech Academy of Sciences Publication Activity Database

Sovová, Helena

2017-01-01

Roč. 129, SI (2017), s. 3-8 ISSN 0896-8446. [Iberoamerican Conference on Supercritical Fluids ProSCiba 2016 /4./. Vina del Mar, 28.03.2016-01.04.2016] Institutional support: RVO:67985858 Keywords : modelling * extraction kinetics * supercritical CO2 Subject RIV: CI - Industrial Chemistry, Chemical Engineering OBOR OECD: Chemical process engineering Impact factor: 2.991, year: 2016

A Novel Model for Multicomponent Supercritical Fluid Extraction and its Application to Ruta graveolens.

Czech Academy of Sciences Publication Activity Database

Sovová, Helena; Sajfrtová, Marie; Stateva, R.P.

2017-01-01

Roč. 120, Part 1 (2017), s. 102-112 ISSN 0896-8446 R&D Projects: GA MŠk 2B06049 Institutional support: RVO:67985858 Keywords : supercritical fluid extraction * multicomponent equilibrium * kinetics Subject RIV: CI - Industrial Chemistry, Chemical Engineering OBOR OECD: Chemical process engineering Impact factor: 2.991, year: 2016

using Supercritical Fluid Extraction

African Journals Online (AJOL)

Methods: Supercritical CO2 extraction technology was adopted in this experiment to study the process of extraction of volatile oil from Polygonatum odoratum while gas chromatograph-mass spectrometer ..... Saponin rich fractions from.

The uranium waste fluid processing examination by liquid and liquid extraction method using the emulsion flow method

International Nuclear Information System (INIS)

Kanda, Nobuhiro; Daiten, Masaki; Endo, Yuji; Yoshida, Hideaki; Mita, Yutaka; Naganawa, Hirochika; Nagano, Tetsushi; Yanase, Nobuyuki

2015-03-01

Spent centrifuges which had used for the development of the uranium enrichment technology are stored in the uranium enrichment facility located in Ningyo-toge Environmental Center, Japan Atomic Energy Agency (JAEA). Our technology of the centrifugal machine processing are supposed to separate the radioactive material adhered on surface of inner parts of centrifuges by the wet way decontamination method using the ultrasonic bath filled dilute sulfuric acid and water, and it is generated the neutralization sediment (sludge) by the processing of the radioactive waste fluid with the decontamination. JAEA had been considering the applicability of a streamlining and reduction of the processing of the sludge by decreases radioactive concentration including the sludge through the removes uranium from the radioactive waste fluid. As part of considerations, JAEA have been promoting technological developments of the uranium extraction separation using The Emulsion Flow Extraction Method (a theory propounded by JAEA-Nuclear Science and Engineering Center) in close coordination and cooperation between with JAEA-Nuclear Science and Engineering Center and Ningyo-toge Environmental Center from 2007 fiscal year. This report describes the outline of the application test using actual waste fluid of dilute sulfuric acid and water by developed the examination system introducing the emulsion flow extraction method. (author)

Chemical Composition of Essential Oils from Zanthoxylum bungeanum Maxim. and Their Bioactivities against Lasioderma serricorne.

Science.gov (United States)

Zhang, Wen-Juan; Guo, Shan-Shan; You, Chun-Xue; Geng, Zhu-Feng; Liang, Jun-Yu; Deng, Zhi-Wei; Wang, Cheng-Fang; Du, Shu-Shan; Wang, Yong-Yan

2016-10-01

Two essential oil samples were obtained from the pericarp of Zanthoxylum bungeanum with the methods of hydrodistillation (HD) and supercritical fluid CO 2 extraction (SFE), their chemical components were identified, and their bioactivities against Lasioderma serricorne adults were evaluated. In the process of testing, the two samples showed significant bioactivities against Lasioderma serricorne adults. For an example, the SFE-sample expressed relatively stronger fumigant toxicity on Lasioderma serricorne adults (LC 50 = 3.99 μg/mL air) than that of the HD-sample (LC 50 = 12.54 μg/mL air). According to GC-MS analysis, the chemical components between two samples were different. The major chemical components for HD included linalool (25.99%), limonene (19.34%), linalyl anthranilate (12.22%), 4-terpinenol (10.49%), eucalyptol (6.53%) and α-terpineol (5.02%), while for SFE included nonanoic acid (21.43%), γ-terpinene (14.51%), eucalyptol (13.45%), α-terpineol (5.83%) and caryophyllene oxide (5.48%). The results showed that different chemical components result in different bioactivities. This work provides theoretical basis for traditional Chinese concept of antagonistic storage, and it also provides important information for the development and comprehensive utilization of Zanthoxylum bungeanum.

Application of supercritical and subcritical fluids for the extraction of hazardous materials from soil

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Skorupan Dara

2002-01-01

Full Text Available Subcritical and supercritical extractions are novel, non destructive techniques which can be applied for the removal of hazardous compounds from contaminated soil without any changes of the soil composition and structure. The aim of the presented review paper is to give information on up-to day results of this method commonly applied by several institutions worldwide. Interest in the application of SC CO2 has been more expressed in the last two decades, which may be related to its favorable characteristics (non-toxic, non-flammable, increase diffusion into small pores, low viscosity under SC conditions, low price and others. However, interest in wet oxidation (WO and especially in SCWO (the application of water under supercritical conditions with air has also increased in the last few years. Interest in H2O as a SC fluid, as well as in extraction with water under subcritical conditions may also be related to specific characteristics and the enhanced rate of extraction. Moreover, the solubility of some specific compounds present in soil can be easily changed by adjusting the pressure and temperature of extraction. The high price of the units designed to operate safely at a pressure and temperature much higher than the a critical one of the applied fluids is the main reason why, at present, there is no more broader application of such techniques for the removal hazardous materials from contaminated soil. In the present paper, among many literature citations and their overall review, some specific details related to the development of specific analytical methods under SC conditions are also considered.

Measurement of polychlorinated biphenyls in solid waste such as transformer insulation paper by supercritical fluid extraction and gas chromatography electron capture detection.

Science.gov (United States)

Chikushi, Hiroaki; Fujii, Yuka; Toda, Kei

2012-09-21

In this work, a method for measuring polychlorinated biphenyls (PCBs) in contaminated solid waste was investigated. This waste includes paper that is used in electric transformers to insulate electric components. The PCBs in paper sample were extracted by supercritical fluid extraction and analyzed by gas chromatography-electron capture detection. The recoveries with this method (84-101%) were much higher than those with conventional water extraction (0.08-14%), and were comparable to those with conventional organic solvent extraction. Limit of detection was 0.0074 mg kg(-1) and measurable up to 2.5 mg kg(-1) for 0.5 g of paper sample. Data for real insulation paper by the proposed method agreed well with those by the conventional organic solvent extraction. Extraction from wood and concrete was also investigated and good performance was obtained as well as for paper samples. The supercritical fluid extraction is simpler, faster, and greener than conventional organic solvent extraction. Copyright © 2012 Elsevier B.V. All rights reserved.

Supercritical Fluid Extraction of Lovastatin from the Wheat Bran Obtained after Solid-State Fermentation

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Ruchir C. Pansuriya

2009-01-01

Full Text Available The objective of the present work is to extract lovastatin with minimum impurity by using supercritical carbon dioxide (SC-CO2. A strain of Aspergillus terreus UV 1617 was used to produce lovastatin by solid-state fermentation (SSF on wheat bran as a solid substrate. Extraction of lovastatin and its hydroxy acid form was initially carried out using organic solvents. Among the different screened solvents, acetonitrile was found to be the most efficient. SC-CO2 was used for extraction of lovastatin from the dry fermented matter. The effect of supercritical extraction parameters such as the amount of an in situ pretreatment solvent, temperature, pressure, flow rate and contact time were investigated. The maximum recovery of lovastatin was obtained with 5 mL of methanol as an in situ pretreatment solvent for 1.5 g of solid matrix, flow rate of the supercritical solvent 2 L/min, temperature 50 °C, and contact time 155 min at a pressure 300 bar. The lovastatin extract obtained after optimizing the conditions of supercritical fluid extraction was found to have 5-fold more HPLC purity than the organic solvent extract.

Supercritical fluid extraction-gas chromatography of volatile organic compounds (VOC) from Tenax devices. Final report, November 1985-September 1986

International Nuclear Information System (INIS)

Wright, B.W.; Kopriva, A.J.; Smith, R.D.

1987-11-01

This report describes the development and evaluation of on-line supercritical-fluid extraction - gas-chromatography instrumentation and methodology for the analysis of volatile organic compounds (VOC) from adsorbent sampling devices. Supercritical fluid extraction offers potential advantages for the removal and transport of organic components from adsorbent matrices including rapid and efficient extraction at mild temperatures. Extraction at mild temperatures eliminates potential problems such as analyte decomposition that can be encountered with the high temperatures needed for thermal desorption analysis. Since a major objective of the study was to develop viable instrumentation and methodology, a relatively detailed description of the instrumentation design requirements and present limitations are discussed. The results of several series of methodology validation studies are also presented. These studies included recovery studies of model VOC spiked on three types of Tenax sampling devices including authentic actively pumped (VOST) and passive (EPA) devices. Replicate devices spiked in an exposure chamber were also subjected to parallel analyses using the new methodology and traditional thermal-desorption gas chromatography

Evaluation of various Crown ethers for the supercritical fluid extraction of uranium from nitric acid medium

International Nuclear Information System (INIS)

Kumar, Pradeep; Rao, Ankita; Ramakumar, K.L.

2009-01-01

Various crowns have been evaluated for supercritical fluid extraction of uranium from nitric acid medium employing HPFOA as counter ion. Uranium extraction efficiency was found to be influenced by cavity size of crown ether and nature of substituents. Complexation tendency of UO 2 2+ increases with increasing cavity size of crown ether. Electron withdrawing substituents decreased the extraction efficiency which could be attributed to decrease in the basicity of four oxygen atoms and hence their bonding ability. Whereas electron donating substituents increased the efficiency due to increases in basicity of oxygen atoms and hence in increase in bonding ability. (author)

Recovery of Oil with Unsaturated Fatty Acids and Polyphenols from Chaenomelessinensis (Thouin Koehne: Process Optimization of Pilot-Scale Subcritical Fluid Assisted Extraction

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Zhenzhou Zhu

2017-10-01

Full Text Available The potential effects of three modern extraction technologies (cold-pressing, microwaves and subcritical fluids on the recovery of oil from Chaenomelessinensis (Thouin Koehne seeds have been evaluated and compared to those of conventional chemical extraction methods (Soxhlet extraction. This oil contains unsaturated fatty acids and polyphenols. Subcritical fluid extraction (SbFE provided the highest yield—25.79 g oil/100 g dry seeds—of the three methods. Moreover, the fatty acid composition in the oil samples was analysed using gas chromatography–mass spectrometry. This analysis showed that the percentages of monounsaturated (46.61%, and polyunsaturated fatty acids (42.14%, after applying SbFE were higher than those obtained by Soxhlet, cold-pressing or microwave-assisted extraction. In addition, the oil obtained under optimized SbFE conditions (35 min extraction at 35 °C with four extraction cycles, showed significant polyphenol (527.36 mg GAE/kg oil, and flavonoid (15.32 mg RE/kg oil, content, had a good appearance and was of high quality.

Recovery of Oil with Unsaturated Fatty Acids and Polyphenols from Chaenomelessinensis (Thouin) Koehne: Process Optimization of Pilot-Scale Subcritical Fluid Assisted Extraction.

Science.gov (United States)

Zhu, Zhenzhou; Zhang, Rui; Zhan, Shaoying; He, Jingren; Barba, Francisco J; Cravotto, Giancarlo; Wu, Weizhong; Li, Shuyi

2017-10-22

The potential effects of three modern extraction technologies (cold-pressing, microwaves and subcritical fluids) on the recovery of oil from Chaenomelessinensis (Thouin) Koehne seeds have been evaluated and compared to those of conventional chemical extraction methods (Soxhlet extraction). This oil contains unsaturated fatty acids and polyphenols. Subcritical fluid extraction (SbFE) provided the highest yield-25.79 g oil/100 g dry seeds-of the three methods. Moreover, the fatty acid composition in the oil samples was analysed using gas chromatography-mass spectrometry. This analysis showed that the percentages of monounsaturated (46.61%), and polyunsaturated fatty acids (42.14%), after applying SbFE were higher than those obtained by Soxhlet, cold-pressing or microwave-assisted extraction. In addition, the oil obtained under optimized SbFE conditions (35 min extraction at 35 °C with four extraction cycles), showed significant polyphenol (527.36 mg GAE/kg oil), and flavonoid (15.32 mg RE/kg oil), content, had a good appearance and was of high quality.

Minimally-invasive, microneedle-array extraction of interstitial fluid for comprehensive biomedical applications: transcriptomics, proteomics, metabolomics, exosome research, and biomarker identification.

Science.gov (United States)

Taylor, Robert M; Miller, Philip R; Ebrahimi, Parwana; Polsky, Ronen; Baca, Justin T

2018-01-01

Interstitial fluid (ISF) has recently garnered interest as a biological fluid that could be used as an alternate to blood for biomedical applications, diagnosis, and therapy. ISF extraction techniques are promising because they are less invasive and less painful than venipuncture. ISF is an alternative, incompletely characterized source of physiological data. Here, we describe a novel method of ISF extraction in rats, using microneedle arrays, which provides volumes of ISF that are sufficient for downstream analysis techniques such as proteomics, genomics, and extracellular vesicle purification and analysis. This method is potentially less invasive than previously reported techniques. The limited invasiveness and larger volumes of extracted ISF afforded by this microneedle-assisted ISF extraction method provide a technique that is less stressful and more humane to laboratory animals, while also allowing for a reduction in the numbers of animals needed to acquire sufficient volumes of ISF for biomedical analysis and application.

Ketosteroid Standardized Cissus quadrangularis L. Extract and its Anabolic Activity: Time to Look Beyond Ketosteroid?

Science.gov (United States)

Jadhav, Atul N; Rafiq, Mohammed; Devanathan, Rajendran; Azeemuddin, Mohammed; Anturlikar, Suryakanth D; Ahmed, Akhil; Sundaram, Ramchandran; Babu, U V; Paramesh, Rangesh

2016-05-01

active principles from CQ L. Abbreviations used: CQ: Cissus quadrangularis, ORX: Orchidectomized, AE: Aqueous extract, EE: Ethyl acetate extract, SFE: Supercritical fluid extract.

Bioavailability of a new iron source used in the fortification of fluid cow's milk. Importance of its use in children after their nursing

International Nuclear Information System (INIS)

Boccio, J.; Zubillaga, M.; Lysionek, A.; Caro, R.; Weill, R.

2000-01-01

Iron deficiency anemia is the most prevalent nutritional deficiency in Argentina, particularly among infants under 2 years old. At this age the most efficient way to prevent it is through the daily intake of bioavailable iron in weaning foods. Fluid cow's milk is the most popular weaning food in our country. Nowadays, it is possible to fortify this kind of food with 15 mg of iron per liter by a new technological procedure in which ferrous sulfate is microencapsulated with phospholipids. Therefore at the beginning we studied the absorption of this novel iron fortification compound called SFE-171 in fluid cow's milk in animal models as well as human beings. In both cases we found that the absorption values obtained for iron from SFE-171 were 2 folds higher with regard to the values obtained in the case of ferrous sulfate in cow's milk. In order to determine the importance that this fortified milk has in children iron balance after their nursing, we have to evaluate the iron intake by children near the weaning period. In this way we standardized the methodology to determine the iron content in breast milk and the method to determine the breast milk intake. The first part was performed and the iron concentration in breast milk was 0.56±0.08 μg/mL, the second part was started but the experimental phase has to be done. After that we have to determine the effect of iron-fortified cow's milk has on children iron status. Preliminary results suggest that the iron fortified fluid cow's milk with this source of iron produce an adequate iron balance in weaning children. (author)

Bioavailability of a new iron source used in the fortification of fluid cow's milk. Importance of its use in children after their nursing

Energy Technology Data Exchange (ETDEWEB)

Boccio, J; Zubillaga, M; Lysionek, A; Caro, R [Laboratorio de Radioisotopos, Facultad de Farmacia y Bioquimica, Universidad de Buenos Aires, Buenos Aires (Argentina); Weill, R [Departamento de Industrias Agrarias, Universidad de Moron, Buenos Aires (Argentina)

2000-07-01

Iron deficiency anemia is the most prevalent nutritional deficiency in Argentina, particularly among infants under 2 years old. At this age the most efficient way to prevent it is through the daily intake of bioavailable iron in weaning foods. Fluid cow's milk is the most popular weaning food in our country. Nowadays, it is possible to fortify this kind of food with 15 mg of iron per liter by a new technological procedure in which ferrous sulfate is microencapsulated with phospholipids. Therefore at the beginning we studied the absorption of this novel iron fortification compound called SFE-171 in fluid cow's milk in animal models as well as human beings. In both cases we found that the absorption values obtained for iron from SFE-171 were 2 folds higher with regard to the values obtained in the case of ferrous sulfate in cow's milk. In order to determine the importance that this fortified milk has in children iron balance after their nursing, we have to evaluate the iron intake by children near the weaning period. In this way we standardized the methodology to determine the iron content in breast milk and the method to determine the breast milk intake. The first part was performed and the iron concentration in breast milk was 0.56{+-}0.08 {mu}g/mL, the second part was started but the experimental phase has to be done. After that we have to determine the effect of iron-fortified cow's milk has on children iron status. Preliminary results suggest that the iron fortified fluid cow's milk with this source of iron produce an adequate iron balance in weaning children. (author)

An Analytical Model for Assessing Stability of Pre-Existing Faults in Caprock Caused by Fluid Injection and Extraction in a Reservoir

Science.gov (United States)

Wang, Lei; Bai, Bing; Li, Xiaochun; Liu, Mingze; Wu, Haiqing; Hu, Shaobin

2016-07-01

Induced seismicity and fault reactivation associated with fluid injection and depletion were reported in hydrocarbon, geothermal, and waste fluid injection fields worldwide. Here, we establish an analytical model to assess fault reactivation surrounding a reservoir during fluid injection and extraction that considers the stress concentrations at the fault tips and the effects of fault length. In this model, induced stress analysis in a full-space under the plane strain condition is implemented based on Eshelby's theory of inclusions in terms of a homogeneous, isotropic, and poroelastic medium. The stress intensity factor concept in linear elastic fracture mechanics is adopted as an instability criterion for pre-existing faults in surrounding rocks. To characterize the fault reactivation caused by fluid injection and extraction, we define a new index, the "fault reactivation factor" η, which can be interpreted as an index of fault stability in response to fluid pressure changes per unit within a reservoir resulting from injection or extraction. The critical fluid pressure change within a reservoir is also determined by the superposition principle using the in situ stress surrounding a fault. Our parameter sensitivity analyses show that the fault reactivation tendency is strongly sensitive to fault location, fault length, fault dip angle, and Poisson's ratio of the surrounding rock. Our case study demonstrates that the proposed model focuses on the mechanical behavior of the whole fault, unlike the conventional methodologies. The proposed method can be applied to engineering cases related to injection and depletion within a reservoir owing to its efficient computational codes implementation.

Extraction and isolation of dictamnine, obacunone and fraxinellone from Dictamnus dasycarpus Turcz. by supercritical fluid extraction and high-speed counter-current chromatography

International Nuclear Information System (INIS)

Wang, Daijie; Lin, Yunliang; Lin, Xiaojing; Geng, Yanling; Wang, Xiao; Zhang, Jinjie; Qiu, Jiying

2012-01-01

Supercritical fluid extraction was used to extract active compounds from the Chinese traditional medicinal D. dasycarpus under the pressure of 30 MPa and temperature of 45 degree C. Further separation and purification was established by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:0.8:1.3:0.9, volume ratio). The separation yielded a total of 47 mg of dictamnine, 24 mg of obacunone and 83 mg of fraxinellone from 1.0 g of the crude extract in one step separation with the purity of 99.2, 98.4 and 99.0%, respectively, as determined by HPLC. The chemical structures of these compounds were identified by ESI-MS, IR, 1H-NMR and 13 C-NMR. (author)

Extraction and isolation of dictamnine, obacunone and fraxinellone from Dictamnus dasycarpus Turcz. by supercritical fluid extraction and high-speed counter-current chromatography

Energy Technology Data Exchange (ETDEWEB)

Wang, Daijie; Lin, Yunliang; Lin, Xiaojing; Geng, Yanling; Wang, Xiao, E-mail: wxjn1998@126.com [Process Control Research Center of TCM. Shandong Academy of Sciences. Shandong Analysis and Test Center (China); Zhang, Jinjie [College of Biosystems Engineering and Food Science, Zhejiang University (China); Qiu, Jiying [Institute of Agro-Food Science and Technology, Shandong Academy of Agricultural Science, Shandong (China)

2012-07-01

Supercritical fluid extraction was used to extract active compounds from the Chinese traditional medicinal D. dasycarpus under the pressure of 30 MPa and temperature of 45 degree C. Further separation and purification was established by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:0.8:1.3:0.9, volume ratio). The separation yielded a total of 47 mg of dictamnine, 24 mg of obacunone and 83 mg of fraxinellone from 1.0 g of the crude extract in one step separation with the purity of 99.2, 98.4 and 99.0%, respectively, as determined by HPLC. The chemical structures of these compounds were identified by ESI-MS, IR, 1H-NMR and {sup 13}C-NMR. (author)

Extraction and isolation of dictamnine, obacunone and fraxinellone from Dictamnus dasycarpus Turcz. by supercritical fluid extraction and high-speed counter-current chromatography

Directory of Open Access Journals (Sweden)

Daijie Wang

2012-01-01

Full Text Available Supercritical fluid extraction was used to extract active compounds from the Chinese traditional medicinal D. dasycarpus under the pressure of 30 MPa and temperature of 45 ºC. Further separation and purification was established by high-speed counter-current chromatography (HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:0.8:1.3:0.9, volume ratio. The separation yielded a total of 47 mg of dictamnine, 24 mg of obacunone and 83 mg of fraxinellone from 1.0 g of the crude extract in one step separation with the purity of 99.2, 98.4 and 99.0%, respectively, as determined by HPLC. The chemical structures of these compounds were identified by ESI-MS, IR, ¹H-NMR and 13C-NMR.

Volatile Constituents, Inorganic Elements and Primary Screening of Bioactivity of Black Coral Cigarette Holders

Directory of Open Access Journals (Sweden)

Ganggang Shi

2011-05-01

Full Text Available Black corals (BC have been used for a long time in Chinese medicine, and may have some pharmaceutical functions when used as material for cigarette holders in southeast China. This study is aimed to investigate the bioactivities of volatile constituents in BC and to explore the folklore behind the use of BC cigarette holders (BCCHs. We extracted the volatile constituents of BC by supercritical fluid extraction (SFE with carbon dioxide (CO2-SFE, then identified and analyzed the constituents by gas chromatography-mass spectrometry (GC-MS. In total, 15 components were reliably identified in BC and found to be biologically active. These included triethyl phosphate, butylated hydroxytoluene, cedrol, n-hexadecanoic acid, squalene, and cholesterol. Meanwhile 13 inorganic elements (P, Ca, Mg, S, B, Si, Fe, Cu, Zn, Ba, etc. were determined by inductively coupled plasma spectrometer (ICPS. In the bioactivity tests, the BC extract (BCE showed a scavenging activity of 2,2-diphenyl-1-picrylhydrazyl free radicals and hydroxyl radicals by phenanthroline-Fe (II oxidation and moderate inhibition of Gram-positive microorganisms. The antioxidant and antimicrobial activities of BC, which are related to the active chemical composition, may explain the perceived benefit for cigarette smokers who use BCCHs.

Solute-matrix and Solute-Solute Interactions during Supercritical Fluid Extraction of Sea Buckthorn Leaves

Czech Academy of Sciences Publication Activity Database

Sajfrtová, Marie; Sovová, Helena

2012-01-01

Roč. 42, SI (2012), s. 1682-1691 E-ISSN 1877-7058. [International Congress of Chemical and Process Engineering CHISA 2012 and 15th Conference PRES 2012 /20./. Prague, 25.08.2012-29.08.2012] R&D Projects: GA TA ČR TA01010578 Institutional support: RVO:67985858 Keywords : supercritical fluid extraction * sea buckthom leaves * solute-solute interaction Subject RIV: CI - Industrial Chemistry, Chemical Engineering

Effect of Supercritical Carbon Dioxide Extraction Parameters on the Biological Activities and Metabolites Present in Extracts from Arthrospira platensis.

Science.gov (United States)

Esquivel-Hernández, Diego A; Rodríguez-Rodríguez, José; Cuéllar-Bermúdez, Sara P; García-Pérez, J Saúl; Mancera-Andrade, Elena I; Núñez-Echevarría, Jade E; Ontiveros-Valencia, Aura; Rostro-Alanis, Magdalena; García-García, Rebeca M; Torres, J Antonio; Chen, Wei Ning; Parra-Saldívar, Roberto

2017-06-12

Arthrospira platensis was used to obtain functional extracts through supercritical carbon dioxide extraction (SFE-CO₂). Pressure (P), temperature (T), co-solvent (CX), static extraction (SX), dispersant (Di) and dynamic extraction (DX) were evaluated as process parameters through a Plackett-Burman design. The maximum extract yield obtained was 7.48 ± 0.15% w/w. The maximum contents of bioactive metabolites in extracts were 0.69 ± 0.09 µg/g of riboflavin, 5.49 ± 0.10 µg/g of α-tocopherol, 524.46 ± 0.10 µg/g of β-carotene, 1.44 ± 0.10 µg/g of lutein and 32.11 ± 0.12 mg/g of fatty acids with 39.38% of palmitic acid, 20.63% of linoleic acid and 30.27% of γ-linolenic acid. A. platensis extracts had an antioxidant activity of 76.47 ± 0.71 µg GAE/g by Folin-Ciocalteu assay, 0.52 ± 0.02, 0.40 ± 0.01 and 1.47 ± 0.02 µmol TE/g by DPPH, FRAP and TEAC assays, respectively. These extracts showed antimicrobial activity against Staphylococcus aureus ATCC 25923, Pseudomonas aeruginosa ATCC 27853, Escherichia coli ATCC 25922 and Candida albicans ATCC 10231. Overall, co-solvent was the most significant factor for all measured effects ( p extraction parameters P: 450 bar, CX: 11 g/min, SX: 15 min, DX: 25 min, T: 60 °C and Di: 35 g.

Improved solid-phase extraction method for systematic toxicological analysis in biological fluids.

Science.gov (United States)

Soriano, T; Jurado, C; Menéndez, M; Repetto, M

2001-03-01

A method for the simultaneous qualitative and quantitative determination of drugs of abuse (opiates, cocaine, or amphetamines) and prescribed drugs (tricyclic antidepressants, phenotiazines, benzodiazepines, etc.) in biological fluids--blood, urine, bile, and gastric contents--was developed. This procedure involves solid-phase extraction with Bond-Elut Certify columns followed by analysis by gas chromatography-nitrogen-phosphorus detection (GC-NPD) and confirmation by gas chromatography-mass spectrometry (GC-MS), after derivatization, when necessary. Pretreatment was performed on all samples: sonication for 15 min plus enzymatic hydrolysis with beta-glucuronidase in urine. With respect to the internal standards, nalorphine and trihexylamine were used for basic substances, allobarbital for acidic drugs, and prazepam for benzodiazepines. Acidic and basic compounds were extracted from different aliquots of samples at different pH levels: 6-6.5 for the acidic and neutral and 8-8.5 for the basic and the benzodiazepines. Several areas of experimental design were considered in the process of method optimization. These included internal standards, pH, sonication, flow rate and washing solvents. It was found that systematic analysis could be reliably performed using optimized extraction conditions. The recovery rates for the compounds tested were always higher than 61.02%.

Magnetic Partitioning Nanofluid for Rare Earth Extraction from Geothermal Fluids

Energy Technology Data Exchange (ETDEWEB)

McGrail, Bernard P. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Thallapally, Praveen K. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Liu, Jian [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Nune, Satish K. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

2017-08-21

Rare earth metals are critical materials in a wide variety of applications in generating and storing renewable energy and in designing more energy efficient devices. Extracting rare earth metals from geothermal brines is a very challenging problem due to the low concentrations of these elements and engineering challenges with traditional chemical separations methods involving packed sorbent beds or membranes that would impede large volumetric flow rates of geothermal fluids transitioning through the plant. We are demonstrating a simple and highly cost-effective nanofluid-based method for extracting rare earth metals from geothermal brines. Core-shell composite nanoparticles are produced that contain a magnetic iron oxide core surrounded by a shell made of silica or metal-organic framework (MOF) sorbent functionalized with chelating ligands selective for the rare earth elements. By introducing the nanoparticles at low concentration (≈0.05 wt%) into the geothermal brine after it passes through the plant heat exchanger, the brine is exposed to a very high concentration of chelating sites on the nanoparticles without need to pass through a large and costly traditional packed bed or membrane system where pressure drop and parasitic pumping power losses are significant issues. Instead, after a short residence time flowing with the brine, the particles are effectively separated out with an electromagnet and standard extraction methods are then applied to strip the rare earth metals from the nanoparticles, which are then recycled back to the geothermal plant. Recovery efficiency for the rare earths at ppm level has now been measured for both silica and MOF sorbents functionalized with a variety of chelating ligands. A detailed preliminary techno-economic performance analysis of extraction systems using both sorbents showed potential to generate a promising internal rate of return (IRR) up to 20%.

Field demonstration of an active reservoir pressure management through fluid injection and displaced fluid extractions at the Rock Springs Uplift, a priority geologic CO₂ storage site for Wyoming

Energy Technology Data Exchange (ETDEWEB)

Jiao, Zunsheng [Univ. of Wyoming, Laramie, WY (United States)

2017-04-05

This report provides the results from the project entitled Field Demonstration of Reservoir Pressure Management through Fluid Injection and Displaced Fluid Extraction at the Rock Springs Uplift, a Priority Geologic CO2 Storage Site for Wyoming (DE-FE0026159 for both original performance period (September 1, 2015 to August 31, 2016) and no-cost extension (September 1, 2016 to January 6, 2017)).

Preliminary analysis of proton magnetic resonance 1D spectra of cerebrospinal fluid and brain cancer extracts

International Nuclear Information System (INIS)

Toczylowska, B.; Jozwik, A.; Kierul, K.; Matysiak, Z.; Sidor, M.; Wojcik, J.

1999-01-01

In series of cerebrospinal fluid samples from 25 patients proton spectra of magnetic resonance were measured. The spectra were measured also for series of brain tumor tissue extracts received from another 25 patients. This paper presents an attempt to apply statistical methods of image recognition for spectra analysis of the two measured series

DNA extraction methods for panbacterial and panfungal PCR detection in intraocular fluids.

Science.gov (United States)

Mazoteras, Paloma; Bispo, Paulo José Martins; Höfling-Lima, Ana Luisa; Casaroli-Marano, Ricardo P

2015-07-01

Three different methods of DNA extraction from intraocular fluids were compared with subsequent detection for bacterial and fungal DNA by universal PCR amplification. Three DNA extraction methods, from aqueous and vitreous humors, were evaluated to compare their relative efficiency. Bacterial (Gram positive and negative) and fungal strains were used in this study: Escherichia coli, Staphylococcus epidermidis and Candida albicans. The quality, quantification, and detection limit for DNA extraction and PCR amplification were analyzed. Validation procedures for 13 aqueous humor and 14 vitreous samples, from 20 patients with clinically suspected endophthalmitis were carried out. The column-based extraction method was the most time-effective, achieving DNA detection limits ≥10(2) and 10(3 )CFU/100 µL for bacteria and fungi, respectively. PCR amplification detected 100 fg, 1 pg and 10 pg of genomic DNA of E. coli, S. epidermidis and C. albicans respectively. PCR detected 90.0% of the causative agents from 27 intraocular samples collected from 20 patients with clinically suspected endophthalmitis, while standard microbiological techniques could detect only 60.0%. The most frequently found organisms were Streptococcus spp. in 38.9% (n = 7) of patients and Staphylococcus spp. found in 22.2% (n = 4). The column-based extraction method for very small inocula in small volume samples (50-100 µL) of aqueous and/or vitreous humors allowed PCR amplification in all samples with sufficient quality for subsequent sequencing and identification of the microorganism in the majority of them.

Utilization of mixed cellulolytic microbes from termite extract, elephant faecal solution and buffalo ruminal fluid to increase in vitro digestibility of King Grass

Directory of Open Access Journals (Sweden)

Agung Prabowo

2007-06-01

Full Text Available Cellulose is a compound of plant cell walls which is difficult to be degraded because it composed of glucose monomers linked by β-(1.4-bound. It will be hydrolysed by cellulase enzyme secreted by cellulolytic microbes. The effective digestion of cellulose needs high activity of cellulase enzyme. This research aims to increase in vitro king grass digestibility utilizing mixed cellulolytic microbes of termite extract, elephant faecal solution, and buffalo ruminal fluid. Twelve syringes contained gas test media were randomly divided into four treatments based on sources of microbe (SM, namely: S (SM: cattle ruminal fluid [S], RGK (SM: mixed cellulolytic microbes of termite extract, elephant faecal solution, and buffalo ruminal fluid [RGK], with composition 1 : 1 : 1, S-RGK (SM: S + RGK, with composition 1:1, and TM (without given treatment microbe. Digestibility was measured using gas test method. Average of gas production treatment of S-RGK (70.2 + 0.6 ml was higher and significantly different (P<0.01 compared to treatment of S (60.3 + 0.8 ml, RGK (40.8 + 2.3 ml, and TM (13.3 + 2.0 ml. Utilization of mixed cellulolytic microbes of termite extract, elephant faecal solution, and buffalo ruminal fluid (RGK that combined with microbes of cattle ruminal fluid (S could increase in vitro digestibility of king grass.

Study on the possibility of supercritical fluid extraction for reprocessing of spent nuclear fuel from high temperature gas-cooled reactor

International Nuclear Information System (INIS)

Duan Wuhua; Zhu Liyang; Zhu Yongjun; Xu Jingming

2011-01-01

International interest in high temperature gas-cooled reactor (HTGR) has been increasing in recent years. It is important to study on reprocessing of spent nuclear fuel from HTGR for recovery of nuclear resource and reduction of nuclear waste. Treatment of UO 2 pellets for preparing fuel elements of the 10 MW high temperature gas-cooled reactor (HTR-10) using supercritical fluid extraction was investigated. UO 2 pellets are difficult to be directly dissolved and extracted with TBP-HNO 3 complex in supercritical CO 2 (SC-CO 2 ), and the extraction efficiency is only about 7% under experimental conditions. UO 2 pellets are also difficult to be converted completely into nitrate with N 2 O 4 . When UO 2 pellets break spontaneously into U 3 O 8 powders with particle size below 100 μm under O 2 flow and 600degc, the extraction efficiency of U 3 O 8 powders with TBP-HNO 3 complex in SC-CO 2 can reach more than 98%. U 3 O 8 powders are easy to be completely converted into nitrate with N 2 O 4 . The extraction efficiency of the nitrate product with TBP in SC-CO 2 can reach more than 99%. So it has a potential prospect that application of supercritical fluid extraction in reprocessing of spent nuclear fuel from HTGR. (author)

Identification and quantification of cannabinoids in Cannabis sativa L. plants by high performance liquid chromatography-mass spectrometry.

Science.gov (United States)

Aizpurua-Olaizola, Oier; Omar, Jone; Navarro, Patricia; Olivares, Maitane; Etxebarria, Nestor; Usobiaga, Aresatz

2014-11-01

High performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) has been successfully applied to cannabis plant extracts in order to identify cannabinoid compounds after their quantitative isolation by means of supercritical fluid extraction (SFE). MS conditions were optimized by means of a central composite design (CCD) approach, and the analysis method was fully validated. Six major cannabinoids [tetrahydrocannabinolic acid (THCA), tetrahydrocannabinol (THC), cannabidiol (CBD), tetrahydrocannabivarin (THCV), cannabigerol (CBG), and cannabinol (CBN)] were quantified (RSD Cannabis sativa L. plant varieties and the principal component analysis (PCA) of the resulting data, a clear difference was observed between outdoor and indoor grown plants, which was attributed to a higher concentration of THC, CBN, and CBD in outdoor grown plants.

Various extraction and analytical techniques for isolation and identification of secondary metabolites from Nigella sativa seeds.

Science.gov (United States)

Liu, X; Abd El-Aty, A M; Shim, J-H

2011-10-01

Nigella sativa L. (black cumin), commonly known as black seed, is a member of the Ranunculaceae family. This seed is used as a natural remedy in many Middle Eastern and Far Eastern countries. Extracts prepared from N. sativa have, for centuries, been used for medical purposes. Thus far, the organic compounds in N. sativa, including alkaloids, steroids, carbohydrates, flavonoids, fatty acids, etc. have been fairly well characterized. Herein, we summarize some new extraction techniques, including microwave assisted extraction (MAE) and supercritical extraction techniques (SFE), in addition to the classical method of hydrodistillation (HD), which have been employed for isolation and various analytical techniques used for the identification of secondary metabolites in black seed. We believe that some compounds contained in N. sativa remain to be identified, and that high-throughput screening could help to identify new compounds. A study addressing environmentally-friendly techniques that have minimal or no environmental effects is currently underway in our laboratory.

Sensitive, automatic method for the determination of diazepam and its five metabolites in human oral fluid by online solid-phase extraction and liquid chromatography with tandem mass spectrometry

DEFF Research Database (Denmark)

Jiang, Fengli; Rao, Yulan; Wang, Rong

2016-01-01

A novel and simple online solid-phase extraction liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous determination of diazepam and its five metabolites including nordazepam, oxazepam, temazepam, oxazepam glucuronide, and temazepam glucuronide...... in human oral fluid. Human oral fluid was obtained using the Salivette(®) collection device, and 100 μL of oral fluid samples were loaded onto HySphere Resin GP cartridge for extraction. Analytes were separated on a Waters Xterra C18 column and quantified by liquid chromatography with tandem mass...

DETERMINATION OF CHLORINATED PHENOLS BY SUPERCRITICAL FLUID EXTRACTION (SFE) -- COUPLED LIQUID CHROMATOGRAPHY (LC) SYSTEM. (R825549C011)

Science.gov (United States)

The perspectives, information and conclusions conveyed in research project abstracts, progress reports, final reports, journal abstracts and journal publications convey the viewpoints of the principal investigator and may not represent the views and policies of ORD and EPA. Concl...

Near-critical and supercritical fluid extraction of polycyclic aromatic hydrocarbons from town gas soil

International Nuclear Information System (INIS)

Kocher, B.S.; Azzam, F.O.; Cutright, T.J.; Lee, S.

1995-01-01

The contamination of soil by hazardous and toxic organic pollutants is an ever-growing problem facing the global community. One particular family of contaminants that are of major importance are polycyclic aromatic hydrocarbons (PAHs). PAHs are the result of coal gasification and high-temperature processes. Sludges from these town gas operations were generally disposed of into unlined pits and left there for eventual biodegradation. However, the high levels of PAH contained in the pits prevented the occurrence of biodegradation. PAH contaminated soil is now considered hazardous and must be cleaned to environmentally acceptable standards. One method for the remediation is extraction with supercritical water. Water in or about its critical region exhibits enhanced solvating power toward most organic compounds. Contaminated soil containing 4% by mass of hydrocarbons was ultra-cleaned in a 300-cm 3 semicontinuous system to an environmentally acceptable standard of less than 200 ppm residual hydrocarbon concentration. The effects of subcritical or supercritical extraction, solvent temperature, pressure, and density have been studied, and the discerning characteristics of this type of fluid have been identified. The efficiencies of subcritical and supercritical extraction have been discussed from a process engineering standpoint

A Swellable Microneedle Patch to Rapidly Extract Skin Interstitial Fluid for Timely Metabolic Analysis.

Science.gov (United States)

Chang, Hao; Zheng, Mengjia; Yu, Xiaojun; Than, Aung; Seeni, Razina Z; Kang, Rongjie; Tian, Jingqi; Khanh, Duong Phan; Liu, Linbo; Chen, Peng; Xu, Chenjie

2017-10-01

Skin interstitial fluid (ISF) is an emerging source of biomarkers for disease diagnosis and prognosis. Microneedle (MN) patch has been identified as an ideal platform to extract ISF from the skin due to its pain-free and easy-to-administrated properties. However, long sampling time is still a serious problem which impedes timely metabolic analysis. In this study, a swellable MN patch that can rapidly extract ISF is developed. The MN patch is made of methacrylated hyaluronic acid (MeHA) and further crosslinked through UV irradiation. Owing to the supreme water affinity of MeHA, this MN patch can extract sufficient ISF in a short time without the assistance of extra devices, which remarkably facilitates timely metabolic analysis. Due to covalent crosslinked network, the MN patch maintains the structure integrity in the swelling hydrated state without leaving residues in skin after usage. More importantly, the extracted ISF metabolites can be efficiently recovered from MN patch by centrifugation for the subsequent offline analysis of metabolites such as glucose and cholesterol. Given the recent trend of easy-to-use point-of-care devices for personal healthcare monitoring, this study opens a new avenue for the development of MN-based microdevices for sampling ISF and minimally invasive metabolic detection. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Supercritical fluid extraction of uranium from tissue paper matrix using organic extractants

International Nuclear Information System (INIS)

Kanekar, A.S.; Bhattacharyya, A.; Pathak, P.N.; Mohapatra, P.K.; Manchanda, V.K.

2009-01-01

Direct extraction of dried uranyl nitrate from tissue paper matrix was carried out using supercritical carbon dioxide modified with methanol solutions of extractants such as tri-n-butyl phosphate (TBP) and di-n-hexyl octanamide (DHOA)). The effects of temperature, pressure, extractant and nitric acid concentration on the extraction of uranyl ion were investigated. (author)

Solid-Phase Extraction Strategies to Surmount Body Fluid Sample Complexity in High-Throughput Mass Spectrometry-Based Proteomics

Science.gov (United States)

Bladergroen, Marco R.; van der Burgt, Yuri E. M.

2015-01-01

For large-scale and standardized applications in mass spectrometry- (MS-) based proteomics automation of each step is essential. Here we present high-throughput sample preparation solutions for balancing the speed of current MS-acquisitions and the time needed for analytical workup of body fluids. The discussed workflows reduce body fluid sample complexity and apply for both bottom-up proteomics experiments and top-down protein characterization approaches. Various sample preparation methods that involve solid-phase extraction (SPE) including affinity enrichment strategies have been automated. Obtained peptide and protein fractions can be mass analyzed by direct infusion into an electrospray ionization (ESI) source or by means of matrix-assisted laser desorption ionization (MALDI) without further need of time-consuming liquid chromatography (LC) separations. PMID:25692071

Seasonal differences in the content of phenols and pigments in thalli of freshwater Cladophora glomerata and its habitat.

Science.gov (United States)

Fabrowska, Joanna; Messyasz, Beata; Pankiewicz, Radosław; Wilińska, Patrycja; Łęska, Bogusława

2018-05-15

Polyphenols are chemicals that primarily inhibit the growth of various autotrophic organisms. The presence of these metabolites greatly boosts the ecological dominance of eg. Cladophora, which creates large surface mats. The main goal of our work was to quantify the phenol and polyphenols (allelopathic substances) secreted by the macroalgae as a result of exposure to biotic stress caused by competition. The research was carried out on the Cladophora glomerata biomass collected from two freshwater ecosystems located in Wielkopolska Region (Poland, Fig. 1): Oporzynskie Lake (N52° 55', E 17° 9') and Nielba River (N52˚48', E 17° 12'). Seasonal variability (May-October 2015) in the properties of C. glomerata mats in the river and lake ecosystem was also analyzed in relation to the physicochemical parameters of water. In addition, the content of pigments in the analyzed biomass was determined during the appearance of algae mats in water reservoirs. Biomass extraction was performed to determine the phenolic and carotenoid contents (chlorophyll and carotenoids) by using two extraction methods: microwave-assisted extraction (MAE) and supercritical fluid extraction (SFE). After isolation of the phenols from the thalli (mats) and the habitat, they were analyzed using the Folin-Ciocalteu method with some modifications, while the pigment content (chlorophyll and carotenoids) was evaluated by the spectrophotometric method Liechtenthaler (1987) with some variations. Analysis of the content of these components in algae extracts indicates that the tendency of changes in their contents was similar or the same. Growth and decrease of phenolic content (Cladophora T MAE and Cladophora T SFE) and pigments (MAE chlorophyll, SFE and MAE carotenoids) at the same time were independent of the insulation method used. The mats formed by C. glomerata on the surface of Lake Oporzyńskie were more stable and larger surface area than those on the Nielba River, which could explain

Stacking fault energy measurements in solid solution strengthened Ni-Cr-Fe alloys using synchrotron radiation

Energy Technology Data Exchange (ETDEWEB)

Unfried-Silgado, Jimy [Metals Characterization and Processing Laboratory, Brazilian Nanothecnology National Laboratory - CNPEM/ABTLuS, Caixa Postal 6192, CEP 13083-970, Campinas, Sao Paulo (Brazil); Universidade Estadual de Campinas UNICAMP, Faculdade de Engenharia Mecanica FEM, Campinas (Brazil); Universidad Autonoma del Caribe, Grupo IMTEF, Ingenieria Mecanica, Barranquilla (Colombia); Wu, Leonardo [Metals Characterization and Processing Laboratory, Brazilian Nanothecnology National Laboratory - CNPEM/ABTLuS, Caixa Postal 6192, CEP 13083-970, Campinas, Sao Paulo (Brazil); Furlan Ferreira, Fabio [Universidade Federal do ABC, Centro de Ciencias Naturais e Humanas (CCNH), Sao Paulo (Brazil); Mario Garzon, Carlos [Universidad Nacional de Colombia, Departamento de Fisica, Bogota (Colombia); Ramirez, Antonio J, E-mail: antonio.ramirez@lnnano.org.br [Metals Characterization and Processing Laboratory, Brazilian Nanothecnology National Laboratory - CNPEM/ABTLuS, Caixa Postal 6192, CEP 13083-970, Campinas, Sao Paulo (Brazil)

2012-12-15

The stacking fault energy (SFE) in a set of experimental Ni-Cr-Fe alloys was determined using line profile analysis on synchrotron X-ray diffraction measurements. The methodology used here is supported by the Warren-Averbach calculations and the relationships among the stacking fault probability ({alpha}) and the mean-square microstrain (<{epsilon}{sup 2}{sub L}>). These parameters were obtained experimentally from cold-worked and annealed specimens extracted from the set of studied Ni-alloys. The obtained results show that the SFE in these alloys is strongly influenced by the kind and quantity of addition elements. Different effects due to the action of carbide-forming elements and the solid solution hardening elements on the SFE are discussed here. The simultaneous addition of Nb, Hf, and, Mo, in the studied Ni-Cr-Fe alloys have generated the stronger decreasing of the SFE. The relationships between SFE and the contributions on electronic structure from each element of additions were established.

Extraction with supercritical gases

Energy Technology Data Exchange (ETDEWEB)

Schneider, G M; Wilke, G; Stahl, E

1980-01-01

The contents of this book derives from a symposium on the 5th and 6th of June 1978 in the ''Haus der Technik'' in Essen. Contributions were made to separation with supercritical gases, fluid extraction of hops, spices and tobacco, physicochemical principles of extraction, phase equilibria and critical curves of binary ammonia-hydrocarbon mixtures, a quick method for the microanalytical evaluation of the dissolving power of supercritical gases, chromatography with supercritical fluids, the separation of nonvolatile substances by means of compressed gases in countercurrent processes, large-scale industrial plant for extraction with supercritical gases, development and design of plant for high-pressure extraction of natural products.

Supercritical fluid extraction of reed (thypa)

Energy Technology Data Exchange (ETDEWEB)

Kucuk, M.; Genel, Y. [YYU Educational Faculty, Van (Turkey); Demir, H. [YYU Science and Art Faculty, Van (Turkey)

2005-04-15

Reed (typha) mill was converted to liquid products by using organic solvents (methanol, ethanol and acetone) with catalysts (% 10 NaOH and ZnCl{sub 2}) and without catalyst in an autoclave at temperatures of 533, 553, and 573 K. The liquid products were extracted by liquid-liquid extraction [DSA1] (benzene and diethyl ether). The yields from supercritical methanol, ethanol and acetone conversions were 36.2, 24.5, and 55.1%, respectively, at 573 K. In the catalytic runs with methanol and ethanol extracts were 46.3 and 35.5% (for NaOH catalyst) and 51.8 and 38.5% (for ZnCl{sub 2} catalyst) respectively, at 573 K. The yields from supercritical methanol were increased from 38.2 to 52.4% as the temperature was increased from 533 to 573 K in the catalytic run. (Author)

Antibacterial and Antiproliferative Activities of Plumericin, an Iridoid Isolated from Momordica charantia Vine

Directory of Open Access Journals (Sweden)

Jutamas Saengsai

2015-01-01

Full Text Available Plumericin, an iridoid lactone, was isolated with relatively high yield from Momordica charantia vine using the supercritical fluid extraction (SFE and the separation box (Sepbox comprising dual combination of high-performance liquid chromatography and solid phase extraction. This compound showed antibacterial activity against Enterococcus faecalis and Bacillus subtilis with minimum inhibitory concentration (MIC values better than cloxacillin. Plumericin potently inhibited proliferation of two leukemic cancer cell lines: they were acute and chronic leukemic cancer cell lines, NB4 and K562, with the effective doses (ED50 of 4.35 ± 0.21 and 5.58 ± 0.35 μg/mL, respectively. In addition, the mechanism of growth inhibition in both cell lines was induced by apoptosis, together with G2/M arrest in K562 cells.

Comparison of Glucose Area Under the Curve Measured Using Minimally Invasive Interstitial Fluid Extraction Technology with Continuous Glucose Monitoring System in Diabetic Patients

OpenAIRE

Uemura, Mei

2017-01-01

Background: Continuous glucose monitoring (CGM) is reported to be a useful technique, but difficult or inconvenient for some patients and institutions. We are developing a glucose area under the curve (AUC) monitoring system without blood sampling using a minimally invasive interstitial fluid extraction technology (MIET). Here we evaluated the accuracy of interstitial fluid glucose (IG) AUC measured by MIET in patients with diabetes for an extended time interval and the potency of detecting h...

Comparison of Glucose Area Under the Curve Measured Using Minimally Invasive Interstitial Fluid Extraction Technology with Continuous Glucose Monitoring System in Diabetic Patients

OpenAIRE

Mei Uemura; Yutaka Yano; Toshinari Suzuki; Taro Yasuma; Toshiyuki Sato; Aya Morimoto; Samiko Hosoya; Chihiro Suminaka; Hiromu Nakajima; Esteban C. Gabazza; Yoshiyuki Takei

2017-01-01

Background Continuous glucose monitoring (CGM) is reported to be a useful technique, but difficult or inconvenient for some patients and institutions. We are developing a glucose area under the curve (AUC) monitoring system without blood sampling using a minimally invasive interstitial fluid extraction technology (MIET). Here we evaluated the accuracy of interstitial fluid glucose (IG) AUC measured by MIET in patients with diabetes for an extended time interval and the potency of detecting hy...

Kinetic models for supercritical CO2 extraction of oilseeds - a review

Directory of Open Access Journals (Sweden)

B. Nagy

2011-01-01

Full Text Available The supercritical fluid extraction of oilseeds is gaining increasing interest in commercial application for the last few decades, most particularly thanks to technical and environmental advantages of supercritical fluid extraction technology compared to current extraction methods with organic solvents. Furthermore, CO2 as a solvent is generally recognized as safe (GRAS. At present moment, supercritical fluid extractions on a commercial scale are limited to decaffeination, production of soluble hops extracts, sesame seed oil production and extraction of certain petroleum products. When considering industrial application, it is essential to test the applicability of the appropriate model for supercritical fluid extraction of oilseeds used for scale up of laboratory data to industrial design purposes. The aim of this paper is to review the most significant kinetic models reported in the literature for supercritical fluid extraction.

Development of a new extraction technique and HPLC method for the analysis of non-psychoactive cannabinoids in fibre-type Cannabis sativa L. (hemp).

Science.gov (United States)

Brighenti, Virginia; Pellati, Federica; Steinbach, Marleen; Maran, Davide; Benvenuti, Stefania

2017-09-05

The present work was aimed at the development and validation of a new, efficient and reliable technique for the analysis of the main non-psychoactive cannabinoids in fibre-type Cannabis sativa L. (hemp) inflorescences belonging to different varieties. This study was designed to identify samples with a high content of bioactive compounds, with a view to underscoring the importance of quality control in derived products as well. Different extraction methods, including dynamic maceration (DM), ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE) and supercritical-fluid extraction (SFE) were applied and compared in order to obtain a high yield of the target analytes from hemp. Dynamic maceration for 45min with ethanol (EtOH) at room temperature proved to be the most suitable technique for the extraction of cannabinoids in hemp samples. The analysis of the target analytes in hemp extracts was carried out by developing a new reversed-phase high-performance liquid chromatography (HPLC) method coupled with diode array (UV/DAD) and electrospray ionization-mass spectrometry (ESI-MS) detection, by using an ion trap mass analyser. An Ascentis Express C 18 column (150mm×3.0mm I.D., 2.7μm) was selected for the HPLC analysis, with a mobile phase composed of 0.1% formic acid in both water and acetonitrile, under gradient elution. The application of the fused-core technology allowed us to obtain a significant improvement of the HPLC performance compared with that of conventional particulate stationary phases, with a shorter analysis time and a remarkable reduction of solvent usage. The analytical method optimized in this study was fully validated to show compliance with international requirements. Furthermore, it was applied to the characterization of nine hemp samples and six hemp-based pharmaceutical products. As such, it was demonstrated to be a very useful tool for the analysis of cannabinoids in both the plant material and its derivatives for

Unstable Simple Volatiles and Gas Chromatography-Tandem Mass Spectrometry Analysis of Essential Oil from the Roots Bark of Oplopanax Horridus Extracted by Supercritical Fluid Extraction

Directory of Open Access Journals (Sweden)

Li Shao

2014-11-01

Full Text Available Volatile oil from the root bark of Oplopanax horridus is regarded to be responsible for the clinical uses of the title plant as a respiratory stimulant and expectorant. Therefore, a supercritical fluid extraction method was first employed to extract the volatile oil from the roots bark of O. horridus, which was subsequently analyzed by GC/MS. Forty-eight volatile compounds were identified by GC/MS analysis, including (S,E-nerolidol (52.5%, τ-cadinol (21.6% and S-falcarinol (3.6%. Accordingly, the volatile oil (100 g was subjected to chromatographic separation and purification. As a result, the three compounds, (E-nerolidol (2 g, τ-cadinol (62 mg and S-falcarinol (21 mg, were isolated and purified from the volatile oil, the structures of which were unambiguously elucidated by detailed spectroscopic analysis including 1D- and 2D-NMR techniques.

Rapid and simple pretreatment of human body fluids using electromembrane extraction across supported liquid membrane for capillary electrophoretic determination of lithium.

Science.gov (United States)

Strieglerová, Lenka; Kubáň, Pavel; Boček, Petr

2011-05-01

Electromembrane extraction was used for simultaneous sample cleanup and preconcentration of lithium from untreated human body fluids. The sample of a body fluid was diluted 100 times with 0.5 mM Tris solution and lithium was extracted by electromigration through a supported liquid membrane composed of 1-octanol into 100 mM acetic acid acceptor solution. Matrix compounds, such as proteins, red blood cells, and other high-molecular-weight compounds were efficiently retained on the supported liquid membrane. The liquid membrane was anchored in pores of a short segment of a polypropylene hollow fiber, which represented a low cost, single use, disposable extraction unit and was discarded after each use. Acceptor solutions were analyzed using capillary electrophoresis with capacitively coupled contactless conductivity detection (CE-C(4) D) and baseline separation of lithium was achieved in a background electrolyte solution consisting of 18 mM L-histidine and 40 mM acetic acid at pH 4.6. Repeatability of the electromembrane extraction-CE-C(4) D method was evaluated for the determination of lithium in standard solutions and real samples and was better than 0.6 and 8.2% for migration times and peak areas, respectively. The concentration limit of detection of 9 nM was achieved. The developed method was applied to the determination of lithium in urine, blood serum, blood plasma, and whole blood at both endogenous and therapeutic concentration levels. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction and Ozonation of organic pollutants in drinking waters

International Nuclear Information System (INIS)

Kenawi, I.M.; Barsoum, B.N.; Abdelhaflz, M.M.

2006-01-01

The continuous liquid-liquid, CLLE, and solid-phase, SPE. extraction techniques were used to study a problem of international relevance. The work was incident on the evaluation of the efficiency and optimisation of extruding techniques, CLLE. SPE and CLLEt-SPE, towards chlorinated pesticides and phenolic compounds from the Giza treatment plant station (Egypt), where the degree of pollution of such substances in drinking waters must be reduced. The total recoveries, rs, using SPE ranged between I).74 -0.87, whereas, the values were much less using the other two methods (0.158 - 0.1961; indicating the preferability of the SF'E technique. Analytical results were obtained through the various chromatographic techniques, liquid or gas. with adequately chosen detectors. A simple mathematical algorithm has been empirically developed allowing the assessment and comparison of the efficiencies of the three extracting procedures. Further treatment with ozone resulted in the oxidation and elimination of organic pollutants, with consequent improvement of water quality (total pesticide content 0.332-0.19μgL -1 ). A useful ozone treatment unit, capable of dealing with the emanation of contaminants in tap water, was built

Effect of Novel Marine Nutraceuticals on IL-1α-Mediated TNF-α Release from UVB-Irradiated Human Melanocyte-Derived Cells

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Visalini Muthusamy

2011-01-01

Full Text Available UV-induced inflammation and reactive oxygen species formation are involved in the development of melanoma. Natural products like 5β-scymnol and CO2-supercritical fluid extract (CO2-SFE of mussel oil contain anti-inflammatory and antioxidant properties that may aid in reducing the deleterious effects of UV radiation. Therefore, their effect on the release of the proinflammatory cytokine, tumour necrosis factor-α (TNF-α, from UVB-irradiated human melanocytic cells was examined. Human epidermal melanocytes (HEM and MM96L melanoma cells were exposed to UVB radiation and IL-1α. Cell viability and TNF-α levels were determined 24 hours after-irradiation while p38 mitogen-activated protein kinase (MAPK activation was observed at 15 min after-irradiation. When α-tocopherol, CO2-SFE mussel oil, and 5β-scymnol were added to the UVB-irradiated HEM cells treated with IL-1α, TNF-α levels fell by 53%, 65%, and 76%, respectively, while no inhibition was evident in MM96L cells. This effect was not due to inhibition of the intracellular p38 MAPK signalling pathway. These compounds may be useful in preventing inflammation-induced damage to normal melanocytes.

Chemical kinetics and transport processes in supercritical fluid extraction of coal. Final report, August 10, 1990--December 30, 1992

Energy Technology Data Exchange (ETDEWEB)

McCoy, B.J.; Smith, J.M.; Wang, M.; Zhang, C.J.

1993-02-01

The overall objective of this project was to study the supercritical fluid extraction of hydrocarbons from coal. Beyond the practical concern of deriving products from coal, the research has provided insights into the structure, properties, and reactivities of coal. Information on engineering fundamentals of coal thermolysis and extraction, including physical and chemical processes, is presented in this final report. To accomplish the goals of the project we developed continuous-flow experiments for fixed-bed samples of coal that allow two types of analysis of the extract: continuous spectrophotometric absorbance measurements of the lumped concentration of extract, and chromatographic determinations of molecular-weight distributions as a function of time. Thermolysis of coal yields a complex mixture of many extract products whose molecular-weight distribution (MWD) varies with time for continuous-flow, semibatch experiments. The flow reactor with a differential, fixed bed of coal particles contacted by supercritical t-butanol was employed to provide dynamic MWD data by means of HPLC gel permeation chromatography of the extract. The experimental results, time-dependent MWDs of extract molecules, were interpreted by a novel mathematical model based on continuous-mixture kinetics for thermal cleavage of chemical bonds in the coal network. The parameters for the MWDs of extractable groups in the coal and the rate constants for one- and two-fragment reaction are determined from the experimental data. The significant effect of temperature on the kinetics of the extraction was explained in terms of one- and two-fragment reactions in the coal.

Computational Fluid Dynamics Based Extraction of Heat Transfer Coefficient in Cryogenic Propellant Tanks

Science.gov (United States)

Yang, H. Q.; West, Jeff

2015-01-01

Current reduced-order thermal model for cryogenic propellant tanks is based on correlations built for flat plates collected in the 1950's. The use of these correlations suffers from: inaccurate geometry representation; inaccurate gravity orientation; ambiguous length scale; and lack of detailed validation. The work presented under this task uses the first-principles based Computational Fluid Dynamics (CFD) technique to compute heat transfer from tank wall to the cryogenic fluids, and extracts and correlates the equivalent heat transfer coefficient to support reduced-order thermal model. The CFD tool was first validated against available experimental data and commonly used correlations for natural convection along a vertically heated wall. Good agreements between the present prediction and experimental data have been found for flows in laminar as well turbulent regimes. The convective heat transfer between tank wall and cryogenic propellant, and that between tank wall and ullage gas were then simulated. The results showed that commonly used heat transfer correlations for either vertical or horizontal plate over predict heat transfer rate for the cryogenic tank, in some cases by as much as one order of magnitude. A characteristic length scale has been defined that can correlate all heat transfer coefficients for different fill levels into a single curve. This curve can be used for the reduced-order heat transfer model analysis.

Simultaneous analysis of nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.

Science.gov (United States)

Huang, Yang; Zhang, Tingting; Zhao, Yumei; Zhou, Haibo; Tang, Guangyun; Fillet, Marianne; Crommen, Jacques; Jiang, Zhengjin

2017-09-10

Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ginseng extracts. Few analytical methods have been developed so far to simultaneously analyze these three classes of compounds with different polarities present in ginseng extracts. In the present study, a simple and efficient analytical method was successfully developed for the simultaneous separation of 17 nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The effect of various experimental factors on the separation performance, such as the column type, temperature and backpressure, the type of modifier and additive, and the concentration of make-up solvent were systematically investigated. Under the selected conditions, the developed method was successfully applied to the quality evaluation of 14 batches of ginseng extracts from different origins. The results obtained for the different batches indicate that this method could be employed for the quality assessment of ginseng extracts. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparative isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. using supercritical fluid extraction combined with consecutive high-speed countercurrent chromatography.

Science.gov (United States)

Yan, Rongwei; Shen, Jie; Liu, Xiaojing; Zou, Yong; Xu, Xinjun

2018-05-01

The objective of this study was to develop a consecutive preparation method for the isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. The process involved supercritical fluid extraction with CO 2 , solvent extraction, and two-step high-speed countercurrent chromatography. Pressure, temperature, and the volume of entrainer were optimized as 27 MPa, 52°C, and 60 mL by response surface methodology in supercritical fluid extraction with CO 2 , and the yield of the crude extracts was 7.91 g from 100 g of leaves. Subsequently, 80% methanol/water was used to extract and condense the three compounds from the crude extracts, and 4.23 g of methanol/water extracts was obtained. Then, a two-step high-speed countercurrent chromatography procedure was developed for the isolation of the three target compounds from methanol/water extracts, including conventional high-speed countercurrent chromatography for further enrichment and consecutive high-speed countercurrent chromatography for purification. The yield of concentrates from high-speed countercurrent chromatography was 2.50 g from 4.23 g of methanol/water extracts. Finally, the consecutive high-speed countercurrent chromatography produced 103.2 mg of hainanmurpanin, 244.7 mg of meranzin, and 255.4 mg of phebalosin with purities up to 97.66, 99.36, and 98.64%, respectively, from 900 mg of high-speed countercurrent chromatography concentrates in one run of three consecutive sample loadings without exchanging a solvent system. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Supercritical fluid extraction of meat lipids: an alternative approach to the identification of irradiated meats

International Nuclear Information System (INIS)

Hampson, J.W.; Jones, K.C.; Foglia, T.A.; Kohout, K.M.

1996-01-01

Ionizing radiation is currently under study as an alternative method for extending the shelf life of meats and meat products. Accordingly, methods are needed to determine if a meat or meat product has been exposed to ionizing radiation. In this study, a method is described for the isolation and analysis of volatile hydrocarbons formed in meat lipids after exposure to ionizing radiation. The method is based on supercritical fluid extraction of the hydrocarbons from meat lipids and subsequent identification and quantitation of individual hydrocarbons by gas chromatography (GC) with a mass selection detector (MSD). Supercritical carbon dioxide at 175 bar and 40°C extracted the hydrocarbon fraction from total meat lipids within 20 min. The presence of radiolytic hydrocarbons, as determined by GC/MSD, was then correlated to the degree of irradiation of the meat from 0 to 10 kGy. Besides being faster, this method has the advantage of reduced solvent consumption when compared to current methods for determining if a meat or meat product has been irradiated

Sedative and hypnotic effects of supercritical carbon dioxide fluid extraction from Schisandra chinensis in mice

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Hongyan Zhu

2016-10-01

Full Text Available Schisandra chinensis is a traditional Chinese medicine that has been used for treating insomnia and neurasthenia for centuries. Lignans, which are considered to be the bioactive components, are apt to be extracted by supercritical carbon dioxide. This study was conducted to investigate the sedative and hypnotic activities of the supercritical carbon dioxide fluid extraction of S. chinensis (SFES in mice and the possible mechanisms. SFES exhibited an obvious sedative effect on shortening the locomotor activity in mice in a dose-dependent (10–200 mg/kg manner. SFES (50 mg/kg, 100 mg/kg, and 200 mg/kg, intragstrically showed a strong hypnotic effect in synergy with pentobarbital in mouse sleep, and reversal of insomnia induced by caffeine, p-chlorophenylalanine and flumazenil by decreasing sleep latency, sleep recovery, and increasing sleeping time. In addition, it produced a synergistic effect with 5-hydroxytryptophan (2.5 mg/kg, intraperitoneally. The behavioral pharmacological results suggest that SFES has significant sedative and hypnotic activities, and the mechanisms might be relevant to the serotonergic and γ-aminobutyric acid (GABAergic system.

Antioxidant and toxicological evaluation of a Tamarindus indica L. leaf fluid extract.

Science.gov (United States)

Escalona-Arranz, J C; Perez-Rosés, R; Rodríguez-Amado, J; Morris-Quevedo, H J; Mwasi, L B; Cabrera-Sotomayor, O; Machado-García, R; Fong-Lórez, O; Alfonso-Castillo, A; Puente-Zapata, E

2016-01-01

In the scientific community, there is a growing interest in Tamarindus indica L. leaves, both as a valuable nutrient and as a functional food. This paper focuses on exploring its safety and antioxidant properties. A tamarind leaf fluid extract (TFE) wholly characterised was evaluated for its anti-DPPH activity (IC50 = 44.36 μg/mL) and its reducing power activity (IC50 = 60.87 μg/mL). TFE also exhibited a high ferrous ion-chelating capacity, with an estimated binding constant of 1.085 mol L(-1) while its influence over nitric oxide production in human leucocytes was irregular. At low concentrations, TFE stimulated NO output, but it significantly inhibited it when there was an increase in concentration. TFE was also classified as a non-toxic substance in two toxicity tests: the acute oral toxicity test and the oral mucous irritability test. Further toxicological assays are needed, although results so far suggest that TFE might become a functional dietary supplement.

A review of lipid extraction from fish processing by-product for use as a biofuel

International Nuclear Information System (INIS)

Adeoti, Ibraheem A.; Hawboldt, Kelly

2014-01-01

Fish processing facilities generate a significant amount of fish by-products that could be an important source of energy, food, or industrial feedstock. While fish oil is a natural source of omega-3 polyunsaturated fatty acids (mostly eicosapentaenoic acid (EPA), and docosahexaenoic acid (DHA)) used in nutritional supplements, the ability to extract, refine, and get to market of these oils may be challenging at processing facilities where there is limited infrastructure and plants are remotely located. Under these conditions, extraction of oil from fish by-product for use as an in-house or regional fuel may be both economically and environmentally be a more sustainable approach. Processes to extract and refine fish oil for fuel are less energy intensive than the processes for nutritional quality oils and do not require the stringent product specifications and approval process as in the food and pharmaceutical industry. Unlike food crops, extraction of oil from fish residue does not negatively impact food production. This paper presents an overview of developments made in fish oil extraction methodologies including physical, chemical and biological processes. - Highlights: • We have reviewed various lipid extraction methods from fish residue. • Low grade fish oils for fuel applications can be beneficial to facility and region. • The environmental impacts and safety issues can be reduced using SFE method

High-throughput analysis of sulfatides in cerebrospinal fluid using automated extraction and UPLC-MS/MS.

Science.gov (United States)

Blomqvist, Maria; Borén, Jan; Zetterberg, Henrik; Blennow, Kaj; Månsson, Jan-Eric; Ståhlman, Marcus

2017-07-01

Sulfatides (STs) are a group of glycosphingolipids that are highly expressed in brain. Due to their importance for normal brain function and their potential involvement in neurological diseases, development of accurate and sensitive methods for their determination is needed. Here we describe a high-throughput oriented and quantitative method for the determination of STs in cerebrospinal fluid (CSF). The STs were extracted using a fully automated liquid/liquid extraction method and quantified using ultra-performance liquid chromatography coupled to tandem mass spectrometry. With the high sensitivity of the developed method, quantification of 20 ST species from only 100 μl of CSF was performed. Validation of the method showed that the STs were extracted with high recovery (90%) and could be determined with low inter- and intra-day variation. Our method was applied to a patient cohort of subjects with an Alzheimer's disease biomarker profile. Although the total ST levels were unaltered compared with an age-matched control group, we show that the ratio of hydroxylated/nonhydroxylated STs was increased in the patient cohort. In conclusion, we believe that the fast, sensitive, and accurate method described in this study is a powerful new tool for the determination of STs in clinical as well as preclinical settings. Copyright © 2017 by the American Society for Biochemistry and Molecular Biology, Inc.

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African Journals Online (AJOL)

AJTCAM

Rhodiolae Radix is reported to contain some biologically active components, such ... including phenolic acids, ethyl gallate, ethereal oil, organic acids and lipids ... supercritical carbon dioxide extraction (SFE), supercritical or subcritical water extraction, .... Effect of solid-liquid ratio on extraction yield of polysaccharides from ...

Nitrate conversion and supercritical fluid extraction of UO2-CeO2 solid solution prepared by an electrolytic reduction-coprecipitation method

International Nuclear Information System (INIS)

Zhu, L.Y.; Duan, W.H.; Wen, M.F.; Xu, J.M.; Zhu, Y.J.

2014-01-01

A low-waste technology for the reprocessing of spent nuclear fuel (SNF) has been developed recently, which involves the conversion of actinide and lanthanide oxides with liquid N 2 O 4 into their nitrates followed by supercritical fluid extraction of the nitrates. The possibility of the reprocessing of SNF from high-temperature gas-cooled reactors (HTGRs) with nitrate conversion and supercritical fluid extraction is a current area of research in China. Here, a UO 2 -CeO 2 solid solution was prepared as a surrogate for a UO 2 -PuO 2 solid solution, and the recovery of U and Ce from the UO 2 -CeO 2 solid solution with liquid N 2 O 4 and supercritical CO 2 containing tri-n-butyl phosphate (TBP) was investigated. The UO 2 -CeO 2 solid solution prepared by electrolytic reduction-coprecipitation method had square plate microstructures. The solid solution after heat treatment was completely converted into nitrates with liquid N 2 O 4 . The XRD pattern of the nitrates was similar to that of UO 2 (NO 3 ) 2 . 3H 2 O. After 120 min of online extraction at 25 MPa and 50 , 99.98% of the U and 98.74% of the Ce were recovered from the nitrates with supercritical CO 2 containing TBP. The results suggest a promising potential technology for the reprocessing of SNF from HTGRs. (orig.)

Supercritical carbon dioxide extraction as a predictor of polycyclic aromatic hydrocarbon bioaccumulation and toxicity by earthworms in manufactured-gas plant site soils.

Science.gov (United States)

Kreitinger, Joseph P; Quiñones-Rivera, Antonio; Neuhauser, Edward F; Alexander, Martin; Hawthorne, Steven B

2007-09-01

The toxicity and uptake of polycyclic aromatic hydrocarbons (PAHs) by earthworms were measured in soil samples collected from manufactured-gas plant sites having a wide range in PAH concentrations (170-42,000 mg/kg) and soil characteristics. Samples varied from vegetated soils to pure lampblack soot and had total organic carbon contents ranging from 3 to 87%. The biota-soil accumulation factors (BSAFs) observed for individual PAHs in field-collected earthworms (Aporrectodea caliginosa) were up to 50-fold lower than the BSAFs predicted using equilibrium-partitioning theory. Acute toxicity to the earthworm Eisenia fetida was unrelated to total PAH concentration: Mortality was not observed in some soils having high concentrations of total PAHs (>42,000 mg/kg), whereas 100% mortality was observed in other soils having much lower concentrations of total PAHs (1,520 mg/kg). Instead, toxicity appeared to be related to the rapidly released fraction of PAHs determined by mild supercritical CO2 extraction (SFE). The results demonstrate that soils having approximately 16,000 mg rapidly released total PAH/kg organic carbon can be acutely toxic to earthworms and that the concentration of PAHs in soil that is rapidly released by SFE can estimate toxicity to soil invertebrates.

The fractal feature and price trend in the gold future market at the Shanghai Futures Exchange (SFE)

Science.gov (United States)

Wu, Binghui; Duan, Tingting

2017-05-01

The price of gold future is affected by many factors, which include the fluctuation of gold price and the change of trading environment. Fractal analysis can help investors gain better understandings of the price fluctuation and make reasonable investment decisions in the gold future market. After analyzing gold future price from January 2th, 2014 to April 12th, 2016 at the Shanghai Futures Exchange (SFE) in China, the conclusion is drawn that the gold future market has sustainability in each trading day, with all Hurst indexes greater than 0.5. The changing features of Hurst index indicate the sustainability of gold future market is strengthened first and weakened then. As a complicatedly nonlinear system, the gold future market can be well reflected by Elman neural network, which is capable of memorizing previous prices and particularly suited for forecasting time series in comparison with other types of neural networks. After analyzing the price trend in the gold future market, the results show that the relative error between the actual value of gold future and the predictive value of Elman neural network is smaller. This model that has a better performance in data fitting and predication, can help investors analyze and foresee the price tendency in the gold future market.

Systems and methods for multi-fluid geothermal energy systems

Science.gov (United States)

Buscheck, Thomas A.

2017-09-19

A method for extracting geothermal energy from a geothermal reservoir formation. A production well is used to extract brine from the reservoir formation. At least one of nitrogen (N.sub.2) and carbon dioxide (CO.sub.2) may be used to form a supplemental working fluid which may be injected into a supplemental working fluid injection well. The supplemental working fluid may be used to augment a pressure of the reservoir formation, to thus drive a flow of the brine out from the reservoir formation.

Environmental management technology demonstration and commercialization: Tasks 2, 3, 4, and 8. Semiannual report, October 1994--March 1995

International Nuclear Information System (INIS)

Hawthorne, S.B.; Ness, R.O. Jr.; Nowok, J.W.; Pflughoeft-Hassett, D.; Hurley, J.P.; Steadman, E.N.

1995-05-01

The objective of the Environmental Management program at the Energy and Environmental Research Center (EERC) is to develop, demonstrate, and commercialize technologies that address the environmental management needs of contaminated sites, including characterization, sensors, and monitoring; low-level mixed waste processing; material disposition technology; improved waste forms; in situ containment and remediation; and efficient separation technologies for radioactive wastes. Task 2 is the extraction and analysis of pollutant organics from contaminated solids using off-line supercritical fluid extraction (SFE) and on-line SFE-infrared spectroscopy. Task 3, pyrolysis of plastics, has as its objectives to develop a commercial process to significantly reduce the volume of mixed-plastics-paper-resin waste contaminated with low-level radioactive material; concentrate contaminants in a collectible form; and determine the distribution and form of contaminants after pyrolysis of the mixed waste. Task 4, stabilization of vitrified wastes, has as its objectives to (1) demonstrate a waste vitrification procedure for enhanced stabilization of waste materials and (2) develop a testing protocol to understand the long-term leaching behavior of the stabilized waste form. The primary objective of Task 8, Management and reporting, is coordination of this project with other programs and opportunities. In addition, management oversight will be maintained to ensure that tasks are completed and coordinated as planned and that deliverables are submitted in a timely manner. Accomplishments to date is each task are described. 62 refs

Industrial applications and current trends in supercritical fluid technologies

Directory of Open Access Journals (Sweden)

Gamse Thomas

2005-01-01

Full Text Available Supercritical fluids have a great potential for wide fields of processes Although CO2 is still one of the most used supercritical gases, for special purposes propane or even fluorinated-chlorinated fluids have also been tested. The specific characteristics of supercritical fluids behaviour were analyzed such as for example the solubilities of different components and the phase equilibria between the solute and solvent. The application at industrial scale (decaffeinating of tea and coffee, hop extraction or removal of pesticides from rice, activity in supercritical extraction producing total extract from the raw material or different fractions by using the fractionated separation of beverages (rum, cognac, whisky, wine, beer cider, of citrus oils and of lipids (fish oils, tall oil were also discussed. The main interest is still for the extraction of natural raw materials producing food ingredients, nutraceuticals and phytopharmaceuticals but also cleaning purposes were tested such as the decontamination of soils the removal of residual solvents from pharmaceutical products, the extraction of flame retardants from electronic waste or precision degreasing and cleaning of mechanical and electronic parts. An increasing interest obviously exists for impregnation purposes based on supercritical fluids behaviour, as well as for the dying of fibres and textiles. The production of fine particles in the micron and submicron range, mainly for pharmaceutical products is another important application of supercritical fluids. Completely new products can be produced which is not possible under normal conditions. Supercritical fluid technology has always had to compete with the widespread opinion that these processes are very expensive due to very high investment costs in comparison with classical low-pressure equipment. Thus the opinion is that these processes should be restricted to high-added value products. A cost estimation for different plant sizes and

Phytochemical Characterization and Biological Evaluation of the Aqueous and Supercritical Fluid Extracts from Salvia sclareoides Brot

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Batista Daniela

2017-04-01

Full Text Available Plants belonging to the genus Salvia (Lamiaceae are known to have a wide range of biological properties. In this work, extracts obtained from the aerial parts of Salvia sclareoides Brot. were evaluated to investigate their chemical composition, toxicity, bioactivity, and stability under in vitro gastrointestinal conditions. The composition of the supercritical fluid extract was determined by GC and GC-MS, while the identification of the infusion constituents was performed by HPLC-DAD and LC-MS. The in vitro cytotoxicity of both extracts (0-2 mg/mL was evaluated in Caco-2 cell lines by the MTT assay. The anti-inflammatory and anticholinesterase activities were determined through the inhibition of cyclooxygenase-1 and acetylcholinesterase enzymes, while β-carotene/linoleic acid bleaching test and the DPPH assays were used to evaluate the antioxidant activity. The infusion inhibited cyclooxygenase-1 (IC50 = 271.0 μg/mL, and acetylcholinesterase (IC50 = 487.7 μg/ mL enzymes, also demonstrated significant antioxidant properties, as evaluated by the DPPH (IC50 = 10.4 μg/mL and β-carotene/linoleic acid (IC50 = 30.0 μg/mL assays. No remarkable alterations in the composition or in the bioactivities of the infusion were observed after in vitro digestion, which supports the potential of S. sclareoides as a source of bioactive ingredients with neuroprotective, anti-inflammatory and antioxidant properties.

Métodos de extração e/ou concentração de compostos encontrados em fluidos biológicos para posterior determinação cromatográfica Methods of extraction and/or concentration of compounds found in biological fluids for subsequent chromatographic determination

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Sonia C. N. Queiroz

2001-02-01

Full Text Available When organic compounds present in biological fluids are analysed by chromatographic methods, it is generally necessary to carry out a prior sample preparation due the high complexity of this type of sample, especially when the compounds to be determinated are found in very low concentrations. This article describes some of the principal methods for sample preparation in analyses of substances present in biological fluids. The methods include liquid-liquid extraction, solid phase extraction, supercritical fluid extraction and extraction using solid and liquid membranes. The advantages and disadvantages of these methods are discussed.

Spectrophotometric Quantification of Toxicologically Relevant Concentrations of Chromium(VI in Cosmetic Pigments and Eyeshadow Using Synthetic Lachrymal Fluid Extraction

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Sarah Wurster

2012-01-01

Full Text Available Chromium(VI salts are possible contaminants of the chromium(III pigments used as colorants in eyeshadow preparations. The use of products containing these contaminants poses acute risks for sensitization and contact allergies. Chromium(VI compounds are also classified as carcinogenic to humans (IARC group 1. An analytical method to analyse trace levels of chromium(VI in eyeshadow was developed in this study. The method is based on an extraction of the chromium(VI from the sample using a maximum extraction with alkali and additionally with synthetic lachrymal fluid to simulate physiological conditions. Following derivatization with 1,5-diphenylcarbazide, the extracted chromium(VI is then quantified by spectrophotometry (540 nm. Validation tests indicated a method standard deviation (inter- and intraday of 8.7% and a linear range up to 25 mg/kg. The average recovery was 107.9%, and the detection limit was 2.7 mg/kg. The applicability of the procedure was confirmed by the analysis of pigments and authentic eyeshadow matrices.

Fluid sampling tool

Science.gov (United States)

Garcia, Anthony R.; Johnston, Roger G.; Martinez, Ronald K.

1999-05-25

A fluid sampling tool for sampling fluid from a container. The tool has a fluid collecting portion which is drilled into the container wall, thereby affixing it to the wall. The tool may have a fluid extracting section which withdraws fluid collected by the fluid collecting section. The fluid collecting section has a fluted shank with an end configured to drill a hole into a container wall. The shank has a threaded portion for tapping the borehole. The shank is threadably engaged to a cylindrical housing having an inner axial passageway sealed at one end by a septum. A flexible member having a cylindrical portion and a bulbous portion is provided. The housing can be slid into an inner axial passageway in the cylindrical portion and sealed to the flexible member. The bulbous portion has an outer lip defining an opening. The housing is clamped into the chuck of a drill, the lip of the bulbous section is pressed against a container wall until the shank touches the wall, and the user operates the drill. Wall shavings (kerf) are confined in a chamber formed in the bulbous section as it folds when the shank advances inside the container. After sufficient advancement of the shank, an o-ring makes a seal with the container wall.

Ion-pair extraction of [3]histobadine from biological fluids

International Nuclear Information System (INIS)

Scasnar, V.

1997-01-01

A simple and specific radiometric assay was developed for determination of stobadine, a cardio protective drug, in the serum of experimental animals. It is based on a single extraction step of the radioactively labeled drug from serum into the benzene solution of dicarbolide of cobalt followed by the quantitation of the extracted radioactivity by using liquid scintillation counting. The extraction mechanism involves the ion-pair formation between the protonized molecule of stobadine and the hydrophobic, negatively charged molecule of dicarbollide of cobalt. The extraction of yield of stobadine from 1 ml of serum was 95% in the concentration range from 1 to 6000 ng/ml. The co extraction of metabolites was less than 5%. The assay was applied to determination of stobadine in serum of dogs and the data obtained were in good agreement with those obtained by high performance liquid chromatography. (author)

Isolation by pressurised fluid extraction (PFE) and identification using CPC and HPLC/ESI/MS of phenolic compounds from Brazilian cherry seeds (Eugenia uniflora L.).

Science.gov (United States)

Oliveira, Alessandra L; Destandau, Emilie; Fougère, Laëtitia; Lafosse, Michel

2014-02-15

Brazilian cherry seeds are a waste product from juice and frozen pulp production and, the seeds composition was investigated to valorize this by-product. Compounds separation was performed with ethanol by pressurised fluid extraction (PFE). Here we determine the effect of temperature (T), static time (ST), number of cycles (C), and flush volume (VF) on the yield, composition and total phenolic content (TPC) of the seed extracts. T, ST and their interaction positively influenced yield and TPC. Extracts were fractionated by high performance liquid chromatography (HPLC) and centrifugal partition chromatography (CPC). The collected fractions characterizations were made by electrospray ionisation mass spectrometry (ESI/MS) and high resolution mass spectrometry (HRMS) indicated the presence of ellagic acid pentoside and deoxyhexose, quercitrin and kaempferol pentoside. All of these compounds have antioxidant properties and normally are found in plant extracts. These results confirm that Brazilian cherry seed extract is a potentially valuable source of antioxidants. Copyright © 2013 Elsevier Ltd. All rights reserved.

Characterisation of dissolved organic compounds in hydrothermal fluids by stir bar sorptive extraction - gas chomatography - mass spectrometry. Case study: the Rainbow field (36°N, Mid-Atlantic Ridge

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Konn Cecile

2012-11-01

Full Text Available Abstract The analysis of the dissolved organic fraction of hydrothermal fluids has been considered a real challenge due to sampling difficulties, complexity of the matrix, numerous interferences and the assumed ppb concentration levels. The present study shows, in a qualitative approach, that Stir Bar Sorptive Extraction (SBSE followed by Thermal Desorption – Gas Chromatography – Mass Spectrometry (TD-GC-MS is suitable for extraction of small sample volumes and detection of a wide range of volatile and semivolatile organic compounds dissolved in hydrothermal fluids. In a case study, the technique was successfully applied to fluids from the Rainbow ultramafic-hosted hydrothermal field located at 36°14’N on the Mid-Atlantic Ridge (MAR. We show that n-alkanes, mono- and poly- aromatic hydrocarbons as well as fatty acids can be easily identified and their retention times determined. Our results demonstrate the excellent repeatability of the method as well as the possibility of storing stir bars for at least three years without significant changes in the composition of the recovered organic matter. A preliminary comparative investigation of the organic composition of the Rainbow fluids showed the great potential of the method to be used for assessing intrafield variations and carrying out time series studies. All together our results demonstrate that SBSE-TD-GC-MS analyses of hydrothermal fluids will make important contributions to the understanding of geochemical processes, geomicrobiological interactions and formation of mineral deposits.

Investigating sub-2 μm particle stationary phase supercritical fluid chromatography coupled to mass spectrometry for chemical profiling of chamomile extracts.

Science.gov (United States)

Jones, Michael D; Avula, Bharathi; Wang, Yan-Hong; Lu, Lu; Zhao, Jianping; Avonto, Cristina; Isaac, Giorgis; Meeker, Larry; Yu, Kate; Legido-Quigley, Cristina; Smith, Norman; Khan, Ikhlas A

2014-10-17

Roman and German chamomile are widely used throughout the world. Chamomiles contain a wide variety of active constituents including sesquiterpene lactones. Various extraction techniques were performed on these two types of chamomile. A packed-column supercritical fluid chromatography-mass spectrometry method was designed for the identification of sesquiterpenes and other constituents from chamomile extracts with no derivatization step prior to analysis. Mass spectrometry detection was achieved by using electrospray ionization. All of the compounds of interest were separated within 15 min. The chamomile extracts were analyzed and compared for similarities and distinct differences. Multivariate statistical analysis including principal component analysis and orthogonal partial least squares-discriminant analysis (OPLS-DA) were used to differentiate between the chamomile samples. German chamomile samples confirmed the presence of cis- and trans-tonghaosu, chrysosplenols, apigenin diglucoside whereas Roman chamomile samples confirmed the presence of apigenin, nobilin, 1,10-epioxynobilin, and hydroxyisonobilin. Copyright © 2014 Elsevier B.V. All rights reserved.

Fluid sampling tool

Science.gov (United States)

Garcia, A.R.; Johnston, R.G.; Martinez, R.K.

1999-05-25

A fluid sampling tool is described for sampling fluid from a container. The tool has a fluid collecting portion which is drilled into the container wall, thereby affixing it to the wall. The tool may have a fluid extracting section which withdraws fluid collected by the fluid collecting section. The fluid collecting section has a fluted shank with an end configured to drill a hole into a container wall. The shank has a threaded portion for tapping the borehole. The shank is threadably engaged to a cylindrical housing having an inner axial passageway sealed at one end by a septum. A flexible member having a cylindrical portion and a bulbous portion is provided. The housing can be slid into an inner axial passageway in the cylindrical portion and sealed to the flexible member. The bulbous portion has an outer lip defining an opening. The housing is clamped into the chuck of a drill, the lip of the bulbous section is pressed against a container wall until the shank touches the wall, and the user operates the drill. Wall shavings (kerf) are confined in a chamber formed in the bulbous section as it folds when the shank advances inside the container. After sufficient advancement of the shank, an o-ring makes a seal with the container wall. 6 figs.

Multi-fluid renewable geo-energy systems and methods

Science.gov (United States)

Buscheck, Thomas A.

2017-08-22

A geo-energy production method for extracting thermal energy from a reservoir formation. A production well extracts brine from the reservoir formation. A plurality of working fluid injection ("WFI") wells may be arranged proximate to the production well to at least partially circumscribe the production well. A plurality of brine production ("BP") wells may be arranged in a vicinity of the WFI wells to at least partially circumscribe the WFI wells. A working fluid is injected into the WFI wells to help drive a flow of the brine up through the production and BP wells, together with at least a portion of the injected working fluid. Parasitic-load time-shifting and to storing of excess solar thermal energy may also be performed.

Supercritical fluid extraction of oregano (Origanum vulgare) essentials oils: anti-inflammatory properties based on cytokine response on THP-1 macrophages.

Science.gov (United States)

Ocaña-Fuentes, A; Arranz-Gutiérrez, E; Señorans, F J; Reglero, G

2010-06-01

Two fractions (S1 and S2) of an oregano (Origanum vulgare) extract obtained by supercritical fluid extraction have been used to test anti-inflammatory effects on activated human THP-1 cells. The main compounds present in the supercritical extract fractions of oregano were trans-sabinene hydrate, thymol and carvacrol. Fractions toxicity was assessed using the mitochondrial-respiration-dependent 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium (MTT) reduction method for several concentrations during 24 and 48 h of incubation. Concentrations higher than 30 microg/mL of both supercritical S1 and S2 oregano fractions caused a reduction in cell viability in a dose-dependent manner. Oxidized-LDLs (oxLDLs) activated THP-1 macrophages were used as cellular model of atherogenesis and the release/secretion of cytokines (TNT-alpha, IL-1beta, IL-6 and IL-10) and their respective mRNA expressions were quantified both in presence or absence of supercritical oregano extracts. The results showed a decrease in pro-inflammatory TNF-alpha, IL-1beta and IL-6 cytokines synthesis, as well as an increase in the production of anti-inflammatory cytokine IL-10. These results may suggest an anti-inflammatory effect of oregano extracts and their compounds in a cellular model of atherosclerosis. Copyright 2010 Elsevier Ltd. All rights reserved.

Influence of soil γ-irradiation and spiking on sorption of p,p'-DDE and soil organic matter chemistry.

Science.gov (United States)

Škulcová, Lucia; Scherr, Kerstin E; Chrást, Lukáš; Hofman, Jakub; Bielská, Lucie

2018-07-15

The fate of organic chemicals and their metabolites in soils is often investigated in model matrices having undergone various pre-treatment steps that may qualitatively or quantitatively interfere with the results. Presently, effects associated with soil sterilization by γ-irradiation and soil spiking using an organic solvent were studied in one freshly spiked soil (sterilization prior to contamination) and its field-contaminated (sterilization after contamination) counterpart for the model organic compound 1,1-Dichloro-2,2-bis(4-chlorophenyl)ethene (p,p'-DDE). Changes in the sorption and potential bioavailability of spiked and native p,p'-DDE were measured by supercritical fluid extraction (SFE), XAD-assisted extraction (XAD), and solid-phase microextraction (SPME) and linked to qualitative changes in soil organic matter (SOM) chemistry measured by diffuse reflectance infrared Fourier-transform (DRIFT) spectroscopy. Reduced sorption of p,p´-DDE detected with XAD and SPME was associated more clearly with spiking than with sterilization, but SFE showed a negligible impact. Spiking resulted in an increase of the DRIFT-derived hydrophobicity index, but irradiation did not. Spectral peak height ratio descriptors indicated increasing hydrophobicity and hydrophilicity in pristine soil following sterilization, and a greater reduction of hydrophobic over hydrophilic groups as a consequence of spiking. In parallel, reduced sorption of p,p´-DDE upon spiking was observed. Based on the present samples, γ-irradiation appears to alter soil sorptive properties to a lesser extent when compared to common laboratory processes such as spiking with organic solvents. Copyright © 2018. Published by Elsevier Inc.

Supercritical fluid technology: concepts and pharmaceutical applications.

Science.gov (United States)

Deshpande, Praful Balavant; Kumar, G Aravind; Kumar, Averineni Ranjith; Shavi, Gopal Venkatesh; Karthik, Arumugam; Reddy, Meka Sreenivasa; Udupa, Nayanabhirama

2011-01-01

In light of environmental apprehension, supercritical fluid technology (SFT) exhibits excellent opportunities to accomplish key objectives in the drug delivery sector. Supercritical fluid extraction using carbon dioxide (CO(2)) has been recognized as a green technology. It is a clean and versatile solvent with gas-like diffusivity and liquid-like density in the supercritical phase, which has provided an excellent alternative to the use of chemical solvents. The present commentary provides an overview of different techniques using supercritical fluids and their future opportunity for the drug delivery industry. Some of the emerging applications of SFT in pharmaceuticals, such as particle design, drug solubilization, inclusion complex, polymer impregnation, polymorphism, drug extraction process, and analysis, are also covered in this review. The data collection methods are based on the recent literature related to drug delivery systems using SFT platforms. SFT has become a much more versatile and environmentally attractive technology that can handle a variety of complicated problems in pharmaceuticals. This cutting-edge technology is growing predominantly to surrogate conventional unit operations in relevance to the pharmaceutical production process. Supercritical fluid technology has recently drawn attention in the field of pharmaceuticals. It is a distinct conception that utilizes the solvent properties of supercritical fluids above their critical temperature and pressure, where they exhibit both liquid-like and gas-like properties, which can enable many pharmaceutical applications. For example, the liquid-like properties provide benefits in extraction processes of organic solvents or impurities, drug solubilization, and polymer plasticization, and the gas-like features facilitate mass transfer processes. It has become a much more versatile and environmentally attractive technology that can handle a variety of complicated problems in pharmaceuticals. This review is

Use of supercritical carbon dioxide extraction

Energy Technology Data Exchange (ETDEWEB)

Taniguchi, Masayuki (Niigata Univ., Faculty of Engineering, Niigata, (Japan))

1989-09-25

Supercritical fluid extraction is a novel diffusion and separation technique which exploits simultaneously the increase of vapor pressure and the difference of chemical affinities of fluids near the critical point. A solvent which is used as the supercritical fluid has the following features: the critical point exists in the position of relatively ease of handling, the solvent is applicable to the extraction of a physiological active substance of thermal instability. Carbon dioxide as the solvent is non-flammable, non-corrosive, non-toxic, cheap, and readily available of high purity. The results of studies on the use of supercritical carbon dioxide (SC-CO{sub 2}) as a solvent for natural products in the fermentation and food industries, were collected. SC-CO{sub 2} extraction are used in many fields, examples for the application are as follows: removal of organic solvents from antibiotics; extraction of vegetable oils contained in wheat germ oil, high quality mustard seeds, rice bran and so on; brewing of sake using rice and rice-koji; use as a non-aqueous medium for the synthesis of precursors of the Aspartame; and use in sterilization. 66 refs., 17 figs., 21 tabs.

Quantitative image processing in fluid mechanics

Science.gov (United States)

Hesselink, Lambertus; Helman, James; Ning, Paul

1992-01-01

The current status of digital image processing in fluid flow research is reviewed. In particular, attention is given to a comprehensive approach to the extraction of quantitative data from multivariate databases and examples of recent developments. The discussion covers numerical simulations and experiments, data processing, generation and dissemination of knowledge, traditional image processing, hybrid processing, fluid flow vector field topology, and isosurface analysis using Marching Cubes.

Volatile and Nonvolatile Constituents and Antioxidant Capacity of Oleoresins in Three Taiwan Citrus Varieties as Determined by Supercritical Fluid Extraction

Directory of Open Access Journals (Sweden)

Min-Hung Chen

2016-12-01

Full Text Available As local varieties of citrus fruit in Taiwan, Ponkan (Citrus reticulata Blanco, Tankan (C. tankan Hayata, and Murcott (C. reticulate × C. sinensis face substantial competition on the market. In this study, we used carbon dioxide supercritical technology to extract oleoresin from the peels of the three citrus varieties, adding alcohol as a solvent assistant to enhance the extraction rate. The supercritical fluid extraction was fractionated with lower terpene compounds in order to improve the oxygenated amounts of the volatile resins. The contents of oleoresin from the three varieties of citrus peels were then analyzed with GC/MS in order to identify 33 volatile compounds. In addition, the analysis results indicated that the non-volatile oleoresin extracted from the samples contains polymethoxyflavones (86.2~259.5 mg/g, limonoids (111.7~406.2 mg/g, and phytosterols (686.1~1316.4 μg/g. The DPPH (1,1-Diphenyl-2-picrylhydrazyl, ABTS [2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid] scavenging and inhibition of lipid oxidation, which test the oleoresin from the three kinds of citrus, exhibited significant antioxidant capacity. The component polymethoxyflavones contributed the greatest share of the overall antioxidant capacity, while the limonoid and phytosterol components effectively coordinated with its effects.

Extraction and Quantitative HPLC Analysis of Coumarin in Hydroalcoholic Extracts of Mikania glomerata Spreng: ("guaco" Leaves

Directory of Open Access Journals (Sweden)

Celeghini Renata M. S.

2001-01-01

Full Text Available Methods for preparation of hydroalcoholic extracts of "guaco" (Mikania glomerata Spreng. leaves were compared: maceration, maceration under sonication, infusion and supercritical fluid extraction. Evaluation of these methods showed that maceration under sonication had the best results, when considering the ratio extraction yield/extraction time. A high performance liquid chromatography (HPLC procedure for the determination of coumarin in these hydroalcoholic extracts of "guaco" leaves is described. The HPLC method is shown to be sensitive and reproducible.

Procedure for controlling the extraction of production fluid from a production well; Fremgangsmaate for aa styre uttrekking av produksjonsfluid fra en produksjonsbroenn

Energy Technology Data Exchange (ETDEWEB)

Curlett, H.B.

1996-06-17

Basic well drilling techniques have not changed throughout the years: a number of drill pipes connected into a drill column are rotated along with a drill bit in the ground formation. It has been difficult to obtain instant information on the local parameters during the drilling operation. Such information is required by the drilling operator for efficient operation. The present invention concerns controlling the extraction of production fluids from a production well, characterized by externally monitoring local well parameters by means of signals from sensors in the well. If the signals indicate that defined limiting values of one or more parameters have been exceeded, one or more of different fluids are pumped simultaneously and independently down individually assigned conduits to restore the parameters to within their normal ranges. 28 figs.

Supercritical Fluid Extraction of Seed Oil from Chinese Licorice ...

African Journals Online (AJOL)

NJD

2005-12-17

Dec 17, 2005 ... a Key Laboratory of Forest Plant Ecology, Northeast Forestry University, Hexing Road 26, 150040, ... Carbon dioxide, the most commonly used supercritical fluid, has ... absorb the remaining water that the chloroform layer had.

Discrimination of reservoir fluid contacts using compressional and ...

African Journals Online (AJOL)

Improved fluid detection and lithology discrimination using rock properties and attributes cross plots have been attempted using well log data in an Onshore Niger Delta field. Rock properties and attributes were extracted using empirical rock physics models on well logs and used to validate their potentials as pore fluid ...

Supercritical fluid reverse micelle separation

Science.gov (United States)

Fulton, J.L.; Smith, R.D.

1993-11-30

A method of separating solute material from a polar fluid in a first polar fluid phase is provided. The method comprises combining a polar fluid, a second fluid that is a gas at standard temperature and pressure and has a critical density, and a surfactant. The solute material is dissolved in the polar fluid to define the first polar fluid phase. The combined polar and second fluids, surfactant, and solute material dissolved in the polar fluid is maintained under near critical or supercritical temperature and pressure conditions such that the density of the second fluid exceeds the critical density thereof. In this way, a reverse micelle system defining a reverse micelle solvent is formed which comprises a continuous phase in the second fluid and a plurality of reverse micelles dispersed in the continuous phase. The solute material is dissolved in the polar fluid and is in chemical equilibrium with the reverse micelles. The first polar fluid phase and the continuous phase are immiscible. The reverse micelles each comprise a dynamic aggregate of surfactant molecules surrounding a core of the polar fluid. The reverse micelle solvent has a polar fluid-to-surfactant molar ratio W, which can vary over a range having a maximum ratio W[sub o] that determines the maximum size of the reverse micelles. The maximum ratio W[sub o] of the reverse micelle solvent is then varied, and the solute material from the first polar fluid phase is transported into the reverse micelles in the continuous phase at an extraction efficiency determined by the critical or supercritical conditions. 27 figures.