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Sample records for liquids ngl extraction

  1. Panola NGL (natural gas liquid) line laid in east Texas

    Energy Technology Data Exchange (ETDEWEB)

    1982-11-01

    Construction is complete on the Panola Products Pipeline Co. 8-in. NGL line in E. Texas. The 60-mile pipeline, which traverses rolling timber country, lightly developed commercial areas, and low-lying wetlands, will ultimately gather liquids from gas plants in E. Texas. Initially, this system is designed to transport natural gas liquids mix from the Carthage Plant, operated by Champlin Petroleum Co., to Gulf Pipeline Co.'s injection station at Lufkin, Texas. Final delivery will be made to various petrochemical facilities in the Mont Belvieu, Texas area. To minimize right-of-way problems, the line was routed parallel to an existing United Gas 22-in. pipeline for a distance of 36 miles from Carthage to near Nacogdoches. The pipeline has a design pressure of 1,480 psi. A back pressure of approx. 450 psi will be maintained on the line at all times to keep the mix in a liquid state. The predominant pipe used along the route is API 5LX-52 with a wall thickness of 0.219-in. Heavier wall thickness pipe, up to 0.375-in., is used for road, railroad, and major water crossings.

  2. Low Cost Chemical Feedstocks Using an Improved and Energy Efficient Natural Gas Liquid (NGL) Removal Process, Final Technical Report

    Energy Technology Data Exchange (ETDEWEB)

    Meyer, Howard, S.; Lu, Yingzhong

    2012-08-10

    The overall objective of this project is to develop a new low-cost and energy efficient Natural Gas Liquid (NGL) recovery process - through a combination of theoretical, bench-scale and pilot-scale testing - so that it could be offered to the natural gas industry for commercialization. The new process, known as the IROA process, is based on U.S. patent No. 6,553,784, which if commercialized, has the potential of achieving substantial energy savings compared to currently used cryogenic technology. When successfully developed, this technology will benefit the petrochemical industry, which uses NGL as feedstocks, and will also benefit other chemical industries that utilize gas-liquid separation and distillation under similar operating conditions. Specific goals and objectives of the overall program include: (i) collecting relevant physical property and Vapor Liquid Equilibrium (VLE) data for the design and evaluation of the new technology, (ii) solving critical R&D issues including the identification of suitable dehydration and NGL absorbing solvents, inhibiting corrosion, and specifying proper packing structure and materials, (iii) designing, construction and operation of bench and pilot-scale units to verify design performance, (iv) computer simulation of the process using commercial software simulation platforms such as Aspen-Plus and HYSYS, and (v) preparation of a commercialization plan and identification of industrial partners that are interested in utilizing the new technology. NGL is a collective term for C2+ hydrocarbons present in the natural gas. Historically, the commercial value of the separated NGL components has been greater than the thermal value of these liquids in the gas. The revenue derived from extracting NGLs is crucial to ensuring the overall profitability of the domestic natural gas production industry and therefore of ensuring a secure and reliable supply in the 48 contiguous states. However, rising natural gas prices have dramatically reduced

  3. NGL data conversion system

    Science.gov (United States)

    Shoji, Masahiro; Horiuchi, Nobuyasu

    2005-06-01

    We are developing a NGL data conversion system for EPL, for LEEPL, and for EBDW, which is based on our established photomask data conversion system, PATACON PC-cluster. For EPL data conversion, it has SF division, Complementary division, Stitching, Proximity effect correction, Alignment mark insertion, EB stepper control data creation, and Mask inspection data creation. For LEEPL data conversion, it has Pattern checking, Complementary division, Stitching, Stress distortion correction, Alignment mark insertion, and Mask inspection data creation. For EB direct-writing data conversion, it has Proximity effect correction and Extraction of aperture pattern for cell projection exposure.

  4. Ultra pressure liquid chromatography-negative electrospray ionization mass spectrometry determination of twelve halobenzoquinones at ng/L levels in drinking water.

    Science.gov (United States)

    Huang, Rongfu; Wang, Wei; Qian, Yichao; Boyd, Jessica M; Zhao, Yuli; Li, Xing-Fang

    2013-05-01

    We report here the characterization of twelve halobenzoquinones (HBQs) using electrospray ionization (ESI) high resolution quadrupole time-of-flight mass spectrometry. The high resolution negative ESI spectra of the twelve HBQs formed two parent ions, [M + H(+) + 2e(-)], and the radical M(-•). The intensities of these two parent ions are dependent on their chemical structures and on instrumental parameters such as the source temperature and flow rate. The characteristic ions of the HBQs were used to develop an ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method. At the UPLC flow rate (400 μL/min) and under the optimized ESI conditions, eleven HBQs showed the stable and abundant transitions [M + H(+) + 2e(-)] → X(-) (X(-) representing Cl(-), Br(-), or I(-)), while dibromo-dimethyl-benzoquinone (DBDMBQ) showed only the transition of M(-•) → Br(-). The UPLC efficiently separates all HBQs including some HBQ isomers, while the MS/MS offers exquisite limits of detection (LODs) at subng/mL levels for all HBQs except DBDMBQ. Combined with solid phase extraction (SPE), the method LOD is down to ng/L. The results from analysis of authentic samples demonstrated that the SPE-UPLC-MS/MS method is reliable, fast, and sensitive for the identification and quantification of the twelve HBQs in drinking water.

  5. Straightforward strategy for quantifying rotundone in wine at ngL(-1) level using solid-phase extraction and gas chromatography-quadrupole mass spectrometry. Occurrence in different varieties of spicy wines.

    Science.gov (United States)

    Culleré, Laura; Ontañón, Ignacio; Escudero, Ana; Ferreira, Vicente

    2016-09-01

    This paper presents a straightforward methodology to quantify rotundone in wine at ngL(-1) level. This compound, responsible for the black pepper aromatic note, may have sensorial relevance in some wines due to its low odor threshold, estimated at only 16ngL(-1) in red wines. The proposed strategy is based on solid phase extraction and analysis by GC-MS. The detection limit value was 0.6ngL(-1), which is more than one order of magnitude below its odor threshold in wine. Matrix effects have not been found and a synthetic wine calibration was proposed. The precision of the method was evaluated in reproducibility terms, obtaining a very acceptable value (RSD 4%). The optimized and validated strategy was applied to quantify this molecule in thirty wines belonging to different varieties as Graciano, Maturana tinta, Schioppettino, Shiraz, Duras and Gamay. Two of these wines exhibited levels higher than 100ngL(-1). Copyright © 2016. Published by Elsevier Ltd.

  6. Parallel artificial liquid membrane extraction

    DEFF Research Database (Denmark)

    Gjelstad, Astrid; Rasmussen, Knut Einar; Parmer, Marthe Petrine

    2013-01-01

    This paper reports development of a new approach towards analytical liquid-liquid-liquid membrane extraction termed parallel artificial liquid membrane extraction. A donor plate and acceptor plate create a sandwich, in which each sample (human plasma) and acceptor solution is separated by an arti...... by an artificial liquid membrane. Parallel artificial liquid membrane extraction is a modification of hollow-fiber liquid-phase microextraction, where the hollow fibers are replaced by flat membranes in a 96-well plate format....

  7. Rapid method for monitoring N-nitrosodimethylamine in drinking water at the ng/L level without pre-concentration using high-performance liquid chromatography-chemiluminescence detection.

    Science.gov (United States)

    Kodamatani, Hitoshi; Yamasaki, Hitomi; Sakaguchi, Takeru; Itoh, Shinya; Iwaya, Yoshimi; Saga, Makoto; Saito, Keiitsu; Kanzaki, Ryo; Tomiyasu, Takashi

    2016-08-19

    As a contaminant in drinking water, N-nitrosodimethylamine (NDMA) is of great concern because of its carcinogenicity; it has been limited to levels of ng/L by regulatory bodies worldwide. Consequently, a rapid and sensitive method for monitoring NDMA in drinking water is urgently required. In this study, we report an improvement of our previously proposed HPLC-based system for NDMA determination. The approach consists of the HPLC separation of NDMA, followed by NDMA photolysis to form peroxynitrite and detection with a luminol chemiluminescence reaction. The detection limit for the improved HPLC method was 0.2ng/L, which is 10 times more sensitive than our previously reported system. For tap water measurements, only the addition of an ascorbic acid solution to eliminate residual chlorine and passage through an Oasis MAX solid-phase extraction cartridge are needed. The proposed NDMA determination method requires a sample volume of less than 2mL and a complete analysis time of less than 15min per sample. The method was utilized for the long-term monitoring of NDMA in tap water. The NDMA level measured in the municipal water survey was 4.9ng/L, and a seasonal change of the NDMA concentration in tap water was confirmed. The proposed method should constitute a useful NDMA monitoring method for protecting drinking water quality. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. FLPP NGL Structural Subsystems Activity

    Science.gov (United States)

    Jaredson, D.; Ramusat, G.; Appel, S.; Cardone, T.; Persson, J.; Baiocco, P.; Lavelle, F.; Bouilly, Th.

    2012-07-01

    The ESA Future Launchers Preparatory Programme (FLPP) is the basis for new paradigms, investigating the key elements, logic and roadmaps to prepare the development of the safe, reliable and low cost next European Launch Vehicle (LV) for access to space (dubbed NGL - Next Generation LV), with an initial operational capability mid-next decade. In addition to carry cargo to conventional GTO or SSO, the European NGL has to be flexible enough to cope with new pioneering institutional missions as well as the evolving commercial payloads market. This achievement is broached studying three main areas relevant to ELVs: System concepts, Propulsion and Core Technology During the preliminary design activity, a number of design alternatives concerning NGL main structural subsystems have been investigated. Technology is one of the ways to meet the NGL challenges to either improve the performances or to reduce the cost or both. The relevant requirements allow to steer a ‘top-down’ approach for their conception and to propose the most effective technologies. Furthermore, all these technology developments represent a significant ‘bottom-up’ approach investment and concern a large range of activities. The structural subsystems portfolio of the FLPP ‘Core Technology’ activity encompasses major cutting-edge challenges for maturation of the various subsystems leading to reduce overall structural mass, increasing structural margins for robustness, metallic and composite containment of cryogenic propellants, significantly reducing fabrication and operations cost, etc. to derive performing upper and booster stages. Application of concurrent engineering methods will allow developments of performing technology demonstrators in terms of need, demonstration objective, size and cost yielding to safe, low-risk technical approaches for a future development. Potential ability of these advanced structural LV technologies to satisfy the system requirements of the NGL and their current

  9. Liquid-Liquid Extraction Equipment

    Energy Technology Data Exchange (ETDEWEB)

    Jack D. Law; Terry A. Todd

    2008-12-01

    Solvent extraction processing has demonstrated the ability to achieve high decontamination factors for uranium and plutonium while operating at high throughputs. Historical application of solvent extraction contacting equipment implies that for the HA cycle (primary separation of uranium and plutonium from fission products) the equipment of choice is pulse columns. This is likely due to relatively short residence times (as compared to mixer-settlers) and the ability of the columns to tolerate solids in the feed. Savannah River successfully operated the F-Canyon with centrifugal contactors in the HA cycle (which have shorter residence times than columns). All three contactors have been successfully deployed in uranium and plutonium purification cycles. Over the past 20 years, there has been significant development of centrifugal contactor designs and they have become very common for research and development applications. New reprocessing plants are being planned in Russia and China and the United States has done preliminary design studies on future reprocessing plants. The choice of contactors for all of these facilities is yet to be determined.

  10. Cyclohexylamine as extraction solvent and chelating agent in extraction and preconcentration of some heavy metals in aqueous samples based on heat-induced homogeneous liquid-liquid extraction.

    Science.gov (United States)

    Sorouraddin, Saeed Mohammad; Farajzadeh, Mir Ali; Okhravi, Tohid

    2017-12-01

    A new sample preparation method has been developed for extraction and preconcentration of some heavy metal cations in aqueous samples using cyclohexylamine-based homogeneous liquid-liquid microextraction. In the proposed method, cyclohexylamine was used as both the complexing agent and the extraction solvent. For this purpose, cyclohexylamine at µL level was initially added into an aqueous solution containing Co(II), Ni(II), and Cu(II) ions which was placed in a glass test tube. The mixture was shaken for forming a homogeneous solution. Then sodium chloride was added to the solution. After shaking manually again, the test tube was placed in a water bath thermostated at 70°C. Due to lower solubility of cyclohexylamine at the elevated temperature, a cloudy solution was formed. The fine droplets of cyclohexylamine containing cation-cyclohexylamine complexes were collected on the top of the aqueous phase by centrifuging. The enriched analytes in the upper phase were determined by graphite furnace atomic absorption spectrometry. Several variables possibly affecting the extraction efficiency were investigated and optimized. Under the optimum conditions the calibration curves were linear in the ranges of 80-1000, 40-700, and 80-800ngL(-1) for Co(2+), Ni(2+), and Cu(2+), respectively. Repeatability of the proposed method, expressed as relative standard deviation, ranged from 3.3% to 5.2% (n = 6, C = 200ngL(-1)). Moreover, the obtained detection limits of the selected analytes were in the range of 15.3-37.7ngL(-1). The accuracy of the developed procedure was verified by analyzing a certified reference material, namely NRCC-SLRS4 Riverine water. Finally, the proposed method was successfully applied for the simultaneous analysis of the selected analytes in environmental water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Metals Separation by Liquid Extraction.

    Science.gov (United States)

    Malmary, G.; And Others

    1984-01-01

    As part of a project focusing on techniques in industrial chemistry, students carry out experiments on separating copper from cobalt in chloride-containing aqueous solution by liquid extraction with triisoctylamine solvent and search the literature on the separation process of these metals. These experiments and the literature research are…

  12. Chiral separation by enantioselective liquid-liquid extraction

    NARCIS (Netherlands)

    Schuur, B.; Verkuijl, B. J. V.; Minnaard, A. J.; De Vries, J. G.; Heeres, H. J.; Feringa, B. L.

    2011-01-01

    The literature on enantioselective liquid-liquid extraction (ELLE) spans more than half a century of research. Nonetheless, a comprehensive overview has not appeared during the past few decades. Enantioselective liquid-liquid extraction is a technology of interest for a wide range of chemists and ch

  13. Analysis of aflatoxins in nonalcoholic beer using liquid-liquid extraction and ultraperformance LC-MS/MS.

    Science.gov (United States)

    Khan, Mohammad R; Alothman, Zeid A; Ghfar, Ayman A; Wabaidur, Saikh M

    2013-02-01

    Aflatoxins AFB1, AFB2, AFG1, and AFG2 are toxic secondary metabolites produced by Aspergillus flavus and Aspergillus parasiticus and posses a potential threat to food safety. In the present work, liquid-liquid extraction and ultraperformance LC-MS/MS method has been applied for the determination of four naturally occurring aflatoxins AFB1, AFB2, AFG1, and AFG2 in nonalcoholic beer. Aflatoxins extraction from nonalcoholic beer was carried out using liquid-liquid extraction procedure. The effects of solvent-types were studied to obtain maximum recovery of the target analytes with minimum contamination. Among different solvents, the aflatoxins extraction was best achieved using ethyl acetate. The obtained recoveries were ranged from 85 to 96% with good quality parameters: LOD values between 0.001 and 0.003 ng/mL, linearity of the calibration curve (r(2) > 0.999), and repeatability (run-to-run) and reproducibility (day-to-day) precisions with RSDs lower than 5% (n = 5) achieved at 0.50 ng/mL concentration. The optimized liquid-liquid extraction in combination with ultraperformance LC-MS/MS was applied successfully to the analysis of AFB1, AFB2, AFG1, and AFG2 aflatoxins in 11 nonalcoholic beers and were detected up to 15.31 ng/L in some of the samples.

  14. Selective Extraction of Bioproducts by Ionic Liquids

    Institute of Scientific and Technical Information of China (English)

    王键吉; 裴渊超; 赵扬; 张锁江

    2005-01-01

    Imidazolium based room temperature ionic liquids have been used to extract selectively L-tryptophan from fermentation broth. BF4 anion was found to enhance dramatically the partitioning of L-tryptophan into ionic liquid phase from aqueous solutions.

  15. Detection of geosmin and 2-methylisoborneol by liquid-liquid extraction-gas chromatograph mass spectrum (LLE-GCMS)and solid phase extraction-gas chromatograph mass spectrum (SPE-GCMS)

    Institute of Scientific and Technical Information of China (English)

    MA Xiaoyan; GAO Naiyun; CHEN Beibei; LI Qingsong; ZHANG Qiaoli; GU Guofen

    2007-01-01

    Two sample preparation methods were introduced and compared in this paper to establish a simple,quick and exact analysis of geosmin and 2-methylisoborneol.LC-18 column was employed in solid phase extraction (SPE),1.0 mL of hexane was adopted in liquid-liquid extraction(LLE),and the extracts were analyzed by gas chromatograph mass spectrum (GCMS) in selected ion mode.Mean recoveries of SPE were low for 2-methylisoborneol (2-MIB)and geosmin (GSM) with values below 50%.For LLE,the recoveries were satisfyingly above 50% for 2-MIB and 80% for GSM.Detection limits of the LLE method were as low as 1.0 ng/L for GSM and 5.0 ng/L for 2-MIB.A year-long investigation on odor chemicals of drinking water in Shanghai demonstrated that in the summer,there was a serious odor problem induced by a high concentration of 2-MIB.The highest concentration of 152.82 ng/L appeared in July in raw water,while GSM flocculation was minimal with concentrations below odor threshold.

  16. Simulation of Multistage Countercurrent Liquid-Liquid Extraction

    Directory of Open Access Journals (Sweden)

    Annasaheb WARADE

    2012-08-01

    Full Text Available Liquid-Liquid Extraction is one of the most significant unit operations used widely in the chemical industry for the separation of liquid-liquid mixture with the aid of an extracting solvent. There are different contacting patterns for the said purpose viz. co-current, counter current and crosscurrent and also a variety of equipments are encountered. This paper deals with the simulation of counter current liquid-liquid extraction operation for the special case of immiscible solvent using MATLAB. In this paper seven case studies have been studied and the results obtained are compared with the literature and it was found that results are in good agreement with the literature available.

  17. Separation of Asphaltenes by Polarity using Liquid-Liquid Extraction

    DEFF Research Database (Denmark)

    Andersen, Simon Ivar

    1997-01-01

    In order to investigate the nature of petroleum asphaltenes in terms of polarity a process was developed using initial liquid-liquid extraction of the oil phase followed by precipitation of the asphaltenes using n-heptane. The liquid-liquid extraction was performed using toluene-methanol mixtures...... with increasing content of toluene. Although large fractions of the crude oil (Alaska ´93) was extracted in the higher polarity solvents (high concentration of methanol), the asphaltene content of the dissolved material was low. As the toluene content increased more asphaltenes were transferred to the solvent...... of the maltene phase also increase while H/C decreases. The content of heteroatoms in the asphaltenes are relatively higher and apparently increase with the polarity of the solvent. It is concluded that these asphaltenes are indeed dominated by high molecular weight substances that cannot be extracted...

  18. Absolute Electron Extraction Efficiency of Liquid Xenon

    Science.gov (United States)

    Kamdin, Katayun; Mizrachi, Eli; Morad, James; Sorensen, Peter

    2016-03-01

    Dual phase liquid/gas xenon time projection chambers (TPCs) currently set the world's most sensitive limits on weakly interacting massive particles (WIMPs), a favored dark matter candidate. These detectors rely on extracting electrons from liquid xenon into gaseous xenon, where they produce proportional scintillation. The proportional scintillation from the extracted electrons serves to internally amplify the WIMP signal; even a single extracted electron is detectable. Credible dark matter searches can proceed with electron extraction efficiency (EEE) lower than 100%. However, electrons systematically left at the liquid/gas boundary are a concern. Possible effects include spontaneous single or multi-electron proportional scintillation signals in the gas, or charging of the liquid/gas interface or detector materials. Understanding EEE is consequently a serious concern for this class of rare event search detectors. Previous EEE measurements have mostly been relative, not absolute, assuming efficiency plateaus at 100%. I will present an absolute EEE measurement with a small liquid/gas xenon TPC test bed located at Lawrence Berkeley National Laboratory.

  19. Planar graphene oxide-based magnetic ionic liquid nanomaterial for extraction of chlorophenols from environmental water samples coupled with liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Cai, Mei-Qiang; Su, Jie; Hu, Jian-Qiang; Wang, Qian; Dong, Chun-Ying; Pan, Sheng-Dong; Jin, Mi-Cong

    2016-08-12

    A planar graphene oxide-based magnetic ionic liquid nanomaterial (PGO-MILN) was synthesized. The prepared PGO-MILN was characterized by transmission electronmicroscopy (TEM) and Fourier-transform infrared spectrometry (FTIR). The results of adsorption experiments showed that the PGO-MILN had great adsorption capacity for 2-chlorophenol (2-CP), 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP) and pentachlorophenol (PCP). Based on the adsorption experimental data, a sensitive magnetic method for determination of the five CPs in environmental water samples was developed by an effective magnetic solid-phase extraction (MSPE) procedure coupled with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The effects of main MSPE parameters including the solution pH, extraction time, desorption time, and volume of desorption solution on the extraction efficiencies had been investigated in detail. The recoveries ranged from 85.3 to 99.3% with correlation coefficients (r) higher than 0.9994 and the linear ranges were between 10 and 500ngL(-1). The limits of detection (LODs) and limits of quantification (LOQs) of the five CPs ranged from 0.2 to 2.6ngL(-1) and 0.6 to 8.7ngL(-1), respectively. The intra- and inter- day relative standard deviations (RSDs) were in the range from 0.6% to 7.4% and from 0.7% to 8.4%, respectively. It was confirmed that the PGO-MILN was a kind of highly effective MSPE materials used for enrichment of trace CPs in the environmental water. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. APPARATUS FOR LIQUID PHASE EXTRACTION

    Science.gov (United States)

    Hicks, T.R.; Lehman, H.R.; Rubin, B.

    1958-09-16

    operation is described. It comprises a tubular colunm having upper and lower enlarged terminal portions, and a constricted central section containing fluid dispersal packing. Pulsing means are coupled to the upper portion of the column. The inlet for the less dense phase is located above the inlet for the denser phase and both are positioned so that liquids enter the constricted packingfilled central section. The apparatos also includes an interfacing level control, and means fer sensing the level of the interface actuate apparatus for controlling the rate of flow of input or discharge. The outlet for the less dense phase is located in the upper packing free portion of the colunm and that of the denser phase in the lower portion.

  1. Ultratrace-level determination of glyphosate, aminomethylphosphonic acid and glufosinate in natural waters by solid-phase extraction followed by liquid chromatography-tandem mass spectrometry: performance tuning of derivatization, enrichment and detection.

    Science.gov (United States)

    Hanke, Irene; Singer, Heinz; Hollender, Juliane

    2008-07-01

    A sensitive and robust analytical method for the quantification of glyphosate, aminomethylphosphonic acid (AMPA) and glufosinate in natural water has been developed on the basis of a derivatization with 9-fluorenylmethylchloroformate (FMOC-Cl), solid-phase extraction (SPE) and liquid chromatography followed by electrospray tandem mass spectrometry (LC-ESI-MS/MS). In order to maximize sensitivity, the derivatization was optimized regarding organic solvent content, amount of FMOC-Cl and reaction time. At an acetonitrile content of 10% a derivatization yield of 100% was reached within two hours in groundwater and surface water samples. After a twofold dilution the low acetonitrile content allowed solid-phase extraction of a sample of originally 80 mL over 200 mg Strata-X cartridges. In order to decrease the load of the LC column and mass spectrometer with derivatization by-products (e.g., 9-fluorenylmethanol FMOC-OH), a rinsing step was performed for the SPE cartridge with dichloromethane. Acidification of the sample and addition of EDTA was used to minimize complexation of the target compounds with metal ions in environmental samples. Due to the large sample volume and the complete FMOC-OH removal, limits of quantification of 0.7 ng/L, 0.8 ng/L and 2.3 ng/L were achieved in surface water for glyphosate, AMPA and glufosinate, respectively. The limits of detection were as low as 0.2 ng/L, 0.2 ng/L and 0.6 ng/L for glyphosate, AMPA and glufosinate, respectively. Surface water and ground water samples spiked at 2 ng/L showed recoveries of 91-107%.

  2. Optimized liquid-liquid extractive rerefining of spent lubricants.

    Science.gov (United States)

    Kamal, Muhammad Ashraf; Naqvi, Syed Mumtaz Danish; Khan, Fasihullah

    2014-01-01

    Central composite design methodology has been employed to model the sludge yield data obtained during liquid-liquid extractive rerefining of spent lubricants using an alcohol (1-butanol) and a ketone (methyl ethyl ketone) as prospective solvents. The study has resulted in two reasonably accurate multivariate process models that relate the sludge yield (R (2) = 0.9065 and 0.9072 for alcohol and ketone, resp.) to process variables (settling time t, operating temperature T, and oil to solvent ratio r). Construction of such models has allowed the maximization of the sludge yield (more than 8% and 3% in case of alcohol and ketone, resp.) so that the extraction of useable oil components from spent lubricants can economically be performed under extremely mild conditions (t = 16.7 h, T = 10°C, and r = 2) and fairly moderate conditions (t = 26.6 h, T = 10°C, and r = 5) established for the alcohol and ketone correspondingly. Based on these performance parameters alcohol appears to be superior over ketone for this extraction process. Additionally extractive treatment results in oil stocks with lesser quantity of environmentally hazardous polyaromatic hydrocarbons that are largely left in the separated sludge.

  3. Optimized Liquid-Liquid Extractive Rerefining of Spent Lubricants

    Directory of Open Access Journals (Sweden)

    Muhammad Ashraf Kamal

    2014-01-01

    Full Text Available Central composite design methodology has been employed to model the sludge yield data obtained during liquid-liquid extractive rerefining of spent lubricants using an alcohol (1-butanol and a ketone (methyl ethyl ketone as prospective solvents. The study has resulted in two reasonably accurate multivariate process models that relate the sludge yield (R2=0.9065 and 0.9072 for alcohol and ketone, resp. to process variables (settling time t, operating temperature T, and oil to solvent ratio r. Construction of such models has allowed the maximization of the sludge yield (more than 8% and 3% in case of alcohol and ketone, resp. so that the extraction of useable oil components from spent lubricants can economically be performed under extremely mild conditions (t = 16.7 h, T=10°C, and r=2 and fairly moderate conditions (t = 26.6 h, T=10°C, and r=5 established for the alcohol and ketone correspondingly. Based on these performance parameters alcohol appears to be superior over ketone for this extraction process. Additionally extractive treatment results in oil stocks with lesser quantity of environmentally hazardous polyaromatic hydrocarbons that are largely left in the separated sludge.

  4. Liquid-Liquid Extraction in Systems Containing Butanol and Ionic Liquids – A Review

    Directory of Open Access Journals (Sweden)

    Kubiczek Artur

    2017-03-01

    Full Text Available Room-temperature ionic liquids (RTILs are a moderately new class of liquid substances that are characterized by a great variety of possible anion-cation combinations giving each of them different properties. For this reason, they have been termed as designer solvents and, as such, they are particularly promising for liquid-liquid extraction, which has been quite intensely studied over the last decade. This paper concentrates on the recent liquid-liquid extraction studies involving ionic liquids, yet focusing strictly on the separation of n-butanol from model aqueous solutions. Such research is undertaken mainly with the intention of facilitating biological butanol production, which is usually carried out through the ABE fermentation process. So far, various sorts of RTILs have been tested for this purpose while mostly ternary liquid-liquid systems have been investigated. The industrial design of liquid-liquid extraction requires prior knowledge of the state of thermodynamic equilibrium and its relation to the process parameters. Such knowledge can be obtained by performing a series of extraction experiments and employing a certain mathematical model to approximate the equilibrium. There are at least a few models available but this paper concentrates primarily on the NRTL equation, which has proven to be one of the most accurate tools for correlating experimental equilibrium data. Thus, all the presented studies have been selected based on the accepted modeling method. The reader is also shown how the NRTL equation can be used to model liquid-liquid systems containing more than three components as it has been the authors’ recent area of expertise.

  5. PERFORMANCE OF A PACKED LIQUID-LIQUID EXTRACTION COLUMN

    Directory of Open Access Journals (Sweden)

    İ. Metin HASDEMİR

    1999-03-01

    Full Text Available The influence of feed ratios ((LE/LR on the performance of a packed liquid-liquid extraction column, with a diameter of 5.86 cm and a column height of 132 cm was investigated. The column is made of borosilicate glass and packed with 10 x 10 mm glass Raschig rings. In this study, a ternary system composed of water + propionic acid + trichloroethylene was used. The data used to triangular diagram were obtained experimentally. The overall mass transfer coefficients, the numbers of overall mass transfer units, the heights of mass transfer units, the numbers of theoretical stages and height equivalent to a theoretical stage (H. E. T. S. values were calculated and compared with each other.

  6. Magnetic microsphere-confined graphene for the extraction of polycyclic aromatic hydrocarbons from environmental water samples coupled with high performance liquid chromatography-fluorescence analysis.

    Science.gov (United States)

    Wang, Weina; Ma, Ruiyang; Wu, Qiuhua; Wang, Chun; Wang, Zhi

    2013-06-07

    In this paper, a magnetic microsphere-confined graphene adsorbent (Fe3O4@SiO2-G) was fabricated and used for the extraction of five polycyclic aromatic hydrocarbons (fluorene, anthracene, phenanthrene, fluoranthene and pyrene) from environmental water samples prior to high performance liquid chromatography with fluorescence detection. The Fe3O4@SiO2-G was characterized by various instrumental methods. Various experimental parameters that could affect the extraction efficiencies, such as the amount of Fe3O4@SiO2-G, the pH and ionic strength of sample solution, the extraction time and the desorption conditions, were investigated. Due to the high surface area and excellent adsorption capacity of the Fe3O4@SiO2-G, satisfactory extraction can be achieved with only 15mg of the adsorbent per 250mL solution and 5min extraction. Under the optimum conditions, a linear response was observed in the concentration range of 5-1500ngL(-1) for fluorene, 2.5-1500ngL(-1) for anthracene and 15-1500ngL(-1) for phenanthrene, fluoranthene and pyrene, with the correlation coefficients (r) ranging from 0.9897 to 0.9961. The limits of detection (S/N=3) of the method were between 0.5 and 5.0ngL(-1). The relative standard deviations (RSDs) were less than 5.6%. The recoveries of the method were in the range between 83.2% and 108.2%. The results indicated that this graphene-based magnetic nanocomposite had a great adsorptive ability toward the five polycyclic aromatic hydrocarbons from environmental water samples.

  7. Separating closely resembling steroids with ionic liquids in liquid-liquid extraction systems

    NARCIS (Netherlands)

    Vitasari, C.R.; Gramblicka, M.; Gibcus, K.; Visser, T.J.; Geertman, R.M.; Schuur, B.

    2015-01-01

    Separation of steroids by liquid–liquid extraction with ionic liquids (ILs) as solvent was studied both experimentally and by simulation using a model mixture of progesterone and pregnenolone. The studies involved a solvent screening using COSMO-RS software for estimation of progesterone solubility.

  8. Sample clean-up, enrichment and determination of s-triazine herbicides from southern ethiopian lakes supported using liquid membrane extraction

    Directory of Open Access Journals (Sweden)

    Jan Åke Jönsson

    2000-06-01

    Full Text Available The liquid membrane extraction method has been employed for selectively extracting trace quantities of s-triazine herbicides in environmental waters collected from lakes Awassa, Chamo and Abbya, located in close proximity to the agricultural farms in Southern Ethiopia. In liquid membrane extraction, the uncharged triazine compounds from the flowing donor solution diffuse through a porous poly(tetrafluoroethylene (PTFE membrane, containing a water immiscible organic solvent. The s-triazine molecules are then irreversibly trapped in the stagnant acidic acceptor phase since they become protonated. Using both di-n-hexylether and n-undecane membrane solvents, s-traizine herbicides were extracted and low detection limits of about 1 ng/L have been obtained by extraction of three liters of sample solution spiked with 0.1 g/L of each triazine. Residues of atrazine and terbutryn ranging in concentration from 0.02 to 0.05 g/L have been successfully determined.

  9. Liquid-liquid extraction for surfactant-contaminant separation and surfactant reuse

    Energy Technology Data Exchange (ETDEWEB)

    Hasegawa, M.A. [Surbec Environmental, Norman, OK (United States); Sabatini, D.A.; Harwell, J.H. [Univ. of Oklahoma, Norman, OK (United States)

    1997-07-01

    Liquid-liquid extraction was investigated for use with surfactant enhanced subsurface remediation. A surfactant liquid-liquid extraction model (SLLEM) was developed for batch equilibrium conditions based on contaminant partitioning between micellar, water, and solvent phases. The accuracy of this fundamental model was corroborated with experimental results (using naphthalene and phenanthrene as contaminants and squalane as the extracting solvent). The SLLEM model was then expanded to nonequilibrium conditions. The effectiveness of this nonequilibrium model was corroborated with experimental results from continuous flow hollow fiber membrane systems. The validated models were used to conduct a sensitivity analysis evaluating the effects of surfactants on the removal of the contaminants in liquid-liquid extraction systems. In addition, liquid-liquid extraction is compared to air stripping for surfactant-contaminant separation. Finally, conclusions are drawn as to the impact of surfactants on liquid-liquid extraction processes, and the significance of these impacts on the optimization of surfactant-enhanced subsurface remediation.

  10. Batch liquid-liquid extraction of phenol from aqueous solutions

    Energy Technology Data Exchange (ETDEWEB)

    Palma, M.S.A.; Shibata, C. [Department of Biochemical Pharmaceutical Technology, Faculty of Pharmaceutical Sciences, University of Sao Paulo, Sao Paulo-SP (Brazil); Paiva, J.L. [Department of Chemical Engineering, Polytechnical School, University of Sao Paulo, Sao Paulo-SP (Brazil); Zilli, M. [Department of Chemical and Process Engineering, University of Genoa, Genoa (Italy); Converti, A.

    2010-01-15

    The aim of this work is the study of batch liquid-liquid extraction of phenol from aqueous solutions in a bench-scale well-mixed reactor. The influence of the ratio of phase volumes, temperature, and rotational speed on phenol removal (0.72-1.1 % w/w) was investigated using methyl isobutyl ketone as an extracting solvent. For this purpose, the ratio of phase volumes were set at 0.1 and 0.2, the temperature at 10, 20, and 30 C, and the rotational speed at 300, 400, and 500 rpm. A physical model based on the material balance of the phases as well as the equation of mass flux between the phases allowed the estimation of the overall coefficient of mass transfer coupled with the superficial area. Moreover, it proved to fit, satisfactorily well, the experimental data of residual phenol concentration in the organic phase versus time under all the conditions investigated. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

  11. Supercritical Fluid Chromatography, Pressurized Liquid Extraction and Supercritical Fluid Extraction

    Energy Technology Data Exchange (ETDEWEB)

    Henry, Matthew C.; Yonker, Clement R.

    2006-06-15

    In this review we examine the related fields of supercritical fluid chromatography (SFC) and supercritical fluid extraction (SFE). We reviewed the published literature in the period from November 2003 to November 2005. Well over 300 papers were published in this period. This large body of work indicates continuing active growth of the field, but an exhaustive review is beyond the scope of this work. We have chosen to include a sampling of publications that best represent the continuing trends and new ideas in the field. In keeping with past reviews on this subject1, we have broadened our scope to include fluid systems operating at high temperature and pressure, but below the critical point. Various terms have been applied to this state: sub-critical fluid extraction, pressurized liquid extraction, and accelerated solvent extraction. The term accelerated solvent extraction has been used by instrument manufacturers to refer to this process, but we will use the more descriptive term pressurized liquid extraction (PLE) to refer to these systems. Most of the research in the field is of an “evolutionary” rather than “revolutionary” nature. As in the previous review period, applications papers make up a majority of the published work. Pharmaceutical applications continue to be a strong theme. Most of the pharmaceutical work has centered on preparative, rather than analytical, separations. Chiral separations are an exception, as analytical scale separations of chiral compounds are an area of intense interest. Food and natural products represent the next largest body of work. Major themes are the isolation and characterization of high-value added foodstuffs, fragrances, and flavor compounds from novel natural materials or agricultural by-products. The areas of food, natural products, and pharmaceutical separation science converge in the area of so-called nutraceuticals. These are typically high-value products, either sold alone or as part of a fortified food, that

  12. Determination of isoxaflutole (balance) and its metabolites in water using solid phase extraction followed by high-performance liquid chromatography with ultraviolet or mass spectrometry

    Science.gov (United States)

    Lin, Chung-Ho; Lerch, Robert N.; Thurman, E. Michael; Garrett , Harold E.; George, Milon F.

    2002-01-01

    Balance (isoxaflutole, IXF) belongs to a new family of herbicides referred to as isoxazoles. IXF has a very short soil half-life (<24 h), degrading to a biologically active diketonitrile (DKN) metabolite that is more polar and considerably more stable. Further degradation of the DKN metabolite produces a nonbiologically active benzoic acid (BA) metabolite. Analytical methods using solid phase extraction followed by high-performance liquid chromatography−UV (HPLC-UV) or high-performance liquid chromatography−mass spectrometry (HPLC-MS) were developed for the analysis of IXF and its metabolites in distilled deionized water and ground water samples. To successfully detect and quantify the BA metabolite by HPLC-UV from ground water samples, a sequential elution scheme was necessary. Using HPLC-UV, the mean recoveries from sequential elution of the parent and its two metabolites from fortified ground water samples ranged from 68.6 to 101.4%. For HPLC-MS, solid phase extraction of ground water samples was performed using a polystyrene divinylbenzene polymer resin. The mean HPLC-MS recoveries of the three compounds from ground water samples spiked at 0.05−2 μg/L ranged from 100.9 to 110.3%. The limits of quantitation for HPLC-UV are approximately 150 ng/L for IXF, 100 ng/L for DKN, and 250 ng/L for BA. The limit of quantitation by HPLC-MS is 50 ng/L for each compound. The methods developed in this work can be applied to determine the transport and fate of Balance in the environment.

  13. Membrane contactor assisted extraction/reaction process employing ionic liquids

    Science.gov (United States)

    Lin, Yupo J.; Snyder, Seth W.

    2012-02-07

    The present invention relates to a functionalized membrane contactor extraction/reaction system and method for extracting target species from multi-phase solutions utilizing ionic liquids. One preferred embodiment of the invented method and system relates to an extraction/reaction system wherein the ionic liquid extraction solutions act as both extraction solutions and reaction mediums, and allow simultaneous separation/reactions not possible with prior art technology.

  14. Determination of Niacinamide in Lotions and Creams Using Liquid-Liquid Extraction and High-Performance Liquid Chromatography

    Science.gov (United States)

    Usher, Karyn M.; Simmons, Carolyn R.; Keating, Daniel W.; Rossi, Henry F., III

    2015-01-01

    Chemical separations are an important part of an undergraduate chemistry curriculum. Sophomore students often get experience with liquid-liquid extraction in organic chemistry classes, but liquid-liquid extraction is not as often introduced as a quantitative sample preparation method in honors general chemistry or quantitative analysis classes.…

  15. Determination of Niacinamide in Lotions and Creams Using Liquid-Liquid Extraction and High-Performance Liquid Chromatography

    Science.gov (United States)

    Usher, Karyn M.; Simmons, Carolyn R.; Keating, Daniel W.; Rossi, Henry F., III

    2015-01-01

    Chemical separations are an important part of an undergraduate chemistry curriculum. Sophomore students often get experience with liquid-liquid extraction in organic chemistry classes, but liquid-liquid extraction is not as often introduced as a quantitative sample preparation method in honors general chemistry or quantitative analysis classes.…

  16. Liquid-Liquid-Liquid Three Phase Extraction Apparatus: Operation Strategy and Influences on Mass Transfer Efficiency

    Institute of Scientific and Technical Information of China (English)

    何秀琼; 黄昆; 于品华; 张超; 谢铿; 李鹏飞; 王娟; 安震涛; 刘会洲

    2012-01-01

    Abstract A new mixer-settler-mixer three chamber integrated extractor is proposed in this work for liquid-liquid- liquid three phase countercurrent and continuous extraction. Experiments revealed the influences of the structural design of the three-liquid-phase extractor and some key operational parameters on three-phase partition of two phenolic isomers, p-nitrophenol (p-NP) and o-nitrophenol (o-NP). The model three-liquid-phase extraction system used here is nonane (organic top-plaase)-polyethylene glycol (PEG 20UU) (polymer mlddle-phase)-(NH4)2SO4 aqueous solution (aqueous bottom-phase). It is indicated that agitating speed and retention time in three-phase mixer are key parameters to extraction fraction of nitrophenol. Dispersion band behavior is related to agitating intensity, and its occurrence does not affect the extraction fraction of target compounds. The present work highlights the possibility of a feasible approach of scaling up of the proposed three-phase extraction apparatus for future in- dustrial-aimed applications.

  17. Improved detection of multiple environmental antibiotics through an optimized sample extraction strategy in liquid chromatography-mass spectrometry analysis.

    Science.gov (United States)

    Yi, Xinzhu; Bayen, Stéphane; Kelly, Barry C; Li, Xu; Zhou, Zhi

    2015-12-01

    A solid-phase extraction/liquid chromatography/electrospray ionization/multi-stage mass spectrometry (SPE-LC-ESI-MS/MS) method was optimized in this study for sensitive and simultaneous detection of multiple antibiotics in urban surface waters and soils. Among the seven classes of tested antibiotics, extraction efficiencies of macrolides, lincosamide, chloramphenicol, and polyether antibiotics were significantly improved under optimized sample extraction pH. Instead of only using acidic extraction in many existing studies, the results indicated that antibiotics with low pK a values (antibiotics with high pK a values (>7) were extracted more efficiently under neutral conditions. The effects of pH were more obvious on polar compounds than those on non-polar compounds. Optimization of extraction pH resulted in significantly improved sample recovery and better detection limits. Compared with reported values in the literature, the average reduction of minimal detection limits obtained in this study was 87.6% in surface waters (0.06-2.28 ng/L) and 67.1% in soils (0.01-18.16 ng/g dry wt). This method was subsequently applied to detect antibiotics in environmental samples in a heavily populated urban city, and macrolides, sulfonamides, and lincomycin were frequently detected. Antibiotics with highest detected concentrations were sulfamethazine (82.5 ng/L) in surface waters and erythromycin (6.6 ng/g dry wt) in soils. The optimized sample extraction strategy can be used to improve the detection of a variety of antibiotics in environmental surface waters and soils.

  18. Routine determination of sulfonylurea, imidazolinone, and sulfonamide herbicides at nanogram-per-liter concentrations by solid-phase extraction and liquid chromatography/mass spectrometry

    Science.gov (United States)

    Furlong, E.T.; Burkhardt, M.R.; Gates, Paul M.; Werner, S.L.; Battaglin, W.A.

    2000-01-01

    Sulfonylurea (SU), imidazolinone (IMI), and sulfonamide (SA) herbicides are new classes of low-application-rate herbicides increasingly used by farmers. Some of these herbicides affect both weed and crop species at low dosages and must be carefully used. Less is known about the effect of these compounds on non-crop plant species, but a concentration of 100 ng/l in water has been proposed as the threshold for possible plant toxicity for most of these herbicides. Hence, analytical methods must be capable of detecting SUs, IMIs, and SAs at concentrations less than 100 ng/l in ambient water samples. The authors developed a two-cartridge, solid-phase extraction method for isolating 12 SU, 3 IMI, and 1 SA herbicides by using high-performance liquid chromatography/electrospray ionization-mass spectrometry (HPLC/ESI-MS) to identify and quantify these herbicides to 10 ng/l. This method was used to analyze 196 surface- and ground-water samples collected from May to August 1998 throughout the Midwestern United States, and more than 100 quality-assurance and quality-control samples. During the 16 weeks of the study, the HPLC/ESI-MS maintained excellent calibration linearity across the calibration range from 5 to 500 ng/l, with correlation coefficients of 0.9975 or greater. Continuing calibration verification standards at 100-ng/l concentration were analyzed throughout the study, and the average measured concentrations for individual herbicides ranged from 93 to 100 ng/l. Recovery of herbicides from 27 reagent-water samples spiked at 50 and 100 ng/l ranged from 39 to 92%, and averaged 73%. The standard deviation of recoveries ranged from 14 to 26%, and averaged 20%. This variability reflects multiple instruments, operators, and the use of automated and manual sample preparation. Spiked environmental water samples had similar recoveries, although for some herbicides, the sample matrix enhanced recoveries by as much as 200% greater than the spiked concentration. This matrix

  19. Determining estrogenic steroids in Taipei waters and removal in drinking water treatment using high-flow solid-phase extraction and liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Chen, Chia-Yang; Wen, Tzu-Yao; Wang, Gen-Shuh; Cheng, Hui-Wen; Lin, Ying-Hsuan; Lien, Guang-Wen

    2007-06-01

    River water and wastewater treatment plant (WWTP) effluents from metropolitan Taipei, Taiwan were tested for the presence of the pollutants estrone (E1), estriol (E3), 17beta-estradiol (E2), and 17alpha-ethinylestradiol (EE2) using a new methodology that involves high-flow solid-phase extraction and liquid chromatography/tandem mass spectrometry. The method was also used to investigate the removal of the analytes by conventional drinking water treatment processes. Without adjusting the pH, we extracted 1-L samples with PolarPlus C18 Speedisks under a flow rate exceeding 100 mL/min, in which six samples could be done simultaneously using an extraction station. The adsorbent was washed with 40% methanol/60% water and then eluted by 50% methanol/50% dichloromethane. The eluate was concentrated until almost dry and was reconstituted by 20 microL of methanol. Quantitation was done by LC-MS/MS-negative electrospray ionization in the selected reaction monitoring mode with isotope-dilution techniques. The mobile phase was 10 mM N-methylmorpholine aqueous solution/acetonitrile with gradient elution. Mean recoveries of spiked Milli-Q water were 65-79% and precisions were within 2-20% of the tested concentrations (5.0-200 ng/L). The method was validated with spiked upstream river water; precisions were most within 10% of the tested concentrations (10-100 ng/L) with most RSDswater matrix may also impact analyte recoveries along with ion suppression. In the Taipei water study, the four steroid estrogens were detected in river samples (ca. 15 ng/L for E2 and EE2 and 35-45 ng/L for E1 and E3). Average levels of 19-26 ng/L for E1, E2, and EE2 were detected in most wastewater effluents, while only a single effluent sample contained E3. The higher level in the river was likely caused by the discharge of untreated human and farming waste into the water. In the drinking water treatment simulations, coagulation removed 20-50% of the estrogens. An increased dose of aluminum sulfate did

  20. Ionic liquid based dispersive liquid-liquid microextraction for the extraction of pesticides from bananas.

    Science.gov (United States)

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Asensio-Ramos, María; Rodríguez-Delgado, Miguel Angel

    2009-10-23

    This paper describes a dispersive liquid-liquid microextraction (DLLME) procedure using room temperature ionic liquids (RTILs) coupled to high-performance liquid chromatography with diode array detection capable of quantifying trace amounts of eight pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox and fenazaquin) in bananas. Fruit samples were first homogenized and extracted (1g) with acetonitrile and after suitable evaporation and reconstitution of the extract in 10 mL of water, a DLLME procedure using 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) as extraction solvent was used. Experimental conditions affecting the DLLME procedure (sample pH, sodium chloride percentage, ionic liquid amount and volume of disperser solvent) were optimized by means of an experimental design. In order to determine the presence of a matrix effect, calibration curves for standards and fortified banana extracts (matrix matched calibration) were studied. Mean recovery values of the extraction of the pesticides from banana samples were in the range of 69-97% (except for thiophanate-methyl and carbofuran, which were 53-63%) with a relative standard deviation lower than 8.7% in all cases. Limits of detection achieved (0.320-4.66 microg/kg) were below the harmonized maximum residue limits established by the European Union (EU). The proposed method, was also applied to the analysis of this group of pesticides in nine banana samples taken from the local markets of the Canary Islands (Spain). To the best of our knowledge, this is the first application of RTILs as extraction solvents for DLLME of pesticides from samples different than water.

  1. NGL Viewer: a web application for molecular visualization.

    Science.gov (United States)

    Rose, Alexander S; Hildebrand, Peter W

    2015-07-01

    The NGL Viewer (http://proteinformatics.charite.de/ngl) is a web application for the visualization of macromolecular structures. By fully adopting capabilities of modern web browsers, such as WebGL, for molecular graphics, the viewer can interactively display large molecular complexes and is also unaffected by the retirement of third-party plug-ins like Flash and Java Applets. Generally, the web application offers comprehensive molecular visualization through a graphical user interface so that life scientists can easily access and profit from available structural data. It supports common structural file-formats (e.g. PDB, mmCIF) and a variety of molecular representations (e.g. 'cartoon, spacefill, licorice'). Moreover, the viewer can be embedded in other web sites to provide specialized visualizations of entries in structural databases or results of structure-related calculations. © The Author(s) 2015. Published by Oxford University Press on behalf of Nucleic Acids Research.

  2. NGL Viewer: a web application for molecular visualization

    Science.gov (United States)

    Rose, Alexander S.; Hildebrand, Peter W.

    2015-01-01

    The NGL Viewer (http://proteinformatics.charite.de/ngl) is a web application for the visualization of macromolecular structures. By fully adopting capabilities of modern web browsers, such as WebGL, for molecular graphics, the viewer can interactively display large molecular complexes and is also unaffected by the retirement of third-party plug-ins like Flash and Java Applets. Generally, the web application offers comprehensive molecular visualization through a graphical user interface so that life scientists can easily access and profit from available structural data. It supports common structural file-formats (e.g. PDB, mmCIF) and a variety of molecular representations (e.g. ‘cartoon, spacefill, licorice’). Moreover, the viewer can be embedded in other web sites to provide specialized visualizations of entries in structural databases or results of structure-related calculations. PMID:25925569

  3. Liquid-Liquid Extraction of Insecticides from Juice: An Analytical Chemistry Laboratory Experiment

    Science.gov (United States)

    Radford, Samantha A.; Hunter, Ronald E., Jr.; Barr, Dana Boyd; Ryan, P. Barry

    2013-01-01

    A laboratory experiment was developed to target analytical chemistry students and to teach them about insecticides in food, sample extraction, and cleanup. Micro concentrations (sub-microgram/mL levels) of 12 insecticides spiked into apple juice samples are extracted using liquid-liquid extraction and cleaned up using either a primary-secondary…

  4. Liquid-Liquid Extraction of Insecticides from Juice: An Analytical Chemistry Laboratory Experiment

    Science.gov (United States)

    Radford, Samantha A.; Hunter, Ronald E., Jr.; Barr, Dana Boyd; Ryan, P. Barry

    2013-01-01

    A laboratory experiment was developed to target analytical chemistry students and to teach them about insecticides in food, sample extraction, and cleanup. Micro concentrations (sub-microgram/mL levels) of 12 insecticides spiked into apple juice samples are extracted using liquid-liquid extraction and cleaned up using either a primary-secondary…

  5. Determination of androgens and progestogens in environmental and biological samples using fabric phase sorptive extraction coupled to ultra-high performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Guedes-Alonso, Rayco; Ciofi, Lorenzo; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan; Bubba, Massimo Del; Kabir, Abuzar; Furton, Kenneth G

    2016-03-11

    Androgens and progestogens are two important groups of endocrine disrupting compounds (EDCs) which are implicated to produce severe detrimental impact over aquatic biota, even at very low concentrations of ngL(-1). For this reason, one of the major challenges to analytical chemists is the development of sensitive and selective extraction processes which allow the rapid and green determination of these emerging pollutants at low concentrations in environmental samples. Fabric phase sorptive extraction is a new, highly sensitive, efficient and solvent minimized technique which combine the advantages of sol-gel derived microextraction sorbents and the rich surface chemistry of cellulose fabric substrate. This process has several advantages such as minimum usage of organic solvents, short extraction times, small sample volumes and high analyte preconcentration factors. In this study, an extraction method based on sorptive fabric phase coupled to ultra-high-performance liquid chromatography tandem mass spectrometry detection (FPSE-UHPLC-MS/MS) has been developed for the determination of four progestogens and six androgens in environmental and biological samples. All the parameters involved in the extraction, such as sample volume, extraction and desorption times, desorption solvent volume and sample pH values have been optimized. The developed method provides satisfactory limits of detection (between 1.7 and 264ngL(-1)), good recoveries and low relative standard deviations (below 10% in tap and osmosis water and below 20% in wastewater and urine). Subsequently, the method was used to analyse tap water, wastewater treated with different processing technologies and urine samples. The concentrations of the detected hormones ranged from 28.3 to 227.3 ngL(-1) in water samples and from 1.1 to 3.7μgL(-1) in urine samples.

  6. Pesticide extraction from table grapes and plums using ionic liquid based dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Herrera-Herrera, Antonio V; Rodríguez-Delgado, Miguel Angel

    2009-12-01

    Room temperature ionic liquids (RTILs) have been used as extraction solvents in dispersive liquid-liquid microextraction (DLLME) for the determination of eight multi-class pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox, and fenazaquin) in table grapes and plums. The developed method involves the combination of DLLME and high-performance liquid chromatography with diode array detection. Samples were first homogenized and extracted with acetonitrile. After evaporation and reconstitution of the extract in water containing sodium chloride, a quick DLLME procedure that used the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) and methanol was developed. The RTIL dissolved in a very small volume of acetonitrile was directed injected in the chromatographic system. The comparison between the calibration curves obtained from standards and from spiked sample extracts (matrix-matched calibration) showed the existence of a strong matrix effect for most of the analyzed pesticides. A recovery study was also developed with five consecutive extractions of the two types of fruits spiked at three concentration levels. Mean recovery values were in the range of 72-100% for table grapes and 66-105% for plum samples (except for thiophanate-methyl and carbofuran, which were 64-75% and 58-66%, respectively). Limits of detection (LODs) were in the range 0.651-5.44 microg/kg for table grapes and 0.902-6.33 microg/kg for plums, representing LODs below the maximum residue limits (MRLs) established by the European Union in these fruits. The potential of the method was demonstrated by analyzing 12 commercial fruit samples (six of each type).

  7. High-throughput liquid-liquid extraction in 96-well format: Parallel artificial liquid membrane extraction

    DEFF Research Database (Denmark)

    Gjelstad, Astrid; Andresen, Alf Terje; Dahlgren, Anders

    2017-01-01

    , highly efficient sample cleanup, and direct compatibility with liquid chromatography–mass spectrometry (LC–MS). The consumption of hazardous organic solvents is also almost eliminated using PALME as the sample preparation technique. This article summarizes current experiences with PALME, based on work...

  8. Kinetics of glycoalkaloid hydrolysis and solanidine extraction in liquid-liquid systems

    Directory of Open Access Journals (Sweden)

    Stanković Mihajlo Z.

    2002-01-01

    Full Text Available The kinetics of glycoalkaloid hydrolysis and solanidine extraction in Analyzed in this study. obtained from dried and milled potato haulm to to which hydrochlotic acid was added is the first liquid phase, while chloroform trichloroethylene or carbon tetrachlondeisthe second organic, liquid phase. The purpose of this paper was to combine the processes of glycoalkaloid hydrolysis to solanidine and solanidine extraction into one step, and to find the optimal liquid-liquid system for such a process.

  9. Determination of sulfadiazine in phosphate- and DOC-rich agricultural drainage water using solid-phase extraction followed by liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Bouyou, P.A. Léon; Weisser, Johan Juhl; Strobel, Bjarne W.

    2014-01-01

    Trace levels of the veterinary antibiotic compound sulfadiazine (SDZ) can be determined in agricultural drainage water samples with this new method. Optimized sample pretreatment and solid-phase extraction was combined with liquid chromatography coupled to tandem mass spectrometry (SPE LC......-MS/MS) using positive electrospray ionization. The linear dynamic range for the LC-MS/MS was assessed from 5 μg/L to 25 mg/L with a 15-point calibration curve displaying a coefficient of correlation r 2 = 0.9915. Agricultural drainage water spiked at a concentration of 25 ng/L gave recoveries between 63 and 98...... % (relative standard deviation 15 %), while at 10 ng/L, it showed a lower recovery of 32 % (relative standard deviation 47 %). The final SPE LC-MS/MS method had a limit of detection (LOD)Method and a limit of quantification (LOQ)Method of 7.5 and 23 ng/L agricultural drainage water, respectively...

  10. Modeling of the thyme: Liquid carbon dioxide extraction system

    Directory of Open Access Journals (Sweden)

    Zeković Zoran P.

    2003-01-01

    Full Text Available The extraction of thyme (Thymus vulgaris L by liquid carbon dioxide was investigated. The obtained extracts were analyzed by HPLC and GC-MS methods, and their composition was compared with that of the essential oil obtained by steam distillation and by supercritical carbon dioxide at 100 bar and 40°C. To model extraction of the thyme - liquid carbon dioxide system, we used the Reverchon - Sesti Osseo equation, as well as our modified equation.

  11. Small volume liquid extraction of amphetamines in saliva.

    Science.gov (United States)

    Meng, Pinjia; Wang, Yanyan

    2010-04-15

    The present study introduced a procedure of small volume liquid extraction of amphetamines, including amphetamine (AM); methamphetamine (MA); 3,4-methylenedioxyamphetamine (MDA); 3,4-methylenemethamphtamine (MDMA), in saliva. Extraction efficiencies were compared between the conventional volume liquid phase extraction (LPE) and the small volume one, in which amphetamine abusers, and was proven to be practical for detecting trace amounts of amphetamines in saliva.

  12. A microfluidic study of liquid-liquid extraction mediated by carbon dioxide.

    Science.gov (United States)

    Lestari, Gabriella; Salari, Alinaghi; Abolhasani, Milad; Kumacheva, Eugenia

    2016-07-05

    Liquid-liquid extraction is an important separation and purification method; however, it faces a challenge in reducing the energy consumption and the environmental impact of solvent (extractant) recovery. The reversible chemical reactions of switchable solvents (nitrogenous bases) with carbon dioxide (CO2) can be implemented in reactive liquid-liquid extraction to significantly reduce the cost and energy requirements of solvent recovery. The development of new effective switchable solvents reacting with CO2 and the optimization of extraction conditions rely on the ability to evaluate and screen the performance of switchable solvents in extraction processes. We report a microfluidic strategy for time- and labour-efficient studies of CO2-mediated solvent extraction. The platform utilizes a liquid segment containing an aqueous extractant droplet and a droplet of a solution of a switchable solvent in a non-polar liquid, with gaseous CO2 supplied to the segment from both sides. Following the reaction of the switchable solvent with CO2, the solvent becomes hydrophilic and transfers from the non-polar solvent to the aqueous droplet. By monitoring the time-dependent variation in droplet volumes, we determined the efficiency and extraction time for the CO2-mediated extraction of different nitrogenous bases in a broad experimental parameter space. The platform enables a significant reduction in the amount of switchable solvents used in these studies, provides accurate temporal characterization of the liquid-liquid extraction process, and offers the capability of high-throughput screening of switchable solvents.

  13. Ternary liquid-liquid equilibria for the phenolic compounds extraction from artificial textile industrial waste

    Science.gov (United States)

    Fardhyanti, Dewi Selvia; Prasetiawan, Haniif; Hermawan, Sari, Lelita Sakina

    2017-03-01

    Liquid waste in textile industry contains large amounts of dyes and chemicals which are capable of harming the environment and human health. It is due to liquid waste characteristics which have high BOD, COD, temperature, dissolved and suspended solid. One of chemical compound which might be harmful for environment when disposed in high concentration is phenol. Currently, Phenol compound in textile industrial waste has reached 10 ppm meanwhile maximum allowable phenol concentration is not more than 0.2 ppm. Otherwise, Phenol also has economic value as feedstock of plastic, pharmaceutical and cosmetic industry. Furthermore, suitable method to separate phenol from waste water is needed. In this research, liquid - liquid extraction method was used with extraction time for 70 minutes. Waste water sample was then separated into two layers which are extract and raffinate. Thereafter, extract and raffinate were then tested by using UV-Vis Spectrophotometer to obtained liquid - liquid equilibrium data. Aim of this research is to study the effect of temperature, stirring speed and type of solvent to obtain distribution coefficient (Kd), phenol yield and correlation of Three-Suffix Margules model for the liquid - liquid extraction data equilibrium. The highest extraction yield at 80.43 % was found by using 70% methanol as solvent at extraction temperature 50 °C with stirring speed 300 rpm, coefficient distribution was found 216.334. From this research it can be concluded that Three-Suffix Margules Model is suitable to predict liquid - liquid equilibrium data for phenol system.

  14. Exergy analysis and thermodynamic optimization in NGL plant in Kharg Island, Iran

    Energy Technology Data Exchange (ETDEWEB)

    Sadeghy, K.; Najafi, A.H. [Tehran Univ., Tehran (Iran, Islamic Republic of). Dept. of Mechanical Engineering

    2010-07-01

    This paper outlined the exergy analysis and thermodynamic optimization of a natural gas liquid (NGL) recovery plant located on Kharg Island in southern Iran. The units at the NGL plant include utility, acid gas removal, dehydration, hydrocarbon recovery and liquid processing units. This study is focused on the utility unit which consists of 4 fire water boilers and five 22 MW gas turbo generators. In order to review the parameters that affect the unit performance, an analytical approach was used to determine the thermodynamic losses in each component under different operational pressures, temperatures, flow rates and fuel gas specifications. The solution for unit performance enhancement was then presented. A feasibility study was also conducted regarding replacement of the boiler with a heat recovery steam generation (HRSG) system to use the energy from the gas turbine discharge air for generating the steam. The effect of this modification on the plant performance and economics was evaluated. The exergy loss quantities were reflective of main exergy destruction occurring in boilers and turbines due to their irreversibilities. The study showed that adding the HRSG can maximize plant performance. 17 refs., 3 tabs., 9 figs.

  15. Simple and quick determination of analgesics and other contaminants of emerging concern in environmental waters by on-line solid phase extraction coupled to liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Ferrer-Aguirre, Alejandra; Romero-González, Roberto; Vidal, J L Martínez; Frenich, Antonia Garrido

    2016-05-13

    A simple and quick analytical method has been developed for the determination of pharmaceutical compounds in water. An on-line solid-phase extraction (SPE) coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been optimized to determine 7 contaminants of emerging concern in environmental waters at ngL(-1) levels. This procedure requires minimal sample handling and small sample volume (900μL) with a total running time of 18min. Several SPE parameters were evaluated and optimized in order to achieve a high sample throughput. Therefore sample volume, carryover and reusability of the cartridges were evaluated. Performance characteristics were evaluated and good linearity was obtained (R(2)>0.98). Recoveries were evaluated in spiked samples at three concentrations and the values ranged from 71 to 104%. Intra and inter-day precision was lower than 10 and 13% respectively. Limits of quantification were equal to or lower than 10ngL(-1), except for 1,7-dimethylxanthine (20ngL(-1)) and ibuprofen (50ngL(-1)). The method was applied to 20 environmental water samples, and ibuprofen was the compound most widely detected at concentrations up to 42.06μgL(-1), whereas the other compounds were detected in fewer samples at lower concentrations (up to 15.99μgL(-1)).

  16. Composite hollow fiber membranes for organic solvent-based liquid-liquid extraction

    NARCIS (Netherlands)

    He, T.; Bolhuis-Versteeg, Lydia A.M.; Mulder, M.H.V.; Wessling, Matthias

    2004-01-01

    Instability issues of liquid membranes extraction significantly limit its wide application in industry. We report research on the application of a new composite hollow fiber membrane to stabilizing liquid membrane extraction. These type of composite membranes have either a polysulfone (PSf) ultrafil

  17. Composite hollow fiber membranes for organic solvent-based liquid-liquid extraction

    NARCIS (Netherlands)

    He, T.; Versteeg, L.A.M.; Mulder, M.H.V.; Wessling, M.

    2004-01-01

    Instability issues of liquid membranes extraction significantly limit its wide application in industry. We report research on the application of a new composite hollow fiber membrane to stabilizing liquid membrane extraction. These type of composite membranes have either a polysulfone (PSf) ultrafil

  18. Extraction of organic compounds with room temperature ionic liquids.

    Science.gov (United States)

    Poole, Colin F; Poole, Salwa K

    2010-04-16

    Room temperature ionic liquids are novel solvents with a rather specific blend of physical and solution properties that makes them of interest for applications in separation science. They are good solvents for a wide range of compounds in which they behave as polar solvents. Their physical properties of note that distinguish them from conventional organic solvents are a negligible vapor pressure, high thermal stability, and relatively high viscosity. They can form biphasic systems with water or low polarity organic solvents and gases suitable for use in liquid-liquid and gas-liquid partition systems. An analysis of partition coefficients for varied compounds in these systems allows characterization of solvent selectivity using the solvation parameter model, which together with spectroscopic studies of solvent effects on probe substances, results in a detailed picture of solvent behavior. These studies indicate that the solution properties of ionic liquids are similar to those of polar organic solvents. Practical applications of ionic liquids in sample preparation include extractive distillation, aqueous biphasic systems, liquid-liquid extraction, liquid-phase microextraction, supported liquid membrane extraction, matrix solvents for headspace analysis, and micellar extraction. The specific advantages and limitations of ionic liquids in these studies is discussed with a view to defining future uses and the need not to neglect the identification of new room temperature ionic liquids with physical and solution properties tailored to the needs of specific sample preparation techniques. The defining feature of the special nature of ionic liquids is not their solution or physical properties viewed separately but their unique combinations when taken together compared with traditional organic solvents.

  19. A generalized theory of chromatography and multistep liquid extraction

    Science.gov (United States)

    Chizhkov, V. P.; Boitsov, V. N.

    2017-03-01

    A generalized theory of chromatography and multistep liquid extraction is developed. The principles of highly efficient processes for fine preparative separation of binary mixture components on a fixed sorbent layer are discussed.

  20. One-step extraction of polar drugs from plasma by Parallel Artificial Liquid Membrane Extraction

    DEFF Research Database (Denmark)

    Pilařová, Veronika; Sultani, Mumtaz; Ask, Kristine Skoglund

    2017-01-01

    The new microextraction technique named parallel artificial liquid membrane extraction (PALME) was introduced as an alternative approach to liquid-liquid extraction of charged analytes from aqueous samples. The concept is based on extraction of analytes across a supported liquid membrane sustained......-throughput is achievable, in addition to the green chemistry offered by using PALME. The consumption of organic solvent is minimized to 3-5μL per sample. With a sample volume of 250μL and acceptor solution volume of 50μL, a maximal enrichment factor of five is achievable. Based on these parameters, a new method...

  1. Solid-liquid solvent extraction of metal ions

    Institute of Scientific and Technical Information of China (English)

    Bo Peng; Haiyan Fan; Jinzhang Gao

    2003-01-01

    An overview of extraction of some trace metal ions using molten solvent (low melting substance) during last two decadesis presented. The development of this technique since its inception is briefly traced. The comparison of extraction efficiency, thermo-dynamics and kinetics mainly involving extraction of rare earth ions between molten solvent extraction at high temperature and usualliquid-liquid extraction at room temperature are discussed in detail. The various parameters obtained from the previous and presentstudies such as equilibrium extraction constant Kex, pH1/2, thermodynamic and kinetic data are displayed in tabular form. Finally, thecurrent demands, disadvantages and future prospects are also evaluated.

  2. SIMULTANEOUS REACTION AND LIQUID-LIQUID EXTRACTION IN THE HYDROGEN PEROXIDE PRODUCTION

    Institute of Scientific and Technical Information of China (English)

    Shuxiang L(u); Li Wang; Zhentao Mi; Yaquan Wang

    2004-01-01

    The gas-liquid-liquid reactive extraction system for preparing hydrogen peroxide via anthraquinone was investigated. The oxidation reaction of hydrogenated working solution was combined with the extraction of hydrogen peroxide from working solution in a sieve plate column. The reaction of 2-ethylanthrahydroquionone with oxygen and the liquid-liquid extraction of hydrogen peroxide take place simultaneously. The oxygen was introduced with hydrogenated working solution through a nozzle in the bottom of the column, which worked as agitated air as well as oxidation reagent. The results showed the oxidation and extraction do not hamper each other, on the contrary, the presence of oxidation gas in the column can promote the transfer of hydrogen peroxide from organic phase to aqueous phase, thus the reaction efficiency and extraction efficiency increased with increasing gas superficial velocity. Furthermore, the oxidation efficiency is almost 100% and the extraction efficiency is higher than 90% in this process.

  3. SIMULTANEOUS REACTION AND LIQUID-LIQUID EXTRACTION IN THE HYDROGEN PEROXIDE PRODUCTION

    Institute of Scientific and Technical Information of China (English)

    ShuxiangLǖ; LiWang; ZhentaoMi; YaquanWang

    2004-01-01

    The gas-liquid-liquid reactive extraction system for preparing hydrogen peroxide via anthraquinone was investigated. The oxidation reaction of hydrogenated working solution was combined with the extraction of hydrogen peroxide from working solution in a sieve plate column. The reaction of 2-ethylanthrahydroquionone with oxygen and the liquid-liquid extraction of hydrogen peroxide take place simultaneously. The oxygen was introduced with hydrogenated working solution through a nozzle in the bottom of the column, which worked as agitated air as well as oxidation reagent. The results showed the oxidation and extraction do not hamper each other, on the contrary, the presence of oxidation gas in the column can promote the transfer of hydrogen peroxide fi'om organic phase to aqueous phase, thus the reaction efficiency and extraction efficiency increased with increasing gas superficial velocity. Furthermore, the oxidation efficiency is almost 100% and the extraction efficiency is higher than 90% in this process.

  4. Trans-Urals replacement NGL line nearing installation

    Energy Technology Data Exchange (ETDEWEB)

    1994-01-24

    Plans are advancing for construction of a Trans-Urals pipeline system to move NGLs from western Siberia to the Urals-Volga region. The system, currently envisioned as three 16-in. lines covering more than 1,000 miles, will move a mostly C[sub 3]-C[sub 5] stream from South Balyk (western Siberia) to petrochemical plants near Minnibaevo (Tatarstan) via Tchaikovsky. Supplies by pipelines have been interrupted since June 1989 when a massive leak from an existing 28-in. line caused an explosion that killed 765 people. Start up of construction was to have taken place later this year, but continuing Russian cash-flow problems to fund such major capital projects and declining NGL production in western Siberia have pushed back the project's timetable, say Western sources close to the project. The paper describes the export scheme which developers hope will improve cash flow, the pipeline and plant, and line size selection.

  5. Supported Liquid Membrane Extraction of Anabolic Androgenic ...

    African Journals Online (AJOL)

    NJD

    performance liquid chromatography coupled to a mass spectrometer operating under positive ion electrospray mode. (LC-PI-ESI-MS) ... for the analysis of anabolic compounds.37–44 However, both GC ..... Table 3 gives a summary of the frag-.

  6. Extractive Deep Desulfurization of Liquid Fuels Using Lewis-Based Ionic Liquids

    Directory of Open Access Journals (Sweden)

    Swapnil A. Dharaskar

    2013-01-01

    Full Text Available A new class of green solvents, known as ionic liquids (ILs, has recently been the subject of intensive research on the extractive desulfurization of liquid fuels because of the limitation of traditional hydrodesulfurization method. In present work, eleven Lewis acid ionic liquids were synthesized and employed as promising extractants for deep desulfurization of the liquid fuel containing dibenzothiophene (DBT to test the desulfurization efficiency. [Bmim]Cl/FeCl3 was the most promising ionic liquid and performed the best among studied ionic liquids under the same operating conditions. It can remove dibenzothiophene from the model liquid fuel in the single-stage extraction process with the maximum desulfurization efficiency of 75.6%. It was also found that [Bmim]Cl/FeCl3 may be reused without regeneration with considerable extraction efficiency of 47.3%. Huge saving on energy can be achieved if we make use of this ionic liquids behavior in process design, instead of regenerating ionic liquids after every time of extraction.

  7. Extraction matrine from Radix Sopheorae Tonkinensis by non-supported liquid membrane extraction technology

    Directory of Open Access Journals (Sweden)

    Zhifeng Guo

    2016-09-01

    Full Text Available Non-Supported Liquid Membrane Extraction (NSLME is a new development extraction technology based on Supported Liquid Membrane Extraction (SLME. Sample extraction assembly is composed of three phases: an acceptor phase: phosphate–sodium dihydrogen phosphate buffer solution at the bottom; an organic phase: chloroform applied as the non-supported liquid membrane in the middle layer; and a donor phase: aqueous solution samples containing alkaloids in the upper layer. The whole system is maintained stable by density difference among the three layers that avoided the mutual interferences. The alkaloid in the donor phase can spread to the underlying acidic acceptor phase, where it is able to form water soluble salt in the acid environment, and thus cannot return to the middle organic phase. Therefore, the transmission of alkaloid is a one-way path, and the extraction of alkaloids can be achieved and enriched. In this study, the extraction of alkaloid was carried out by using matrine aqueous solution as the donor phase, and the extraction quantity and efficiency were investigated by GC/MS. This study evaluated the relationship between extracted quantity and extraction time. The effects of extraction temperature, membrane thickness, pH value of acceptor phase on extraction quantity and efficiency were also studied, and the optimal extraction condition was found. The extracted quantity achieved the largest amount at 45 °C when pure phosphoric acid was applied as the acceptor phase; the organic solvent volume was 0.2 mL. The extraction of alkaloid from Radix Sophorae Tonkinensis was performed under the optimized condition. The extraction rate of matrine was up to 54% after a four-hour extraction. A huge advantage of NSLME technology is that the extracted alkaloid enjoyed high purity compared with that extracted by the traditional Liquid–Liquid Extraction (LLE.

  8. An inkjet-printed microfluidic device for liquid-liquid extraction.

    Science.gov (United States)

    Watanabe, Masashi

    2011-04-01

    A microfluidic device for liquid-liquid extraction was quickly produced using an office inkjet printer. An advantage of this method is that normal end users, who are not familiar with microfabrication, can produce their original microfluidic devices by themselves. In this method, the printer draws a line on a hydrophobic and oil repellent surface using hydrophilic ink. This line directs a fluid, such as water or xylene, to form a microchannel along the printed line. Using such channels, liquid-liquid extraction was successfully performed under concurrent and countercurrent flow conditions.

  9. One-step extraction of polar drugs from plasma by parallel artificial liquid membrane extraction.

    Science.gov (United States)

    Pilařová, Veronika; Sultani, Mumtaz; Ask, Kristine Skoglund; Nováková, Lucie; Pedersen-Bjergaard, Stig; Gjelstad, Astrid

    2017-02-01

    The new microextraction technique named parallel artificial liquid membrane extraction (PALME) was introduced as an alternative approach to liquid-liquid extraction of charged analytes from aqueous samples. The concept is based on extraction of analytes across a supported liquid membrane sustained in the pores of a thin polymeric membrane, a well-known extraction principle also used in hollow fiber liquid-phase microextraction (HF-LPME). However, the new PALME technique offers a more user-friendly setup in which the supported liquid membrane is incorporated in a 96 well plate system. Thus, high-throughput is achievable, in addition to the green chemistry offered by using PALME. The consumption of organic solvent is minimized to 3-5μL per sample. With a sample volume of 250μL and acceptor solution volume of 50μL, a maximal enrichment factor of five is achievable. Based on these parameters, a new method for extraction of polar basic drugs was developed in the present work. The basic drugs hydralazine, ephedrine, metaraminol, salbutamol, and cimetidine were used as model analytes, and were extracted from alkalized human plasma into an aqueous solution via the supported liquid membrane. The extraction was promoted by a carrier dissolved in the membrane, creating a temporary ion-pair complex between the hydrophilic drug and the carrier. As the model analytes were extracted directly into an aqueous solution, there was no need for evaporation of the extract before injection into LC-MS. Hence, the sample preparation is performed in one step. With optimized conditions, the extraction recoveries were in the range 50-89% from human plasma after 45min extraction. The data from the method evaluation were satisfactory and in line with current guidelines, and revealed an extraction method with substantial potential for high throughput bioanalysis of polar basic drugs.

  10. Miniscale Liquid-Liquid Extraction Coupled with Full Evaporation Dynamic Headspace Extraction for the Gas Chromatography/Mass Spectrometric Analysis of Polycyclic Aromatic Hydrocarbons with 4000-to-14 000-fold Enrichment.

    Science.gov (United States)

    Liew, Christina Shu Min; Li, Xiao; Lee, Hian Kee

    2016-09-20

    A new sample preparation approach of combining a miniscale version of liquid-liquid extraction (LLE), termed miniscale-LLE (msLLE), with automated full evaporation dynamic headspace extraction (FEDHS) was developed. Its applicability was demonstrated in the extraction of several polycyclic aromatic hydrocarbons (PAHs) (acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, and pyrene) from aqueous samples. In the first step, msLLE was conducted with 1.75 mL of n-hexane, and all of the extract was vaporized through a Tenax TA sorbent tube via a nitrogen gas flow, in the FEDHS step. Due to the stronger π-π interaction between the Tenax TA polymer and PAHs, only the latter, and not n-hexane, was adsorbed by the sorbent. This selectivity by the Tenax TA polymer allowed an effective concentration of PAHs while eliminating n-hexane by the FEDHS process. After that, thermal desorption was applied to the PAHs to channel them into a gas chromatography/mass spectrometric (GC/MS) system for analysis. Experimental parameters affecting msLLE (solvent volume and mixing duration) and FEDHS (temperature and duration) were optimized. The obtained results achieved low limits of detection (1.85-3.63 ng/L) with good linearity (r(2) > 0.9989) and high enrichment factors ranging from 4200 to 14 100. The optimized settings were applied to the analysis of canal water sampled from an industrial area and tap water, and this methodology was compared to stir-bar sorptive extraction (SBSE). This innovative combined extraction-concentration approach proved to be fast, effective, and efficient in determining low concentrations of PAHs in aqueous samples.

  11. Optimized determination of polybrominated diphenyl ethers by ultrasound-assisted liquid-liquid extraction and high-performance liquid chromatography.

    Science.gov (United States)

    He, Kuang; Lv, YuanCai; Chen, YuanCai

    2014-10-01

    A method based on ultrasound-assisted liquid-liquid extraction and high-performance liquid chromatography has been optimized for the determination of six polybrominated diphenyl ether congeners. The optimal condition relevant to the extraction was first investigated, more than 98.7 ± 0.7% recovery was achieved with dichloromethane as extractant, 5 min extraction time, and three cycles of ultrasound-assisted liquid-liquid extraction. Then multiple function was employed to optimize polybrominated diphenyl ether detection conditions with overall resolution and chromatography signal area as the responses. The condition chosen in this experiment was methanol/water 93:7 v/v, flow rate 0.80 mL/min, column temperature 30.0°C. The optimized technique revealed good linearity (R(2) > 0.9962 over a concentration range of 1-100 μg/L) and repeatability (relative standard deviation liquid-liquid extraction coupled with high-performance liquid chromatography was effective to identify and quantify the complex polybrominated diphenyl ethers in effluent samples.

  12. AFM fluid delivery/liquid extraction surface sampling/electrostatic spray cantilever probe

    Science.gov (United States)

    Van Berkel, Gary J.

    2015-06-23

    An electrospray system comprises a liquid extraction surface sampling probe. The probe comprises a probe body having a liquid inlet and a liquid outlet, and having a liquid extraction tip. A solvent delivery conduit is provided for receiving solvent liquid from the liquid inlet and delivering the solvent liquid to the liquid extraction tip. An open liquid extraction channel extends across an exterior surface of the probe body from the liquid extraction tip to the liquid outlet. An electrospray emitter tip is in liquid communication with the liquid outlet of the liquid extraction surface sampling probe. A system for analyzing samples, a liquid junction surface sampling system, and a method of analyzing samples are also disclosed.

  13. determination of lipophilic extractives in ionic liquid extracts of ...

    African Journals Online (AJOL)

    dell

    liquids are biodegradable and non-volatile, this approach of analysis is definitely a highly green process ... oxidation reaction (Freire et al 2006b,. Gutiérrez ... In this paper, we report the results of the ..... Structural changes evidenced by FTIR.

  14. Novel thiosalicylate-based ionic liquids for heavy metal extractions

    Energy Technology Data Exchange (ETDEWEB)

    Leyma, Raphlin; Platzer, Sonja [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, A-1090 Vienna (Austria); Jirsa, Franz [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, A-1090 Vienna (Austria); Department of Zoology, University of Johannesburg, PO Box 524, Auckland Park, 2006, Johannesburg (South Africa); Kandioller, Wolfgang, E-mail: wolfgang.kandioller@univie.ac.at [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, A-1090 Vienna (Austria); Krachler, Regina; Keppler, Bernhard K. [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, A-1090 Vienna (Austria)

    2016-08-15

    Highlights: • Six thiosalicylate-based ammonium and phosphonium ionic liquids (ILs) were newly synthesized. • ILs showed good extraction of cadmium, copper, and zinc. • Phosphonium ILs showed better extraction efficiencies than their ammonium counterparts. - Abstract: This study aims to develop novel ammonium and phosphonium ionic liquids (ILs) with thiosalicylate (TS) derivatives as anions and evaluate their extracting efficiencies towards heavy metals in aqueous solutions. Six ILs were synthesized, characterized, and investigated for their extracting efficacies for cadmium, copper, and zinc. Liquid-liquid extractions of Cu, Zn, or Cd with ILs after 1–24 h using model solutions (pH 7; 0.1 M CaCl{sub 2}) were assessed using flame atomic absorption spectroscopy (F-AAS). Phosphonium-based ILs trihexyltetradecylphosphonium 2-(propylthio)benzoate [P{sub 66614}][PTB] and 2-(benzylthio)benzoate [P{sub 66614}][BTB] showed best extraction efficiency for copper and cadmium, respectively and zinc was extracted to a high degree by [P{sub 66614}][BTB] exclusively.

  15. Enhanced flavour extraction in continuous liquid-liquid extractors

    CSIR Research Space (South Africa)

    Apps

    2005-08-12

    Full Text Available stream_source_info apps_2005.pdf.txt stream_content_type text/plain stream_size 10017 Content-Encoding ISO-8859-1 stream_name apps_2005.pdf.txt Content-Type text/plain; charset=ISO-8859-1 Journal of Chromatography A...: +27 12 841 3594. E-mail address: papps@csir.co.za (P. Apps). extraction yields sufficient concentrated extract for repeated analyses under different conditions, as required for exam- ple by aroma dilution analysis [11,12]. CLLE is especially valuable...

  16. Ionic liquids screening for desulfurization of natural gasoline by liquid-liquid extraction.

    Science.gov (United States)

    Likhanova, Natalya V; Guzmán-Lucero, Diego; Flores, Eugenio A; García, Paloma; Domínguez-Aguilar, Marco A; Palomeque, Jorge; Martínez-Palou, Rafael

    2010-11-01

    Seventy five ionic liquids (ILs) were tested as a sequestering agent of sulfured compounds in natural gasoline (NG). Desulphurization of NG was performed by means of liquid-liquid extraction method at room temperature and atmospheric pressure. Experimental ILs containing imidazolium, pyridinium, and ammonium cations along with organic and inorganic anions were synthesized conventionally and under microwave and sonochemical conditions. The effect of the molecular structure of ILs on the desulfurization efficiency of NG with high sulfur content was evaluated. Analysis indicated that the anion type played a more important role than the cation on the desulphurization process. ILs based on halogen-ferrates and halogen-aluminates exhibited the highest efficiency in sulfur removal, and their efficiency is further improved when there is an excess of metallic salt in a ratio of at least 1:1.3 during the synthesis of the corresponding IL. An explanation for the ability of metallic ILs to remove sulfur-containing compounds from natural gasoline based on the ratio of the ionic charge to the atomic radius is proposed. Furthermore, a method to recover and reuse water-sensitive to halogenated precursors is described.

  17. Extraction of proteins with ionic liquid aqueous two-phase system based on guanidine ionic liquid.

    Science.gov (United States)

    Zeng, Qun; Wang, Yuzhi; Li, Na; Huang, Xiu; Ding, Xueqin; Lin, Xiao; Huang, Songyun; Liu, Xiaojie

    2013-11-15

    Eight kinds of green ionic liquids were synthesized, and an ionic liquid aqueous two-phase system (ILATPS) based on 1,1,3,3-tetramethylguandine acrylate (TMGA) guanidine ionic liquid was first time studied for the extraction of proteins. Single factor experiments proved that the extraction efficiency of bovine serum albumin (BSA) was influenced by the mass of IL, K2HPO4 and BSA, also related to the separation time and temperature. The optimum conditions were determined through orthogonal experiment by the five factors described above. The results showed that under the optimum conditions, the extraction efficiency could reach up to 99.6243%. The relative standard deviations (RSD) of extraction efficiencies in precision experiment, repeatability experiment and stability experiment were 0.8156% (n=5), 1.6173% (n=5) and 1.6292% (n=5), respectively. UV-vis and FT-IR spectra confirmed that there were no chemical interactions between BSA and ionic liquid in the extraction process, and the conformation of the protein was not changed after extraction. The conductivity, DLS and TEM were combined to investigate the microstructure of the top phase and the possible mechanism for the extraction. The results showed that hydrophobic interaction, hydrogen bonding interaction and the salt out effect played important roles in the transferring process, and the aggregation and embrace phenomenon was the main driving force for the separation. All these results proved that guanidine ionic liquid-based ATPSs have the potential to offer new possibility in the extraction of proteins.

  18. SELECTION OF ROBUST COMBINATIONS OF EXTRACTION LIQUID COMPOSITION AND INTERNAL STANDARD - MONTE-CARLO SIMULATION OF IMPROVEMENT OF ASSAY-METHODS WITH LIQUID-LIQUID-EXTRACTION PRIOR TO HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY

    NARCIS (Netherlands)

    WIELING, J; COENEGRACHT, PMJ; MENSINK, CK; JONKMAN, JHG; DOORNBOS, DA

    1992-01-01

    The liquid-liquid extraction of a mixture of sulphonamides was achieved to examine the correlation between the experimental errors in the recoveries. Also, the impact of the composition of the extraction liquid was investigated. Six sulphonamides were repeatedly extracted simultaneously with ten dif

  19. Determination of pesticide residues in wine by membrane-assisted solvent extraction and high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Moeder, M; Bauer, C; Popp, P; van Pinxteren, M; Reemtsma, T

    2012-06-01

    The determination of pesticides in food products is an essential issue to guarantee food safety and minimise health risks of consumers. A protocol based on membrane-assisted solvent extraction and liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) that allows the determination of 18 pesticides in red wine at minimum labour effort for sample preparation was developed and validated. Ten millilitres of wine were extracted using 100 μL of toluene filled in a non-porous polyethylene membrane bag which is immersed in the wine sample. After 150 min extraction under stirring, an aliquot of the extraction solution is analysed using HPLC-MS/MS. The limits of quantification ranged from 3 ng/L for Pirimicarb to 1.33 μg/L for Imidacloprid. Quantification by matrix-matched calibration provided relative standard deviations ≤16 % for most of the target pesticides. The linearity of calibration was given over three to four orders of magnitude, which enables the reliable measurement of a broad range of pesticide concentrations, and for each target pesticide, the sensitivity of the protocol meets the maximum residue levels set by legislations at least for wine grapes. Good agreement of results was found when the new method was compared with a standard liquid-liquid extraction protocol. In five wine samples analysed, Carbendazim and Metalaxyl were determined at micrograms per litre concentrations, even in some of the organic wines. Tebuconazol and Cyprodinitril were determined at lower abundance and concentration, followed by Spiroxamin and Diuron.

  20. A Guided Inquiry Liquid/Liquid Extractions Laboratory for Introductory Organic Chemistry

    Science.gov (United States)

    Raydo, Margaret L.; Church, Megan S.; Taylor, Zane W.; Taylor, Christopher E.; Danowitz, Amy M.

    2015-01-01

    A guided inquiry laboratory experiment for teaching liquid/liquid extractions to first semester undergraduate organic chemistry students is described. This laboratory is particularly useful for introductory students as the analytes that are separated are highly colored dye molecules. This allows students to track into which phase each analyte…

  1. Pressurized liquid extraction followed by liquid chromatography with tandem mass spectrometry to determine pharmaceuticals in mussels.

    Science.gov (United States)

    Núñez, Mireia; Borrull, Francesc; Pocurull, Eva; Fontanals, Núria

    2016-02-01

    An analytical method based on pressurized liquid extraction and solid-phase extraction with a mixed-mode Oasis(®) MAX sorbent as cleanup, followed by liquid chromatography with electrospray ionization and tandem mass spectrometry was developed and validated for the determination of seven widely used pharmaceuticals in mussel species. The optimization of the pressurized liquid extraction and the solid-phase extraction parameters is described. The method provided extraction recoveries ranging from 61 to 90%, and limits of detection ranging from 2 to 50 ng/g (dry weight). The repeatability and reproducibility of the method, expressed as relative standard deviation, were lower than 15 and 19%, respectively. The method was successfully applied to the analysis of mussel samples from different locations. The analyses showed that salicylic acid was present in mussels at concentrations up to 177 ng/g (dry weight).

  2. Selective determination of antimycotic drugs in environmental water samples by mixed-mode solid-phase extraction and liquid chromatography quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Casado, J; Rodríguez, I; Ramil, M; Cela, R

    2014-04-25

    The suitability of mixed-mode (reversed-phase and cationic exchange) solid-phase extraction (SPE) for the selective concentration of basic antimycotic drugs (belonging to triazole, imidazole and allylamine chemical classes) in environmental water samples has been demonstrated for first time. The use of a sequential elution protocol, allowing the removal of neutral and acidic interferences before analytes extraction, led to a significant reduction of matrix effects, during electrospray ionization (ESI), in comparison with results reported for reversed-phase sorbents. In combination with liquid chromatography (LC) quadrupole time-of-flight (QTOF) mass spectrometry (MS) determination, the developed method attained limits of quantification (LOQs) comprised between 2 and 15ngL(-1). After internal surrogate correction, accurate results (in most cases, recoveries ranged between 75 and 117%) were obtained for spiked aliquots of raw and treated wastewater, as well as river water, using quantification against calibration standard solutions in methanol (2% in NH3). Accurate, scan MS/MS spectra allowed the unambiguous identification of target compounds in environmental samples; furthermore, the information contained in MS spectra was used for the screening of additional antimycotics in the processed samples. Fluconazole, ketoconazole, miconazole and clotrimazole were measured in wastewater samples at concentrations up to 200ngL(-1). The screening capabilities of the LC-QTOF-MS system permitted to identify the systematic presence of climbazole in the processed samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Determination of Organic Pollutants in Small Samples of Groundwaters by Liquid-Liquid Extraction and Capillary Gas Chromatography

    DEFF Research Database (Denmark)

    Harrison, I.; Leader, R.U.; Higgo, J.J.W.

    1994-01-01

    A method is presented for the determination of 22 organic compounds in polluted groundwaters. The method includes liquid-liquid extraction of the base/neutral organics from small, alkaline groundwater samples, followed by derivatisation and liquid-liquid extraction of phenolic compounds after...

  4. Hybrid Multiphase CFD Solver for Coupled Dispersed/Segregated Flows in Liquid-Liquid Extraction

    Directory of Open Access Journals (Sweden)

    Kent E. Wardle

    2013-01-01

    Full Text Available The flows in stage-wise liquid-liquid extraction devices include both phase segregated and dispersed flow regimes. As a additional layer of complexity, for extraction equipment such as the annular centrifugal contactor, free-surface flows also play a critical role in both the mixing and separation regions of the device and cannot be neglected. Traditionally, computional fluid dynamics (CFD of multiphase systems is regime dependent—different methods are used for segregated and dispersed flows. A hybrid multiphase method based on the combination of an Eulerian multifluid solution framework (per-phase momentum equations and sharp interface capturing using Volume of Fluid (VOF on selected phase pairs has been developed using the open-source CFD toolkit OpenFOAM. Demonstration of the solver capability is presented through various examples relevant to liquid-liquid extraction device flows including three-phase, liquid-liquid-air simulations in which a sharp interface is maintained between each liquid and air, but dispersed phase modeling is used for the liquid-liquid interactions.

  5. Design of guanidinium ionic liquid based microwave-assisted extraction for the efficient extraction of Praeruptorin A from Radix peucedani.

    Science.gov (United States)

    Ding, Xueqin; Li, Li; Wang, Yuzhi; Chen, Jing; Huang, Yanhua; Xu, Kaijia

    2014-12-01

    A series of novel tetramethylguanidinium ionic liquids and hexaalkylguanidinium ionic liquids have been synthesized based on 1,1,3,3-tetramethylguanidine. The structures of the ionic liquids were confirmed by (1)H NMR spectroscopy and mass spectrometry. A green guanidinium ionic liquid based microwave-assisted extraction method has been developed with these guanidinium ionic liquids for the effective extraction of Praeruptorin A from Radix peucedani. After extraction, reversed-phase high-performance liquid chromatography with UV detection was employed for the analysis of Praeruptorin A. Several significant operating parameters were systematically optimized by single-factor and L9 (3(4)) orthogonal array experiments. The amount of Praeruptorin A extracted by [1,1,3,3-tetramethylguanidine]CH2CH(OH)COOH is the highest, reaching 11.05 ± 0.13 mg/g. Guanidinium ionic liquid based microwave-assisted extraction presents unique advantages in Praeruptorin A extraction compared with guanidinium ionic liquid based maceration extraction, guanidinium ionic liquid based heat reflux extraction and guanidinium ionic liquid based ultrasound-assisted extraction. The precision, stability, and repeatability of the process were investigated. The mechanisms of guanidinium ionic liquid based microwave-assisted extraction were researched by scanning electron microscopy and IR spectroscopy. All the results show that guanidinium ionic liquid based microwave-assisted extraction has a huge potential in the extraction of bioactive compounds from complex samples.

  6. Hollow fiber-based liquid-liquid-liquid micro-extraction with osmosis: I. Theoretical simulation and verification.

    Science.gov (United States)

    Wu, Qian; Wu, Dapeng; Geng, Xuhui; Shen, Zheng; Guan, Yafeng

    2012-07-27

    Osmosis in hollow fiber-based liquid-liquid-liquid micro-extraction (HF-LLLME) was validated and utilized to improve enrichment factor of extraction in this study. When donor phase (sample solution) with higher ion strength than acceptor phase (extraction phase) was used, osmosis was established from acceptor phase, through organic membrane to donor phase. The mass flux expression of analytes across the organic membrane was established based on the convective-diffusive kinetic model, and the kinetic process for HF-LLLME with osmosis was simulated. Simulation results indicated that osmosis from acceptor phase to donor phase can increase enrichment factor of HF-LLLME, accelerate extraction process, and even result in the distribution ratio of analytes between donor and acceptor phase exceeding their partition coefficient. This phenomenon was verified by the experimental data of extraction with six organic acids and four organic bases as the model analytes.

  7. Equilibrium study on the reactive liquid-liquid extraction of 4-cyanopyridine with 4-nonylphenol

    NARCIS (Netherlands)

    Bokhove, J.; Schuur, Boelo; de Haan, A.B.

    2012-01-01

    A liquid–liquid extraction equilibrium model was developed describing the extraction of aqueous 4-cyanopyridine with the reactive solvent 4-nonylphenol. The model describes the capacity of the solvent up to an equilibrium aqueous phase concentration of 20 g/L within a temperature interval of 25 to

  8. Ambient Mass Spectrometry Imaging Using Direct Liquid Extraction Techniques

    Energy Technology Data Exchange (ETDEWEB)

    Laskin, Julia; Lanekoff, Ingela

    2015-11-13

    Mass spectrometry imaging (MSI) is a powerful analytical technique that enables label-free spatial localization and identification of molecules in complex samples.1-4 MSI applications range from forensics5 to clinical research6 and from understanding microbial communication7-8 to imaging biomolecules in tissues.1, 9-10 Recently, MSI protocols have been reviewed.11 Ambient ionization techniques enable direct analysis of complex samples under atmospheric pressure without special sample pretreatment.3, 12-16 In fact, in ambient ionization mass spectrometry, sample processing (e.g., extraction, dilution, preconcentration, or desorption) occurs during the analysis.17 This substantially speeds up analysis and eliminates any possible effects of sample preparation on the localization of molecules in the sample.3, 8, 12-14, 18-20 Venter and co-workers have classified ambient ionization techniques into three major categories based on the sample processing steps involved: 1) liquid extraction techniques, in which analyte molecules are removed from the sample and extracted into a solvent prior to ionization; 2) desorption techniques capable of generating free ions directly from substrates; and 3) desorption techniques that produce larger particles subsequently captured by an electrospray plume and ionized.17 This review focuses on localized analysis and ambient imaging of complex samples using a subset of ambient ionization methods broadly defined as “liquid extraction techniques” based on the classification introduced by Venter and co-workers.17 Specifically, we include techniques where analyte molecules are desorbed from solid or liquid samples using charged droplet bombardment, liquid extraction, physisorption, chemisorption, mechanical force, laser ablation, or laser capture microdissection. Analyte extraction is followed by soft ionization that generates ions corresponding to intact species. Some of the key advantages of liquid extraction techniques include the ease

  9. Selective Extraction of Uranium from Liquid or Supercritical Carbon Dioxide

    Energy Technology Data Exchange (ETDEWEB)

    Farawila, Anne F.; O' Hara, Matthew J.; Wai, Chien M.; Taylor, Harry Z.; Liao, Yu-Jung

    2012-07-31

    Current liquid-liquid extraction processes used in recycling irradiated nuclear fuel rely on (1) strong nitric acid to dissolve uranium oxide fuel, and (2) the use of aliphatic hydrocarbons as a diluent in formulating the solvent used to extract uranium. The nitric acid dissolution process is not selective. It dissolves virtually the entire fuel meat which complicates the uranium extraction process. In addition, a solvent washing process is used to remove TBP degradation products, which adds complexity to the recycling plant and increases the overall plant footprint and cost. A liquid or supercritical carbon dioxide (l/sc -CO2) system was designed to mitigate these problems. Indeed, TBP nitric acid complexes are highly soluble in l/sc -CO2 and are capable of extracting uranium directly from UO2, UO3 and U3O8 powders. This eliminates the need for total acid dissolution of the irradiated fuel. Furthermore, since CO2 is easily recycled by evaporation at room temperature and pressure, it eliminates the complex solvent washing process. In this report, we demonstrate: (1) A reprocessing scheme starting with the selective extraction of uranium from solid uranium oxides into a TBP-HNO3 loaded Sc-CO2 phase, (2) Back extraction of uranium into an aqueous phase, and (3) Conversion of recovered purified uranium into uranium oxide. The purified uranium product from step 3 can be disposed of as low level waste, or mixed with enriched uranium for use in a reactor for another fuel cycle. After an introduction on the concept and properties of supercritical fluids, we first report the characterization of the different oxides used for this project. Our extraction system and our online monitoring capability using UV-Vis absorbance spectroscopy directly in sc-CO2 is then presented. Next, the uranium extraction efficiencies and kinetics is demonstrated for different oxides and under different physical and chemical conditions: l/sc -CO2 pressure and temperature, TBP/HNO3 complex used

  10. Salting-out assisted liquid-liquid extraction coupled to dispersive liquid-liquid microextraction for the determination of chlorophenols in wine by high-performance liquid chromatography.

    Science.gov (United States)

    Fan, Yingying; Hu, Shibin; Liu, Shuhui

    2014-12-01

    A novel procedure of sample preparation combined with high-performance liquid chromatography with diode array detection is introduced for the analysis of highly chlorinated phenols (trichlorophenols, tetrachlorophenols, and pentachlorophenol) in wine. The main features of the proposed method are (i) low-toxicity diethyl carbonate as extraction solvent to selectively extract the analytes without matrix effect, (ii) the combination of salting-out assisted liquid-liquid extraction and dispersive liquid-liquid microextraction to achieve an enrichment factor of 334-361, and (iii) the extract is analyzed by high-performance liquid chromatography to avoid derivatization. Under the optimum conditions, correlation coefficients (r) were >0.997 for calibration curves in the range 1-80 ng/mL, detection limits and quantification limits ranged from 0.19 to 0.67 and 0.63 to 2.23 ng/mL, respectively, and relative standard deviation was wines, with recovery rates in the range 82-104%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Pre-concentration of uranium from water samples by dispersive liquid-liquid micro-extraction

    Energy Technology Data Exchange (ETDEWEB)

    Khajeh, Mostafa; Nemch, Tabandeh Karimi [Zabol Univ. (Iran, Islamic Republic of). Dept. of Chemistry

    2014-07-01

    In this study, a simple and rapid dispersive liquid-liquid microextraction (DLLME) was developed for the determination of uranium in water samples prior to high performance liquid chromatography with diode array detection. 1-(2-pyridylazo)-2-naphthol (PAN) was used as complexing agent. The effect of various parameters on the extraction step including type and volume of extraction and dispersive solvents, pH of solution, concentration of PAN, extraction time, sample volume and ionic strength were studied and optimized. Under the optimum conditions, the limit of detection (LOD) and preconcentration factor were 0.3 μg L{sup -1} and 194, respectively. Furthermore, the relative standard deviation of the ten replicate was <2.6%. The developed procedure was then applied to the extraction and determination of uranium in the water samples.

  12. SYNTHESE D’EXTRACTANTS ACIDES HEXADECYL- ET DECYLAMINOBIMETHYLENEDIPHOSPHONIQUES APPLICATION A L’EXTRACTION LIQUIDE-LIQUIDE DE Ni (II

    Directory of Open Access Journals (Sweden)

    M.A DIDI

    2007-06-01

    Après purification puis caractérisation des produits, nous avons réalisé divers tests d’extraction liquide - liquide de Ni (II en milieu sulfaté. Le temps d’équilibre déterminé par étude cinétique a été fixé à 40 minutes. Les paramètres changeant tels la température ( T = 20°C, 30°C et 50°C, le rapport du nombre de moles (n extractant / n métal (Q =1 à 6 et le rapport des volumes (Vaq / Vorg= 1, 2, 3 et 4 ont permis de maximiser le rendement d’extraction qui est de 46% avec le HABMP et de 44% pour le DADMP et ceci pour des extractions à un seul plateau.

  13. Ultra-preconcentration and determination of selected pharmaceutical and personal care products in different water matrices by solid-phase extraction combined with dispersive liquid-liquid microextraction prior to ultra high pressure liquid chromatography tandem mass spectrometry analysis.

    Science.gov (United States)

    Celano, Rita; Piccinelli, Anna Lisa; Campone, Luca; Rastrelli, Luca

    2014-08-15

    Pharmaceutical and personal care products (PPCPs) are one of the most important classes of emerging contaminants. The potential of ecological and environmental impacts associated with PPCPs are of particular concern because they continually penetrate the aquatic environment. This work describes a novel ultra-preconcentration technique for the rapid and highly sensitive analysis of selected PPCPs in environmental water matrices at ppt levels. Selected PPCPs were rapidly extracted and concentrated from large volumes of aqueous solutions (500 and 250mL) by solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME) and then analyzed using UHPLC-MS/MS. Experimental parameters were carefully investigated and optimized to achieve the best SPE-DLLME efficiency and higher enrichment factors. The best results were obtained using the ternary mixture acetonitrile/methanol/dichloromethane 3:3:4, v/v/v, both as SPE eluent and DLLME extractant/dispersive mixture. DLLME aqueous solution (5% NaCl, 10mgL(-1) TBAB) was also modified to improve the extraction efficiency of more hydrophilic PPCPs. Under the optimal conditions, an exhaustive extraction for most of the investigated analytes (recoveries >70%), with a precision (RSD <10%) and very high enrichment factors were attained for different aqueous matrices (drinking, sea, river and wastewater). Method detection and quantification limits were at very low ppt levels and below 1 and 3ngL(-1), respectively, for 15 of selected PPCPs. The proposed analytical procedure offers numerous advantages such as the simplicity of operation, rapidity, a high enrichment factor and sensitivity. So it is suitable for monitoring and studies of occurrence of PPCPs in different environmental compartments.

  14. Group extraction of organic compounds present in liquid samples

    Science.gov (United States)

    Jahnsen, Vilhelm J. (Inventor)

    1976-01-01

    An extraction device is disclosed comprising a tube containing a substantially inert, chemically non-reactive packing material with a large surface area to volume ratio. A sample which consists of organic compounds dissolved in a liquid, is introduced into the tube. As the sample passes through the packing material it spreads over the material's large surface area to form a thin liquid film which is held on the packing material in a stationary state. A particular group or family of compounds is extractable from the sample by passing a particular solvent system consisting of a solvent and selected reagents through the packing material. The reagents cause optimum conditions to exist for the compounds of the particular family to pass through the phase boundary between the sample liquid and the solvent of the solvent system. Thus, the compounds of the particular family are separated from the sample liquid and become dissolved in the solvent of the solvent system. The particular family of compounds dissolved in the solvent, representing an extract, exits the tube together with the solvent through the tube's nozzle, while the rest of the sample remains on the packing material in a stationary state. Subsequently, a different solvent system may be passed through the packing material to extract another family of compounds from the remaining sample on the packing material.

  15. Lunar Oxygen Production and Metals Extraction Using Ionic Liquids

    Science.gov (United States)

    Marone, Matthew; Paley, Mark Steven; Donovan, David N.; Karr, Laurel J.

    2009-01-01

    Initial results indicate that ionic liquids are promising media for the extraction of oxygen from lunar regolith. IL acid systems can solubilize regolith and produce water with high efficiency. IL electrolytes are effective for water electrolysis, and the spent IL acid media are capable of regeneration.

  16. A magnetic-based dispersive micro-solid-phase extraction method using the metal-organic framework HKUST-1 and ultra-high-performance liquid chromatography with fluorescence detection for determining polycyclic aromatic hydrocarbons in waters and fruit tea infusions.

    Science.gov (United States)

    Rocío-Bautista, Priscilla; Pino, Verónica; Ayala, Juan H; Pasán, Jorge; Ruiz-Pérez, Catalina; Afonso, Ana M

    2016-03-04

    A hybrid material composed by the metal-organic framework (MOF) HKUST-1 and Fe3O4 magnetic nanoparticles (MNPs) has been synthetized in a quite simple manner, characterized, and used in a magnetic-assisted dispersive micro-solid-phase extraction (M-d-μSPE) method in combination with ultra-high-performance liquid chromatography (UHPLC) and fluorescence detection (FD). The application was devoted to the determination of 8 heavy polycyclic aromatic hydrocarbons (PAHs) in different aqueous samples, specifically tap water, wastewaters, and fruit tea infusion samples. The overall M-d-μSPE-UHPLC-FD method was optimized and validated. The method is characterized by: its simplicity in both the preparation of the hybrid material (simple mixing) and the magnetic-assisted approach (∼10min extraction time), the use of low sorbent amounts (20mg of HKUST-1 and 5mg of Fe3O4 MNPs), and the low organic solvent consumption in the overall M-d-μSPE-UHPLC-FD method (1.5mL of acetonitrile in the M-d-μSPE method and 2.8mL of acetonitrile in the UHPLC-FD run). The resulting method has high sensitivity, with LODs down to 0.8ngL(-1); adequate intermediate precision, with relative standard deviation values (RSD) always lower than 6.3% (being the range 5.9-9.0% in tap water for a spiked level of 45ngL(-1), 6.1-14% in wastewaters for a spiked level of 45ngL(-1), and 7.2-17% in fruit tea infusion samples for a spiked level of 45ngL(-1)); and adequate relative recoveries, with average values of 82% in tap water, and 94% and 75% in wastewater and fruit tea infusion samples, respectively, if using the proper matrix-matched calibration.

  17. Low-temperature liquid-liquid extraction of phenols from aqueous solutions with hydrophilic mixtures of extractants

    Science.gov (United States)

    Rudakov, O. B.; Khorokhordina, E. A.; Preobrazhenskii, M. A.; Rudakova, L. V.

    2016-08-01

    The volume ratios in acetonitrile-ethyl acetate (90 : 10, 95 : 5), acetonitrile-isopropanol-ethyl acetate (70 : 15 : 15, 80 : 5 : 15), and isopropanol-1-butanol (50 : 50) mixtures were determined. Their mixing with water (1 : 1) and storage at-10°C led to partitioning into two immiscible liquid phases without formation of the ice phase. The mixtures were shown to be useful as hydrophilic extractants in low-temperature liquidliquid extraction of phenol from aqueous solutions.

  18. Emulsion liquid membrane for selective extraction of Bi(III)

    Institute of Scientific and Technical Information of China (English)

    Bahram Mokhtari; Kobra Pourabdollah

    2015-01-01

    Di(2-ethylhexyl)phosphoric acid was used as extractant of bismuth ions from nitrate medium by emulsion liquid membrane, with Triton X-100 as the biodegradable surfactant in n-pentanol bulk membrane. The novelties and innovative points of this work are the application of emulsion liquid membrane for selective and efficient extraction of bismuth ions as wel as the relevant optimization procedures. The extraction of bismuth ions was evaluated by the yield of extraction. The experimental parameters were evaluated and optimized, including the ratio of di(2-ethylhexyl)phosphoric acid mass concentration to Triton X-100 (1.0%:0.5%), nature of diluent (n-pentanol), nature and concentration of stripping solution (sulfuric acid, 0.5 mol·L−1), stirring speed (1800 r·min−1) and equilibrium time of extraction (20 min), initial feed solution of bismuth (350 mg·L−1) and the volume ratio of internal stripping phase to membrane phase (14). The experimental parameters of kinetic extraction reveal that the bismuth ions can be extracted by 100%.

  19. Determination of Organic Pollutants in Small Samples of Groundwaters by Liquid-Liquid Extraction and Capillary Gas Chromatography

    DEFF Research Database (Denmark)

    Harrison, I.; Leader, R.U.; Higgo, J.J.W.;

    1994-01-01

    A method is presented for the determination of 22 organic compounds in polluted groundwaters. The method includes liquid-liquid extraction of the base/neutral organics from small, alkaline groundwater samples, followed by derivatisation and liquid-liquid extraction of phenolic compounds after...... neutralisation. The extracts were analysed by capillary gas chromatography. Dual detection by flame Ionisation and electron capture was used to reduce analysis time....

  20. Extraction efficiency of hydrophilic and lipophilic antioxidants from lyophilized foods using pressurized liquid extraction and manual extraction.

    Science.gov (United States)

    Watanabe, Jun; Oki, Tomoyuki; Takebayashi, Jun; Takano-Ishikawa, Yuko

    2014-09-01

    The efficient extraction of antioxidants from food samples is necessary in order to accurately measure their antioxidant capacities. α-Tocopherol and gallic acid were spiked into samples of 5 lyophilized and pulverized vegetables and fruits (onion, cabbage, Satsuma mandarin orange, pumpkin, and spinach). The lipophilic and hydrophilic antioxidants in the samples were sequentially extracted with a mixed solvent of n-hexane and dichloromethane, and then with acetic acid-acidified aqueous methanol. Duplicate samples were extracted: one set was extracted using an automated pressurized liquid extraction apparatus, and the other set was extracted manually. Spiked α-tocopherol and gallic acid were recovered almost quantitatively in the extracted lipophilic and hydrophilic fractions, respectively, especially when pressurized liquid extraction was used. The expected increase in lipophilic oxygen radical absorbance capacity (L-ORAC) due to spiking with α-tocopherol, and the expected increase in 2,2-diphenyl-1-picrylhydrazyl radical scavenging activities and total polyphenol content due to spiking with gallic acid, were all recovered in high yield. Relatively low recoveries, as reflected in the hydrophilic ORAC (H-ORAC) value, were obtained following spiking with gallic acid, suggesting an interaction between gallic acid and endogenous antioxidants. The H-ORAC values of gallic acid-spiked samples were almost the same as those of postadded (spiked) samples. These results clearly indicate that lipophilic and hydrophilic antioxidants are effectively extracted from lyophilized food, especially when pressurized liquid extraction is used.

  1. Salting-out homogenous extraction followed by ionic liquid/ionic liquid liquid-liquid micro-extraction for determination of sulfonamides in blood by high performance liquid chromatography.

    Science.gov (United States)

    Liu, Zhongling; Yu, Wei; Zhang, Hanqi; Gu, Fanbin; Jin, Xiangqun

    2016-12-01

    Salting-out homogenous extraction followed by ionic liquid/ionic liquid dispersive liquid-liquid micro-extraction system was developed and applied to the extraction of sulfonamides in blood. High-performance liquid chromatography was applied to the determination of the analytes. The blood sample was centrifuged to obtain the serum. After the proteins in the serum were removed in the presence of acetonitrile, ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate, dipotassium hydrogen phosphate, ionic liquid 1-Hexyl-3-methylimidazolium hexafluorophosphate were added into the resulting solution. After the resulting mixture was ultrasonically shaken and centrifuged, the precipitate was separated. The acetonitrile was added in the precipitate and the analytes were extracted into the acetonitrile phase. The parameters affecting the extraction efficiency, such as volume of ionic liquid, amount of dipotassium hydrogen phosphate, volume of dispersant, extraction time and temperature were investigated. The limits of detection of sulfamethizole (STZ), sulfachlorpyridazine (SCP), sulfamethoxazole (SMX) and Sulfisoxazole (SSZ) were 4.78, 3.99, 5.21 and 3.77μgL(-1), respectively. When the present method was applied to the analysis of real blood samples, the recoveries of analytes ranged from 90.0% to 113.0% and relative standard deviations were lower than 7.2%.

  2. Extraction and Separation of Molybdenum by Using Homogeneous Liquid-Liquid Microextraction via Flotation Assistance

    OpenAIRE

    Rezaee, Mohammad; Mozaffari,Maryam; Haddadi,Hedayat; Pourjavid,Mohammad R.; SEMNANI, Abolfazl

    2015-01-01

    Homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA) was investigated for the extraction of molybdenum from the water samples. Alizarin Red S and cetyl trimethylammonium bromide (CTAB) were used as a complexing ligand and ion-pairing reagent, respectively. The enriched analyte in the floated organic phase was determined by electrothermal atomic absorption spectrometry (ETAAS). In this work, low density organic solvent was used and no centrifugation was required in thi...

  3. Pyridinium ionic liquid-based liquid-solid extraction of inorganic and organic iodine from Laminaria.

    Science.gov (United States)

    Peng, Li-Qing; Yu, Wen-Yan; Xu, Jing-Jing; Cao, Jun

    2018-01-15

    A simple, green and effective extraction method, namely, pyridinium ionic liquid- (IL) based liquid-solid extraction (LSE), was first designed to extract the main inorganic and organic iodine compounds (I(-), monoiodo-tyrosine (MIT) and diiodo-tyrosine (DIT)). The optimal extraction conditions were as follows: ultrasonic intensity 100W, IL ([EPy]Br) concentration 200mM, extraction time 30min, liquid/solid ratio 10mL/g, and pH value 6.5. The morphologies of Laminaria were studied by scanning electron microscopy and transmission electron microscopy. The recovery values of I(-), MIT and DIT from Laminaria were in the range of 88% to 94%, and limits of detection were in the range of 59.40 to 283.6ng/g. The proposed method was applied to the extraction and determination of iodine compounds in three Laminaria. The results showed that IL-based LSE could be a promising method for rapid extraction of bioactive iodine from complex food matrices. Copyright © 2017 Elsevier Ltd. All rights reserved.

  4. Automated dispersive liquid-liquid microextraction coupled to high performance liquid chromatography - cold vapour atomic fluorescence spectroscopy for the determination of mercury species in natural water samples.

    Science.gov (United States)

    Liu, Yao-Min; Zhang, Feng-Ping; Jiao, Bao-Yu; Rao, Jin-Yu; Leng, Geng

    2017-04-14

    An automated, home-constructed, and low cost dispersive liquid-liquid microextraction (DLLME) device that directly coupled to a high performance liquid chromatography (HPLC) - cold vapour atomic fluorescence spectroscopy (CVAFS) system was designed and developed for the determination of trace concentrations of methylmercury (MeHg(+)), ethylmercury (EtHg(+)) and inorganic mercury (Hg(2+)) in natural waters. With a simple, miniaturized and efficient automated DLLME system, nanogram amounts of these mercury species were extracted from natural water samples and injected into a hyphenated HPLC-CVAFS for quantification. The complete analytical procedure, including chelation, extraction, phase separation, collection and injection of the extracts, as well as HPLC-CVAFS quantification, was automated. Key parameters, such as the type and volume of the chelation, extraction and dispersive solvent, aspiration speed, sample pH, salt effect and matrix effect, were thoroughly investigated. Under the optimum conditions, linear range was 10-1200ngL(-1) for EtHg(+) and 5-450ngL(-1) for MeHg(+) and Hg(2+). Limits of detection were 3.0ngL(-1) for EtHg(+) and 1.5ngL(-1) for MeHg(+) and Hg(2+). Reproducibility and recoveries were assessed by spiking three natural water samples with different Hg concentrations, giving recoveries from 88.4-96.1%, and relative standard deviations <5.1%.

  5. Removal of nitrogen compounds from Brazilian petroleum samples by oxidation followed by liquid-liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Conceicao, L.; Pergher, S.B.C. [Universidade Regional Integrada do Alto Uruguai e das Misses (URI), Erechim, RS (Brazil). Dept. de Quimica], E-mail: pergher@uricer.edu.br; Oliveira, J.V. [Universidade Regional Integrada do Alto Uruguai e das Misses (URI), Erechim, RS (Brazil). Dept. de Engenharia dos Alimentos; Souza, W.F. [Petroleo Brasileiro S.A. (CENPES/PETROBRAS), Rio de Janeiro, RJ (Brazil). Centro de Pesquisas

    2009-10-15

    This work reports liquid-liquid extraction of nitrogen compounds from oxidized and non-oxidized Brazilian petroleum samples. The experiments were accomplished in a laboratory-scale liquid-liquid apparatus in the temperature range of 303 K-323 K, using methanol, n-methyl-2-pyrrolidone (NMP) and N,Ndimethylformamide (DMF), and their mixtures as extraction solvents, employing solvent to sample volume ratios of 1:2, 1:1 and 2:1, exploring up to three separation stages. Results show that an increase in temperature, solvent to oil ratio, and number of equilibrium stages greatly improves the nitrogen removal from the oxidized sample (from 2600 to 200 ppm). The employed oxidation scheme is thus demonstrated to be an essential and efficient step of sample preparation for the selective liquid-liquid removal of nitrogen compounds. It is shown that the use of mixtures of DMF and NMP as well their use as co-solvents with methanol did not prove to be useful for selective nitrogen extraction since great oil losses were observed in the final process. (author)

  6. Task-specific ionic liquids for An and Ln extraction: unusual speciation and extraction mechanisms

    Energy Technology Data Exchange (ETDEWEB)

    Billard, Isabelle; Jobin, Emilie; Ouadi, Ali; Gaillard, Clotilde [IPHC-DRS, Chimie nucleaire, 23 rue du Loess, BP28, 67037 Strasbourg cedex 2 (France)

    2008-07-01

    Extraction mechanisms of uranium by TBP (tributylphosphate) diluted in an ionic liquid BumimTf{sub 2}N (1-butyl-3-methyl-imidazolium bis(tri-fluoro-methyl-sulfonyl)imide) and by Task-Specific Ionic Liquids (TSILs) bearing a phosphoryl group were investigated. Great differences between these mechanisms and the one in the industrial solvent, dodecane, have been put in evidence. While in dodecane, the neutral species, UO{sub 2}(NO{sub 3}){sub 2}(TBP){sub 2}, is the major extracted complex, in BumimTf{sub 2}N and TSILs, at least two species are extracted with more or less similar proportions. Moreover, no uranyl species with two nitrates could be observed in these ionic liquids. Finally, the mechanisms vary from TBP in BumimTf{sub 2}N to TSILs. These results led to a so-to-say new kind of actinide chemistry. (authors)

  7. Using cyclic liquid-liquid extraction method for isolation and identification of relative compounds during lignin biodegradation

    Institute of Scientific and Technical Information of China (English)

    黄峰; 高培基; 陈嘉翔

    1999-01-01

    By using the cyclic liquid-liquid extraction method the lignin biodegradated derivatives can be effectively extracted from the effluent liquors in ligninolytic enzymes treated kraft pulps. More than forty compounds were identified from the extractives by gas chromatography-mass spectrometry analysis. The result showed that lignin is treated with different ligninolytic enzymes, and the composition and content of the extractives differ obviously. These results suggest that the cyclic liquid-liquid extraction method can be used effectively as one new technique for the study of lignin biodegrada-tion mechanisms.

  8. CELLULOSE EXTRACTION FROM PALM KERNEL CAKE USING LIQUID PHASE OXIDATION

    OpenAIRE

    FARM YAN YAN; DUDUKU KRISHNIAH; MARIANI RAJIN; AWANG BONO

    2009-01-01

    Cellulose is widely used in many aspect and industries such as food industry, pharmaceutical, paint, polymers, and many more. Due to the increasing demand in the market, studies and work to produce cellulose are still rapidly developing. In this work, liquid phase oxidation was used to extract cellulose from palm kernel cake to separate hemicellulose, cellulose and lignin. The method is basically a two-step process. Palm kernel cake was pretreated in hot water at 180°C and followed by liquid ...

  9. Determination of sulfadiazine in phosphate- and DOC-rich agricultural drainage water using solid-phase extraction followed by liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Bouyou, P.A. Léon; Weisser, Johan Juhl; Strobel, Bjarne W.

    2014-01-01

    Trace levels of the veterinary antibiotic compound sulfadiazine (SDZ) can be determined in agricultural drainage water samples with this new method. Optimized sample pretreatment and solid-phase extraction was combined with liquid chromatography coupled to tandem mass spectrometry (SPE LC...... obtained ranged from 104 to 109 % (relative standard deviation 2.8–5.2 %). The new methods enable determination of the veterinary antibiotic compound SDZ in agricultural drainage water from field experiments and monitoring schemes for phosphate- and dissolved organic carbon (DOC)-rich water samples......-MS/MS) using positive electrospray ionization. The linear dynamic range for the LC-MS/MS was assessed from 5 μg/L to 25 mg/L with a 15-point calibration curve displaying a coefficient of correlation r 2 = 0.9915. Agricultural drainage water spiked at a concentration of 25 ng/L gave recoveries between 63 and 98...

  10. Ionic liquid pre-treatment of microalgae and extraction of biomolecules

    OpenAIRE

    2016-01-01

    Liquid-liquid extraction (LLE) techniques are widely used in separation primarily due to ease of scale up. Conventional (LLE) systems based on organic solvents are not suitable for extraction of fragile molecules such as proteins as it would result in denaturation. On the other hand aqueous biphasic system though suitable for extraction of proteins they are restricted by limited polarity range. Ionic liquids are salts which are liquid at room temperature. Ionic liquids have gained interest in...

  11. Liquid-liquid equilibrium extraction of ethanol with mixed solvent for bioethanol concentration

    Institute of Scientific and Technical Information of China (English)

    Hiroaki Habaki; Haihao Hu; Ryuichi Egashira

    2016-01-01

    The extraction of ethanol with the solvents of aldehydes mixed with m-xylene was studied for the bioethanol concentration process. Furfural and benzaldehyde were selected as extraction solvents, with which the solubility of water is smal , expecting large distribution coefficient of ethanol. The liquid–liquid two-phase region was the largest with m-xylene solvent, followed by benzaldehyde and furfural. The region of two liquid–liquid phase be-came larger with the mixed solvent of m-xylene and furfural than that with furfural solvent. The NRTL model was applied to the ethanol–water–furfural–m-xylene system, and the model could well express the liquid–liquid equilibrium of the system. For any solvent used in this study, the separation selectivity of ethanol relative to water decreased as the distribution coefficient of ethanol increased. The separation selectivity with m-xylene was the largest among the employed solvents, but the distribution coefficient was the smal est. The solvent mix-ture of furfural and m-xylene showed relatively high distribution coefficient of ethanol and separation selectivity, even in the higher mass fraction of m-xylene in the solvent phase. The ethanol extraction with a countercurrent multistage extractor by a continuous operation was simulated to evaluate the extraction performance. The ethanol content could be concentrated in the extract phase with relatively small number of extraction stages but low yield of ethanol was obtained.

  12. 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°...

  13. 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°...

  14. Are extraction methods in quantitative assays of pharmacopoeia monographs exhaustive? A comparison with pressurized liquid extraction.

    Science.gov (United States)

    Basalo, Carlos; Mohn, Tobias; Hamburger, Matthias

    2006-10-01

    The extraction methods in selected monographs of the European and the Swiss Pharmacopoeia were compared to pressurized liquid extraction (PLE) with respect to the yield of constituents to be dosed in the quantitative assay for the respective herbal drugs. The study included five drugs, Belladonnae folium, Colae semen, Boldo folium, Tanaceti herba and Agni casti fructus. They were selected to cover different classes of compounds to be analyzed and different extraction methods to be used according to the monographs. Extraction protocols for PLE were optimized by varying the solvents and number of extraction cycles. In PLE, yields > 97 % of extractable analytes were typically achieved with two extraction cycles. For alkaloid-containing drugs, the addition of ammonia prior to extraction significantly increased the yield and reduced the number of extraction cycles required for exhaustive extraction. PLE was in all cases superior to the extraction protocol of the pharmacopoeia monographs (taken as 100 %), with differences ranging from 108 % in case of parthenolide in Tanaceti herba to 343 % in case of alkaloids in Boldo folium.

  15. Optimization of Ultrasonic Extraction and Clean-up Protocol for the Determination of Polycyclic Aromatic Hydrocarbons in Marine Sediments by High-performance Liquid Chromatography Coupled with Fluorescence Detection

    Institute of Scientific and Technical Information of China (English)

    PENG Xuewei; YAN Guofang; LI Xianguo; GUO Xinyun; ZHOU Xiao; WANG Yan

    2012-01-01

    The procedures of ultrasonic extraction and clean-up were optimized for the determination of polycyclic aromatic hydrocarbons(PAHs)in marine sediments.Samples were ultrasonically extracted,and the extracts were purified with a miniaturized silica gel chromatographic column and analyzed with high performance liquid chromatography(HPLC)with a fluorescence detector.Ultrasonication with methanol-dichloromethane(2:1,v/v)mixture gave higher extraction efficiency than that with dichloromethane.Among the three elution solvents used in clean-up step,dichloromethane-hexane(2:3,v/v)mixture was the most satisfactory.Under the optimized conditions,the recoveries in the range of 54.82% to 94.70% with RSDs of 3.02% to 23.22% for a spiked blank,and in the range of 61.20% to 127.08% with RSDs of 7.61% to 26.93% for a spiked matrix,were obtained for the 15 PAHs studied,while the recoveries for a NIST standard reference SRM 1941b were in the range of 50.79% to 83.78% with RSDs of 5.24% to 21.38%.The detection limits were between 0.75ngL-1 and 10.99ngL-1for different PAHs.A sample from the Jiaozhou Bay area was examined to test the established methods.

  16. Liquid-Liquid Extraction and Solid Phase Extraction for Urinary Organic Acids: A Comparative Study from a Resource Constraint Setting.

    Science.gov (United States)

    Kumari, Chandrawati; Varughese, Bijo; Ramji, Siddarth; Kapoor, Seema

    2016-10-01

    Pre analytical process of extraction for accurate detection of organic acids is a crucial step in diagnosis of organic acidemias by GCMS analysis. This process is accomplished either by solid phase extraction (SPE) or by liquid-liquid extraction (LLE). Both extraction procedures are used in different metabolic laboratories all over the world. In this study we compared these two extraction procedures in respect of precision, accuracy, percent recovery of metabolites, number of metabolites isolated, time and cost in a resource constraint setup. We observed that the mean recovery from SPE was 84.1 % and by LLE it was 77.4 % (p value <0.05). Moreover, the average number of metabolites isolated by SPE and LLE was 161.8 ± 18.6 and 140.1 ± 20.4 respectively. The processing cost of LLE was economical. In a cost constraint setting using LLE may be the practical option if used for organic acid analysis.

  17. Equilibrium Studies on Enantioselective Liquid-Liquid Amino Acid Extraction Using a Cinchona Alkaloid Extractant

    NARCIS (Netherlands)

    Schuur, Boelo; Winkelman, Jozef G. M.; Heeres, Hero J.

    2008-01-01

    The enantioselective extraction of aqueous 3,5-dinitrobenzoyl-R,S-leucine (A(R,S)) by a cinchona alkaloid extractant (C) in 1,2-dichloroethane was studied at room temperature (294 K) in a batch system for a range of intake concentrations (10(-4)-10(-3) mol/L) and pH values (3.8-6.6). The experimenta

  18. Extraction of polycyclic aromatic hydrocarbons from smoked fish using pressurized liquid extraction with integrated fat removal

    DEFF Research Database (Denmark)

    Lund, Mette; Duedahl-Olesen, Lene; Christensen, Jan H.

    2009-01-01

    Quantification of polycyclic aromatic hydrocarbons (PAHs) in smoked fish products often requires multiple clean-up steps to remove fat and other compounds that may interfere with the chemical analysis. We present a novel pressurized liquid extraction (PLE) method that integrates exhaustive...

  19. Successive pH- and heat-induced homogenous liquid-liquid extraction.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Feriduni, Behruz

    2016-08-12

    A simple and efficient analytical method known as pH- and heat-induced homogenous liquid-liquid extraction combined with high-performance liquid chromatography has been successfully developed for the extraction and determination of neonicotinoid pesticides in aqueous samples. In this method, a few mL of a water-miscible basic extraction solvent is mixed with a high volume of an aqueous phase containing the analytes and passed through a tube which a portion of the tube is filled with sodium carbonate as a separating agent. By passing the solution, salt is dissolved and the fine droplets of the extraction solvent are formed. The produced droplets go up through the remained solution and collect as a separated layer. In the following, the collected organic phase is removed and placed into a micro tube. Then it is heated in a water bath to form two phases. Several experimental parameters that influence extraction efficiency such as type and volume of extraction solvent, type of phase separation agent, temperature, and extraction time were investigated. Under the optimum conditions, the extraction recoveries and enrichment factors ranged between 51 and 81% and 680 and 1080, respectively. Calibration curves showed a high-level of linearity for all target analytes with coefficients of determination ranging between 0.997 and 0.999. The repeatability of the proposed method expressed as relative standard deviation varied between 3 and 5% (n=6, C=50μgL(-1)), and the detection limits were in the range of 0.52-1.0μgL(-1). Finally, the performance of the method was evaluated by analyzing the selected pesticides in different fruit juice and vegetable samples.

  20. Solvent Extraction: Structure of the Liquid-Liquid Interface Containing a Diamide Ligand.

    Science.gov (United States)

    Scoppola, Ernesto; Watkins, Erik B; Campbell, Richard A; Konovalov, Oleg; Girard, Luc; Dufrêche, Jean-Francois; Ferru, Geoffroy; Fragneto, Giovanna; Diat, Olivier

    2016-08-01

    Knowledge of the (supra)molecular structure of an interface that contains amphiphilic ligand molecules is necessary for a full understanding of ion transfer during solvent extraction. Even if molecular dynamics already yield some insight in the molecular configurations in solution, hardly any experimental data giving access to distributions of both extractant molecules and ions at the liquid-liquid interface exist. Here, the combined application of X-ray and neutron reflectivity measurements represents a key milestone in the deduction of the interfacial structure and potential with respect to two different lipophilic ligands. Indeed, we show for the first time that hard trivalent cations can be repelled or attracted by the extractant-enriched interface according to the nature of the ligand.

  1. Multiple headspace extraction for gas detection in ionic liquids.

    Science.gov (United States)

    Müller, D; Fühl, M; Pinkwart, K; Baltes, N

    2014-10-16

    In this study multiple headspace extraction was used for the first time to measure the saturation concentration of carbon monoxide and oxygen in various ionic liquids (ILs). Many processes in ILs involve the reaction of gases so that the reactant solubility is not a mere characteristical parameter, but understanding the solubility of gases in ILs is required for assessing the feasibility of possible applications. Multiple headspace extraction has proofed to be a powerful tool to obtain solubilities in good accordance with literature data. The measured saturation concentration for carbon monoxide and oxygen in ILs based on rarely researched tetracyanoborates and other anions was in the range of 1.5-6.5mmol/L. The great advantage of multiple headspace extraction is that it is a nonexpensive method that can be realised in most analytical laboratories by combination of a simple gas chromatograph and an eligible headspace injector.

  2. Selective pressurized liquid extraction of polybrominated diphenyl ethers in fish.

    Science.gov (United States)

    Losada, S; Santos, F J; Galceran, M T

    2009-12-15

    A fast and simple method for the analysis of polybrominated diphenyl ethers (PBDEs) in fish samples was developed using a one-step extraction and clean-up by means of pressurized liquid extraction (PLE) combined with gas chromatography-ion trap tandem mass spectrometry (GC-ITMS-MS). The selective PLE method provided to obtain ready-to-analyse extracts without any additional clean-up step, using a sorbent as fat retainer inside the PLE cell. Several PLE operating conditions, such as solvent type, extraction temperature and time, number of cycles and type of fat retainer, were studied. Using Florisil as fat retainer, maximum recoveries of PBDEs (83-108%) with minimum presence of matrix-interfering compounds were obtained using a mixture of n-hexane:dichloromethane 90:10 (v/v) as solvent, an extraction temperature of 100 degrees C and a static extraction time of 5 min in combination with three static cycles. Quality parameters of the method were established using standards and fish samples. Limits of detection and quantification ranged from 10 to 34 pg g(-1) wet weight and between 34 and 68 pg g(-1) wet weight, respectively. In addition, good linearity (between 1 and 500 ng ml(-1)) and high precision (RSD %<15%) were achieved. The method was validated using the standard reference material SRM-1945 (whale blubber) and was then applied to the analysis of PBDEs in fish samples.

  3. Hydrolytical instability of hydroxyanthraquinone glycosides in pressurized liquid extraction.

    Science.gov (United States)

    Wianowska, Dorota

    2014-05-01

    Hydroxyanthraquinones represent a group of pharmacologically active compounds characteristic for plants of the Rumex and Rheum genera. These compounds in the human intestine act as laxative compounds. As they cause the greatest side effects and are often abused by the public, their accurate analysis in plants and plant-derived laxatives is much needed. To isolate compounds from plants, pressurized liquid extraction (PLE) is frequently applied. The technique has been regarded, so far, as very effective, even in isolation of sensitive compounds for which exposure time in high temperature has a negative impact. This work demonstrates some interesting and surprising results accompanying PLE of hydroxyanthraquinones from the Rumex crispus L. root using methanol/water mixtures as extractant. The presented results demonstrate that glycoside forms of hydroxyanthraquinones (emodin-8-O-β-D-glucopyranoside, chrysophanol-8-O-β-D-glucopyranoside, and physcion-8-O-β-D-glucopyranoside) are hydrolytically unstable even in the short-lasting PLE. The increase of water concentration in the extractant leads to the increase of the transformation degree of the glycoside forms to the corresponding aglycones (emodin, chrysophanol, and physcion), increasing the concentration of the latter. The rise in the PLE temperature accelerates the hydrolytical degradation of the glycoside forms. The extension of the extraction time also intensifies this process. The presented results show that extraction of glycosides using extractants containing water can lead to false conclusions about the chemical composition of plants.

  4. A novel solid-phase extraction for the concentration of sweeteners in water and analysis by ion-pair liquid chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Gan, Zhiwei; Sun, Hongwen; Wang, Ruonan; Feng, Biting

    2013-01-25

    A highly sensitive method for the simultaneous trace (ng/L) quantification of seven commonly used artificial sweeteners in a variety of water samples using solid-phase extraction and ion-pair high-performance liquid chromatography (HPLC) triple quadrupole mass spectrometer with an electrospray ionization source (ESI-MS) in negative ion multiple reaction monitoring mode was developed. Ten solid phase extraction (SPE) cartridges were tested to evaluate their applicability for the pre-concentration of the analytes, and their loading and eluting parameters were optimized. Satisfactory recoveries (77-99%) of all of the studied sweeteners were obtained using a Poly-Sery PWAX cartridge with 25 mM sodium acetate solution (pH 4) as wash buffer and methanol containing 1mM tris (hydroxymethyl) amino methane (TRIS) as eluent. The method is sound and does not require pH adjustment or buffering of water samples. The HPLC separation was performed on an Athena C18-WP column with water and acetonitrile, both containing 5mM ammonium acetate and 1mM TRIS as mobile phases, in gradient elution mode. The linearity, precision, and accuracy of the method were evaluated, and good reproducibility was obtained. Method quantification limits varied between 0.4 and 7.5 ng/L for different water samples. The post-extraction spike method was applied to assess matrix effects, and quantification was achieved using internal standard calibration to overcome the unavoidable matrix effects during ESI-MS analysis. The method was applied to the analysis of thirteen water samples from Tianjin, China, including wastewater, tap water, surface water, and groundwater. The method described here is time-saving, accurate and precise, and is suitable for monitoring artificial sweeteners in different water matrices.

  5. Recovery of acids from anaerobic acidification broth by liquid-liquid extraction.

    Science.gov (United States)

    Alkaya, Emrah; Kaptan, Serkan; Ozkan, Leyla; Uludag-Demirer, Sibel; Demirer, Göksel N

    2009-11-01

    In this study, anaerobic acidification of sugar beet processing wastes and subsequent liquid-liquid extraction of produced fermentation metabolites were investigated. The aim of extraction experiments was to asses the influence of pH and extractant (trioctylphosphine oxide (TOPO) in kerosene) concentrations on the recovery of volatile fatty acids (VFAs) from fermentation broth. The effect of TOPO in kerosene concentration was as crucial as the effect of pH on the recovery of VFAs via extraction. Consequently, pH 2.5 was determined as optimum. At this pH, percent recoveries of VFAs were changed from 43% to 98%, depending on the type of the acid extracted (acetic, butyric, propionic and valeric acids) and the concentration of TOPO in kerosene (5-20%). As the concentration of TOPO in kerosene was increased, efficiency of extraction was increased. As a result, highest VFA recoveries (61-98%) were observed at 20% TOPO in kerosene with distribution ratio values ranging between 1.54 and 40.79. At pH 2.5, the increase in TOPO concentration directly increased the chemical oxygen demand (COD) removal efficiencies, as it does for total VFA recovery. Up to 72% COD removals were achieved, at 20% TOPO in kerosene at pH 2.5, while the removal efficiencies remained between 19% and 22% at pH 5.5.

  6. In situ recovery of 2,3-butanediol from fermentation by liquid-liquid extraction.

    Science.gov (United States)

    Anvari, Masumeh; Pahlavanzadeh, Hassan; Vasheghani-Farahani, Ebrahim; Khayati, Gholam

    2009-02-01

    End-product conversion, low product concentration and large volumes of fermentation broth, the requirements for large bioreactors, in addition to the high cost involved in generating the steam required to distil fermentation products from the broth largely contributed to the decline in fermentative products. These considerations have motivated the study of organic extractants as a means to remove the product during fermentation and minimize downstream recovery. The aim of this study is to assess the practical applicability of liquid-liquid extraction in 2,3-butanediol fermentations. Eighteen organic solvents were screened to determine their biocompatibility, and bioavailability for their effects on Klebsiella pneumoniae growth. Candidate solvents at first were screened in shake flasks for toxicity to K. pneumoniae. Cell density and substrate consumption were used as measures of cell toxicity. The possibility of employing oleyl alcohol as an extraction solvent to enhance end product in 2,3-butanediol fermentation was evaluated. Fermentation was carried out at an initial glucose concentration of 80 g/l. Oleyl alcohol did not inhibit the growth of the fermentative organism. 2,3-Butanediol production increased from 17.9 g/l (in conventional fermentation) to 23.01 g/l (in extractive fermentation). Applying oleyl alcohol as the extraction solvent, about 68% of the total 2,3-butanediol produced was extracted.

  7. [Preparation and applications of a supported liquid-liquid extraction column with a composite diatomite material].

    Science.gov (United States)

    Bao, Jianmin; Ma, Zhishuang; Sun, Ying; Wang, Yongzun; Li, Youxin

    2012-08-01

    A rapid and special supported liquid-liquid extraction (SLE) column was developed with a composite diatomite material. The SLE column was evaluated by high performance liquid chromatography (HPLC) with acidic, neutral and alkaline compounds dissolved in water. Furthermore, some real complex samples were also analyzed by HPLC with the SLE method. The recoveries of benzoic acid (acidic), p-nitroaniline (alkaline) and 4-hydroxy-benzoic methyl ester (neutral) treated by the SLE column were 90.6%, 98.1% and 97.7%. However, the recoveries of the three compounds treated by traditional liquid-liquid extraction (LLE) method were 71.9%, 81.9% and 83.9%. The results showed that the SLE technique had higher recoveries than the traditional LLE method. The spiked recoveries of the complex samples, such as benzoic acid in Sprite and dexamethasone acetate, chlorphenamine maleate, indomethacin in bovine serum, were between 80% and 110% and the relative standard deviations (RSDs) were less than 15%. For biological specimen, the results could be accepted. Meantime, many disadvantages associated with traditional LLE method, such as emulsion formation, didn't occur using SLE column. The SLE column technique is a good sample preparation method with many advantages, such as rapid, simple, robust, easily automated, high recovery and high-throughput, which would be widely used in the future.

  8. Simultaneous determination of mono- and disubstituted polyfluoroalkyl phosphates in drinking water by liquid chromatography-electrospray tandem mass spectrometry.

    Science.gov (United States)

    Ding, Huanhuan; Peng, Hui; Yang, Min; Hu, Jianying

    2012-03-02

    A sensitive liquid chromatography-electrospray tandem mass spectrometry method was established for the simultaneous determination of five monosubstituted polyfluoroalkyl phosphates (monoPAPs) and eight disubstituted polyfluoroalkyl phosphates (diPAPs) in drinking water. Complete separation and good retention for 13 polyfluoroalkyls phosphates (PAPs) were achieved with a Waters ACUITY UPLC BEH C8 column using a mixture of methanol/water containing 0.1% NH₄OH as the mobile phases. Extraction of drinking water samples was performed on weak anion exchange (WAX) cartridges, and the recoveries of target compounds were from 65 to 110%. The limits of quantization (LOQs) for 13 analytes were in the range of 0.4-40 ng/L. This method was applied to analyze the PAPs in drinking water samples from three cities in China. Of the 13 PAPs, six PAPs including 6:2 monoPAP (13.0 ng/L), 8:2 monoPAP (3.6 ng/L), 10:1 monoPAP (4.3-70.3 ng/L), 10:2 monoPAP (1.4-5.6 ng/L), 8:2 diPAP (0.10 ng/L), and 10:1 diPAP (0.8-3.8 ng/L) were detected.

  9. Liquid-Liquid Extraction-Chromogenic Systems Containing Iron(III), 4-Nitrocatechol and Tetrazolium Salts

    OpenAIRE

    Galya K. Toncheva; Teodora S. Stefanova; Gavazov, Kiril B.

    2015-01-01

    Complex formation and liquid-liquid extraction were studied in systems containing iron(III), 4-nitrocatechol (4NC),tetrazolium salt (TZS), water and organic solvent. Three different TZS were used: 3-(4,5-dimethyl-2-thiazol)-2,5-diphenyl-2H-tetrazolium bromide (MTT), 3-(2-naphtyl)-2,5-diphenyl-2H-tetrazolium chloride (Tetrazolium violet, TV) and 2-(4-iodophenyl)-3-(4-nitrophenyl)-5-phenyl-2H-tetrazolium chloride (INT).The cations of the first two TZSs (TZ+: MTT+ and TV+) form intensively color...

  10. 40 YEARS OF EXPERIENCE WITH LIQUID-LIQUID EXTRACTION EQUIPMENT IN THE NUCLEAR INDUSTRY

    Energy Technology Data Exchange (ETDEWEB)

    Drain, F.; Vinoche, R.; Duhamet, J.

    2003-02-27

    Three types of liquid-liquid extraction equipment are used in industrial reprocessing plants. Each is described below, with a special focus on pulsed columns and centrifugal extractors, which have been the subject of an extensive R&D program by the French Atomic Energy Commission (CEA). Various models have been developed to simulate equipment behavior and flowsheets. The excellent results obtained during industrial operation of the UP3 and UP2-800 plants in La Hague have confirmed the validity of the choices made during the design phases and pave the way for future improvement of the reprocessing process, from a technical and a financial standpoint.

  11. CELLULOSE EXTRACTION FROM PALM KERNEL CAKE USING LIQUID PHASE OXIDATION

    Directory of Open Access Journals (Sweden)

    FARM YAN YAN

    2009-03-01

    Full Text Available Cellulose is widely used in many aspect and industries such as food industry, pharmaceutical, paint, polymers, and many more. Due to the increasing demand in the market, studies and work to produce cellulose are still rapidly developing. In this work, liquid phase oxidation was used to extract cellulose from palm kernel cake to separate hemicellulose, cellulose and lignin. The method is basically a two-step process. Palm kernel cake was pretreated in hot water at 180°C and followed by liquid oxidation process with 30% H2O2 at 60°C at atmospheric pressure. The process parameters are hot water treatment time, ratio of palm kernel cake to H2O2, liquid oxidation reaction temperature and time. Analysis of the process parameters on production cellulose from palm kernel cake was performed by using Response Surface Methodology. The recovered cellulose was further characterized by Fourier Transform Infrared (FTIR. Through the hot water treatment, hemicellulose in the palm kernel cake was successfully recovered as saccharides and thus leaving lignin and cellulose. Lignin was converted to water soluble compounds in liquid oxidation step which contains small molecular weight fatty acid as HCOOH and CH3COOH and almost pure cellulose was recovered.

  12. Increment of the operational stability of the NGL I plant located in the Tablazo Petrochemical Complex, working with a low feed gas flow rate

    Energy Technology Data Exchange (ETDEWEB)

    Mendez, Alejandro

    2004-07-01

    The function of the plant NGL I is to extract the ethane and the liquids of the current of natural gas coming from Maracaibo Lake, emphatically in the ethane and propane for being a raw material for the olefins synthesis. The needed temperature for the condensation takes place cooling the dehydrated feed gas, by means of the heat exchange with two currents, cooling propane and the other cold methane gas. In 1998 some improvements to the plant were made, which are known as (MERE) (Ethane Recovery Improvements Project), these modifications were made in order to enhance the ethane recovery during the process, however, when it started to work under this modifications high instability in the performance of the compressor located in the refrigeration system was observed, which produced the shutdown of the ethane recovery process when working with feed gas stream flow rates (under 130 MMSCFD). Moreover, during the last years a decrease in the feed gas flow has been observed, in a mean of 120 MMSCFD, which has had a negative effect on the plant, because it has worked in a non-continuous state. Thanks to several improvements implemented in the actuality, we have achieved to diminish the minimal flow of operation of the plant to 95 MMPCSD, allowing the ethane production at this flow of feeding and increased the operational stability of the plant of LNG I. (author)

  13. Solvent extraction of gold using ionic liquid based process

    Science.gov (United States)

    Makertihartha, I. G. B. N.; Zunita, Megawati; Rizki, Z.; Dharmawijaya, P. T.

    2017-01-01

    In decades, many research and mineral processing industries are using solvent extraction technology for metal ions separation. Solvent extraction technique has been used for the purification of precious metals such as Au and Pd, and base metals such as Cu, Zn and Cd. This process uses organic compounds as solvent. Organic solvents have some undesired properties i.e. toxic, volatile, excessive used, flammable, difficult to recycle, low reusability, low Au recovery, together with the problems related to the disposal of spent extractants and diluents, even the costs associated with these processes are relatively expensive. Therefore, a lot of research have boosted into the development of safe and environmentally friendly process for Au separation. Ionic liquids (ILs) are the potential alternative for gold extraction because they possess several desirable properties, such as a the ability to expanse temperature process up to 300°C, good solvent properties for a wide range of metal ions, high selectivity, low vapor pressures, stability up to 200°C, easy preparation, environmentally friendly (commonly called as "green solvent"), and relatively low cost. This review paper is focused in investigate of some ILs that have the potentials as solvent in extraction of Au from mineral/metal alloy at various conditions (pH, temperature, and pressure). Performances of ILs extraction of Au are studied in depth, i.e. structural relationship of ILs with capability to separate Au from metal ions aggregate. Optimal extraction conditon in order to gain high percent of Au in mineral processing is also investigated.

  14. Application of Ionic Liquids in the Microwave-Assisted Extraction of Proanthocyanidins from Larix gmelini Bark

    OpenAIRE

    Yuangang Zu; Chunjian Zhao; Lin Zhang,; Fengjian Yang; Xiaowei Sun; Lei Yang

    2012-01-01

    Ionic liquid based, microwave-assisted extraction (ILMAE) was successfully applied to the extraction of proanthocyanidins from Larix gmelini bark. In this work, in order to evaluate the performance of ionic liquids in the microwave-assisted extraction process, a series of 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were evaluated for extraction yield, and 1-butyl-3-methylimidazolium bromide was selected as the optimal solvent. In addition, ...

  15. Extraction of pesticides in water samples using vortex-assisted liquid-liquid microextraction.

    Science.gov (United States)

    Jia, Chunhong; Zhu, Xiaodan; Wang, Jihua; Zhao, Ercheng; He, Min; Chen, Li; Yu, Pingzhong

    2010-09-10

    A simple solvent microextraction method termed vortex-assisted liquid-liquid microextraction (VALLME) coupled with gas chromatography micro electron-capture detector (GC-microECD) has been developed and used for the pesticide residue analysis in water samples. In the VALLME method, aliquots of 30 microL toluene used as extraction solvent were directly injected into a 25 mL volumetric flask containing the water sample. The extraction solvent was dispersed into the water phase under vigorously shaking with the vortex. The parameters affecting the extraction efficiency of the proposed VALLME such as extraction solvent, vortex time, volumes of extraction solvent and salt addition were investigated. Under the optimum condition, enrichment factors (EFs) in a range of 835-1115 and limits of detection below 0.010 microg L(-1) were obtained for the determination of target pesticides in water. The calculated calibration curves provide high levels of linearity yielding correlation coefficients (r(2)) greater than 0.9958 with the concentration level ranged from 0.05 to 2.5 microg L(-1). Finally, the proposed method has been successfully applied to the determination of pesticides from real water samples and acceptable recoveries over the range of 72-106.3% were obtained.

  16. Ecotoxicology of heavy metals: Liquid-phase extraction by nanosorbents

    Science.gov (United States)

    Burakov, A.; Romantsova, I.; Babkin, A.; Neskoromnaya, E.; Kucherova, A.; Kashevich, Z.

    2015-11-01

    The paper considers the problem of extreme toxicity heavy metal compounds dissolved in wastewater and liquid emissions of industrial enterprises to living organisms and environment as a whole. The possibility of increasing extraction efficiency of heavy metal ions by sorption materials was demonstrated. The porous space of the latter was modified by carbon nanotubes (CNTs) during process of the chemical vapour deposition (CVD) of carbon on metal oxide catalysts. The increasing of the sorption capacity (10-30%) and the sorption rate of nanomodified activated carbons in comparison with standard materials in the example of absorption of Co2+ and Ni2+ ions from aqueous solutions was proven.

  17. The Liquid-Liquid Extraction of Toxic Metals (Cd, Hg and Pb by Calixarenes

    Directory of Open Access Journals (Sweden)

    D. Max Roundhill

    2009-12-01

    Full Text Available Toxic metals (Cd, Hg and Pb are mostly present in the environment due to natural phenomenon and human activities as well. Exposure of these non-essential elements in the environment causes severe effects. They are known to cause problems in humans as well as in aquatic life. In this work, we demonstrate various studies regarding liquid-liquid extraction of selected ions with different functionalized calixarenes. This review article briefly discusses several molecular designs of calixarenes for divalent ion (Cd2+, Hg2+ and Pb2+ recognition; as well as the relationship between structure and selectivity of the macrocycles is elaborated. The article does not, however, attempt to cover all of the different approaches to these toxic metal ions extraction.

  18. Liquid-Liquid Extraction-Chromogenic Systems Containing Iron(III, 4-Nitrocatechol and Tetrazolium Salts

    Directory of Open Access Journals (Sweden)

    Galya K. Toncheva

    2015-03-01

    Full Text Available Complex formation and liquid-liquid extraction were studied in systems containing iron(III, 4-nitrocatechol (4NC,tetrazolium salt (TZS, water and organic solvent. Three different TZS were used: 3-(4,5-dimethyl-2-thiazol-2,5-diphenyl-2H-tetrazolium bromide (MTT, 3-(2-naphtyl-2,5-diphenyl-2H-tetrazolium chloride (Tetrazolium violet, TV and 2-(4-iodophenyl-3-(4-nitrophenyl-5-phenyl-2H-tetrazolium chloride (INT.The cations of the first two TZSs (TZ+: MTT+ and TV+ form intensively colored (molar absorptivity of 4.6´104 L mol–1 cm–1 and 4.4´104 L mol–1 cm–1, respectively chloroform extractable ion-associates with the FeIII-4NC anionic chelate. These ternary complexes can be represented with the following general formula: (TZ+3[FeIII(4NC3]3−.

  19. Liquid-solid extraction coupled with magnetic solid-phase extraction for determination of pyrethroid residues in vegetable samples by ultra fast liquid chromatography.

    Science.gov (United States)

    Jiang, Chunzhu; Sun, Ying; Yu, Xi; Gao, Yan; Zhang, Lei; Wang, Yuanpeng; Zhang, Hanqi; Song, Daqian

    2013-09-30

    In this study, liquid-solid extraction coupled with magnetic solid-phase extraction was successfully developed for the extraction of pyrethroid residues in vegetable samples. The analytes were determined by ultra fast liquid chromatography. The pyrethroids were extracted by liquid-solid extraction and then adsorbed onto magnetic adsorbent. Magnetic adsorbent, C18-functionalized ultrafine magnetic silica nanoparticles, was synthesized by chemical coprecipitation, silanization and alkylation. The analytes adsorbed onto the magnetic adsorbent can be simply and rapidly isolated from sample solution with a strong magnet on the bottom of the extraction vessel. The extraction parameters, such as liquid-solid extraction solvent, liquid-solid extraction time, the amount of magnetic adsorbent, magnetic solid-phase extraction time and magnetic solid-phase extraction desorption solvent, were optimized to improve the extraction efficiency. The analytical performances of this method, including linear range, detection limit, precision, and recovery were evaluated. The limits of detection for pyrethroid were between 0.63 and 1.2 ng g(-1). Recoveries obtained by analyzing the four spiked vegetable samples were between 76.0% and 99.5%. The results showed that the present method was a simple, accurate and high efficient approach for the determination of pyrethroids in the vegetable samples.

  20. Thiolene and SIFEL-based Microfluidic Platforms for Liquid-Liquid Extraction.

    Science.gov (United States)

    Goyal, Sachit; Desai, Amit V; Lewis, Robert W; Ranganathan, David R; Li, Hairong; Zeng, Dexing; Reichert, David E; Kenis, Paul J A

    2014-01-01

    Microfluidic platforms provide several advantages for liquid-liquid extraction (LLE) processes over conventional methods, for example with respect to lower consumption of solvents and enhanced extraction efficiencies due to the inherent shorter diffusional distances. Here, we report the development of polymer-based parallel-flow microfluidic platforms for LLE. To date, parallel-flow microfluidic platforms have predominantly been made out of silicon or glass due to their compatibility with most organic solvents used for LLE. Fabrication of silicon and glass-based LLE platforms typically requires extensive use of photolithography, plasma or laser-based etching, high temperature (anodic) bonding, and/or wet etching with KOH or HF solutions. In contrast, polymeric microfluidic platforms can be fabricated using less involved processes, typically photolithography in combination with replica molding, hot embossing, and/or bonding at much lower temperatures. Here we report the fabrication and testing of microfluidic LLE platforms comprised of thiolene or a perfluoropolyether-based material, SIFEL, where the choice of materials was mainly guided by the need for solvent compatibility and fabrication amenability. Suitable designs for polymer-based LLE platforms that maximize extraction efficiencies within the constraints of the fabrication methods and feasible operational conditions were obtained using analytical modeling. To optimize the performance of the polymer-based LLE platforms, we systematically studied the effect of surface functionalization and of microstructures on the stability of the liquid-liquid interface and on the ability to separate the phases. As demonstrative examples, we report (i) a thiolene-based platform to determine the lipophilicity of caffeine, and (ii) a SIFEL-based platform to extract radioactive copper from an acidic aqueous solution.

  1. Miniaturized preconcentration methods based on liquid-liquid extraction and their application in inorganic ultratrace analysis and speciation: A review

    Science.gov (United States)

    Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2009-01-01

    Liquid-liquid extraction (LLE) is widely used as a pre-treatment technique for separation and preconcentration of both organic and inorganic analytes from aqueous samples. Nevertheless, it has several drawbacks, such as emulsion formation or the use of large volumes of solvents, which makes LLE expensive and labour intensive. Therefore, miniaturization of conventional liquid-liquid extraction is needed. The search for alternatives to the conventional LLE using negligible volumes of extractant and the minimum number of steps has driven the development of three new miniaturized methodologies, i.e. single-drop microextraction (SDME), hollow fibre liquid-phase microextraction (HF-LPME) and dispersive liquid-liquid microextraction (DLLME). The aim of this paper is to provide an overview of these novel preconcentration approaches and their potential use in analytical labs involved in inorganic (ultra)trace analysis and speciation. Relevant applications to the determination of metal ions, metalloids, organometals and non-metals are included.

  2. Miniaturized preconcentration methods based on liquid-liquid extraction and their application in inorganic ultratrace analysis and speciation: A review

    Energy Technology Data Exchange (ETDEWEB)

    Pena-Pereira, Francisco; Lavilla, Isela [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Quimica, Universidad de Vigo, Campus As Lagoas-Marcosende s/n, 36310 Vigo (Spain); Bendicho, Carlos [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Quimica, Universidad de Vigo, Campus As Lagoas-Marcosende s/n, 36310 Vigo (Spain)], E-mail: bendicho@uvigo.es

    2009-01-15

    Liquid-liquid extraction (LLE) is widely used as a pre-treatment technique for separation and preconcentration of both organic and inorganic analytes from aqueous samples. Nevertheless, it has several drawbacks, such as emulsion formation or the use of large volumes of solvents, which makes LLE expensive and labour intensive. Therefore, miniaturization of conventional liquid-liquid extraction is needed. The search for alternatives to the conventional LLE using negligible volumes of extractant and the minimum number of steps has driven the development of three new miniaturized methodologies, i.e. single-drop microextraction (SDME), hollow fibre liquid-phase microextraction (HF-LPME) and dispersive liquid-liquid microextraction (DLLME). The aim of this paper is to provide an overview of these novel preconcentration approaches and their potential use in analytical labs involved in inorganic (ultra)trace analysis and speciation. Relevant applications to the determination of metal ions, metalloids, organometals and non-metals are included.

  3. Trace level determination of beta-blockers in waste waters by highly selective molecularly imprinted polymers extraction followed by liquid chromatography-quadrupole-linear ion trap mass spectrometry.

    Science.gov (United States)

    Gros, Meritxell; Pizzolato, Tânia-Mara; Petrović, Mira; de Alda, Maria José López; Barceló, Damià

    2008-05-02

    This paper describes the development of an analytical methodology to determine eight beta-blockers in waste waters using molecularly imprinted polymers (MIPs) as extraction and pre-concentration material, followed by liquid chromatography-quadrupole-linear ion trap mass spectrometry (LC-QqLIT MS). The advantages offered by MIPs, in terms of selectivity and specificity, were compared with the most commonly polymeric materials used (the lipophilic-hydrophilic balanced Oasis HLB cartridges). Even though recoveries achieved with both sorbents were similar, ranging from 50 to 110% for sewage treatment plant (STP) effluent and 40-110 for STP influent, respectively, MIPs provided lower method detection limits than Oasis HLB, due to their specificity for target analytes and closely related analogues. Method detection limits (MDL) achieved using MIPs ranged from 0.2 to 6.4 ng/L for STP effluent and from 0.4 to 6.5 ng/L for STP influent. To highlight the advantages of MIPs against conventional polymeric cartridges, a detailed matrix effects study as well as cross reactivity tests were performed. For the latter purpose, the extraction efficiency of some pharmaceuticals and pesticides belonging to different therapeutic classes was assessed. LC-QqLIT MS, used for quantification and confirmation, proved to be a powerful analytical tool, as instrumental detection limits (IDL) achieved ranged from 0.2 to 2.7 pg injected (in multiple reaction monitoring mode (MRM)). In addition the inclusion of high sensitive MS/MS scans for each compound when working in Information Dependent Acquisition mode (IDA) provided extra confirmation for unequivocal identification of target compounds in complex environmental matrices.

  4. Graphene-derivatized silica as an efficient solid-phase extraction sorbent for pre-concentration of fluoroquinolones from water followed by liquid-chromatography fluorescence detection.

    Science.gov (United States)

    Speltini, Andrea; Sturini, Michela; Maraschi, Federica; Consoli, Luana; Zeffiro, Alberto; Profumo, Antonella

    2015-01-30

    This work presents a novel analytical method based on graphene for the determination of five widely used fluoroquinolones (FQs) in aqueous matrices. The procedure entails solid-phase extraction (SPE) on graphene-derivatized silica (200mg), followed by liquid chromatography with fluorescence detection. Monolayer graphene oxide (GO) flakes were covalently bonded onto aminopropyl silica microparticles, and then treated with aqueous hydrazine to obtain the reduced GO (RGO). The final material (RGO-silica) was characterized by thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and BET analysis, and for the first time evaluated as mixed-mode sorbent for the SPE of FQs from natural waters. Accuracy was studied on tap/raw river water in the concentration range 5-10,000ngL(-1), obtaining mean absolute recoveries from 72 to 118%. The inter-day precision was good, showing relative standard deviations (RSDs) in the range 5-15%. Sample volumes up to 1L provided enrichment factors up to 1000, achieving accurate quantification of concentrations as low as 5ngL(-1). The analytes were simultaneously and quantitatively eluted from the RGO-silica cartridge in a single fraction by using acetonitrile combined with aqueous tetrabutyl ammonium hydroxide. The batch-to-batch reproducibility was verified on three independently prepared RGO-silica samples. RGO-silica was advantageous in terms of adsorption capacity and reusability with respect to commercial sorbents; the cartridge proved to be reusable for at least 10 consecutive extractions, with no significant loss of efficiency (recovery >70%). The analytical procedure was applied to the determination of FQs in actual environmental waters.

  5. Selective extraction of emerging contaminants from water samples by dispersive liquid-liquid microextraction using functionalized ionic liquids.

    Science.gov (United States)

    Yao, Cong; Li, Tianhao; Twu, Pamela; Pitner, William R; Anderson, Jared L

    2011-03-25

    Functionalized ionic liquids containing the tris(pentafluoroethyl)trifluorophosphate (FAP) anion were used as extraction solvents in dispersive liquid-liquid microextraction (DLLME) for the extraction of 14 emerging contaminants from water samples. The extraction efficiencies and selectivities were compared to those of an in situ IL DLLME method which uses an in situ metathesis reaction to exchange 1-butyl-3-methylimidazolium chloride (BMIM-Cl) to 1-butyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide (BMIM-NTf(2)). Compounds containing tertiary amine functionality were extracted with high selectivity and sensitivity by the 1-(6-amino-hexyl)-1-methylpyrrolidinium tris(pentafluoroethyl)trifluorophosphate (HNH(2)MPL-FAP) IL compared to other FAP-based ILs and the BMIM-NTf(2) IL. On the other hand, polar or acidic compounds without amine groups exhibited higher enrichment factors using the BMIM-NTf(2) IL. The detection limits for the studied analytes varied from 0.1 to 55.1 μg/L using the traditional IL DLLME method with the HNH(2)MPL-FAP IL as extraction solvent, and from 0.1 to 55.8 μg/L using in situ IL DLLME method with BMIM-Cl+LiNTf(2) as extraction solvent. A 93-fold decrease in the detection limit of caffeine was observed when using the HNH(2)MPL-FAP IL compared to that obtained using in situ IL DLLME method. Real water samples including tap water and creek water were analyzed with both IL DLLME methods and yielded recoveries ranging from 91% to 110%.

  6. Multi-residue analysis of pharmaceuticals in aqueous environmental samples by online solid-phase extraction-ultra-high-performance liquid chromatography-tandem mass spectrometry: optimisation and matrix effects reduction by quick, easy, cheap, effective, rugged and safe extraction.

    Science.gov (United States)

    Bourdat-Deschamps, Marjolaine; Leang, Sokha; Bernet, Nathalie; Daudin, Jean-Jacques; Nélieu, Sylvie

    2014-07-04

    The aim of this study was to develop and optimise an analytical method for the quantification of a bactericide and 13 pharmaceutical products, including 8 antibiotics (fluoroquinolones, tetracyclines, sulfonamides, macrolide), in various aqueous environmental samples: soil water and aqueous fractions of pig slurry, digested pig slurry and sewage sludge. The analysis was performed by online solid-phase extraction coupled to ultra-high performance liquid chromatography with tandem mass spectrometry (online SPE-UHPLC-MS-MS). The main challenge was to minimize the matrix effects observed in mass spectrometry, mostly due to ion suppression. They depended on the dissolved organic carbon (DOC) content and its origin, and ranged between -22% and +20% and between -38% and -93% of the signal obtained without matrix, in soil water and slurry supernatant, respectively. The very variable levels of these matrix effects suggested DOC content cut-offs above which sample purification was required. These cut-offs depended on compounds, with concentrations ranging from 30 to 290mgC/L for antibiotics (except tylosine) up to 600-6400mgC/L for the most apolar compounds. A modified Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction procedure was therefore optimised using an experimental design methodology, in order to purify samples with high DOC contents. Its performance led to a compromise, allowing fluoroquinolone and tetracycline analysis. The QuEChERS extraction salts consisted therefore of sodium acetate, sodium sulfate instead of magnesium sulfate, and sodium ethylenediaminetetraacetate (EDTA) as a ligand of divalent cations. The modified QuEChERS procedure employed for the extraction of pharmaceuticals in slurry and digested slurry liquid phases reduced the matrix effects for almost all the compounds, with extraction recoveries generally above 75%. The performance characteristics of the method were evaluated in terms of linearity, intra-day and inter

  7. CONTRIBUTION TO THE DEVELOPMENT OF A SIMULATION SOFTWARE PERFORMANCE AND SHARING RATIO IN LIQUID-LIQUID EXTRACTION

    Directory of Open Access Journals (Sweden)

    A. Hadj Seyd

    2015-07-01

    Full Text Available The present work is to develop software to predict the value yield and the distribution coefficient in the process of liquid-liquid extraction of components of a mixture, from mathematical models expressing these entities, based on equations equilibrium between liquid-liquid phases, and predict the conditions under which the extraction operation is favorable, unfavorable or impossible to realize, by studying the variation of the entities cited, based on the parameters influencing the extraction, which are: initial concentrations, rate of solvent and pH, in the case of a simple extraction (extraction of neutral products or when it is reactive (extraction of complex acids or bases for one or more components.The programming language used is "Delphi" which is a very powerful oriented object programming under Windows.

  8. Extraction of plutonium(IV) by diglycolamide extractants in room temperature ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    Prabhu, Dattaprasad R.; Raut, Dhaval R.; Murali, Mallekav S.; Mohapatra, Prasanta K. [Bhabha Atomic Research Centre, Mumbai (India). Radiochemistry Div.

    2017-06-01

    Extraction of Pu(IV) was investigated using solutions of two diglycolamide extractants viz., N,N,N{sup '},N{sup '}-tetra-n-octyldiglycolamide (TODGA) and its branched homolog, N,N,N{sup '},N{sup '}-tetra(2-ethylhexyl) diglycolamide (T2EHDGA), dissolved in two imidazolium based room temperature ionic liquids viz., 1-butyl-3-methylimidazolium bis(trifluoromethanesulphonyl) imide ([C{sub 4}mim][NTf{sub 2}]) and 1-octyl-3-methylimidazolium bis(trifluoromethanesulphonyl) imide ([C{sub 8}mim][NTf{sub 2}]) from aqueous nitric acid medium. The extraction kinetics was found to be extremely slow which is reported for the first time for analogous extraction systems and took as long as 30 h to attain equilibrium D{sub Pu} values. In general, TODGA based solvents showed better extraction of Pu(IV) than the T2EHDGA based solvents, one order of magnitude higher, and though both the ionic liquids ultimately yielded comparable D{sub Pu} values, attainment of equilibrium was slower with [C{sub 4}mim][NTf{sub 2}]. The extracted species conformed to 1:1 for TODGA in both the ionic liquids while a mixture of 1:1 and 1:2 species was observed for T2EHDGA at 1 M HNO{sub 3} which changed to 1:1 species at 4 M HNO{sub 3}. The extracted species is proposed to be (Pu(L){sub x}{sup 4+}){sub IL} (where, L is the extractant and x=1 or 2) at lower acidities suggesting a cation exchange mechanism which changes over to (Pu(NO{sub 3}){sub 4} .L){sub IL} at 4 M HNO{sub 3} conforming to a solvation mechanism for all the systems except for T2EHDGA-[C{sub 8}mim][NTf{sub 2}]. UV-VIS spectroscopic studies were carried out to throw light on the nature of the extracted species.

  9. Homogeneous liquid-liquid extraction method for the selective separation and preconcentration of ultra trace molybdenum.

    Science.gov (United States)

    Ghiasvand, A R; Shadabi, S; Mohagheghzadeh, E; Hashemi, P

    2005-05-15

    A new simple and efficient homogeneous liquid-liquid extraction method for the selective separation and preconcentration of molybdenyl ions was developed. alpha-Benzoin oxime (ABO) was investigated as a complexing ligand, and perfluorooctanoate ion (PFOA(-)) was applied as a phase-separator agent under strongly acidic conditions. Under the optimal conditions ([ABO]=2.1x10(-3)M, [PFOA(-)]=1.8x10(-2)M, [HNO(3)]=1.7M, [acetone]=11.8% (v/v)), 10mug of molybdenum in 5ml aqueous phase could be extracted quantitatively into 40mul of the sedimented phase. The maximum concentration factor was 125-fold. Thiocyanate was applied as a chromogenic reagent for the direct spectrophotometric determination of molybdenum in the sedimented phase. The reproducibility of the proposed method is at the most 2.4%. The influence of the type and concentration of acid solution, the concentration of ABO, the type and volume of the water-miscible organic solvent, the concentration of PFOA(-), and the effect of different diverse ions on the extraction and determination of molybdenum(VI) were investigated. The proposed method was applied to the extraction and determination of molybdenum(VI) in natural water, Spinach, and Lucerne samples. A satisfactory agreement exists between the results obtained by the proposed method and those reported by GF-AAS.

  10. Ultrasonic-Assisted Extraction of Procyanidins Using Ionic Liquid Solution from Larix gmelinii Bark

    OpenAIRE

    Xiaowei Sun; Zhimin Jin; Lei Yang; Jingwei Hao; Yuangang Zu; Wenjie Wang; Wenbin Liu

    2013-01-01

    An ionic liquid-based ultrasonic-assisted extraction method has been developed for the effective extraction of procyanidins from Larix gmelinii bark. So as to evaluate the performance of ionic liquids in ultrasonic-assisted extraction process, the effects caused by changes in the anion and the alkyl chain length of the cation on the extraction efficiency were investigated in this paper. The results indicated that the characteristics of anions had remarkable effects on the extraction efficienc...

  11. Solvent Extraction: Structure of the Liquid-Liquid Interface Containing a Diamide Ligand

    Energy Technology Data Exchange (ETDEWEB)

    Scoppola, Ernesto [Institut Laue-Langevin, 38000 Grenoble France; Institut de Chimie Séparative de Marcoule, UMR 5257 CEA/CNRS/ENSCM/Université Montpellier, 30207 Bagnols-sur-Cèze France; Watkins, Erik B. [Institut Laue-Langevin, 38000 Grenoble France; Materials Synthesis and Integrated Devices, Los Alamos National Laboratory, Los Alamos NM 87545 USA; Campbell, Richard A. [Institut Laue-Langevin, 38000 Grenoble France; Konovalov, Oleg [European Synchrotron Radiation Facility, 38430 Grenoble France; Girard, Luc [Institut de Chimie Séparative de Marcoule, UMR 5257 CEA/CNRS/ENSCM/Université Montpellier, 30207 Bagnols-sur-Cèze France; Dufrêche, Jean-Francois [Institut de Chimie Séparative de Marcoule, UMR 5257 CEA/CNRS/ENSCM/Université Montpellier, 30207 Bagnols-sur-Cèze France; Ferru, Geoffroy [Argonne National Labororatory, Lemont IL 60439 USA; Fragneto, Giovanna [Institut Laue-Langevin, 38000 Grenoble France; Diat, Olivier [Institut de Chimie Séparative de Marcoule, UMR 5257 CEA/CNRS/ENSCM/Université Montpellier, 30207 Bagnols-sur-Cèze France

    2016-06-20

    Knowledge of the (supra)molecular structure of an interface that contains amphiphilic ligand molecules is necessary for a full understanding of ion transfer during solvent extraction. Even if molecular dynamics already yield some insight in the molecular configurations in solution, hardly any experimental data giving access to distributions of both extractant molecules and ions at the liquid–liquid interface exist. Here, the combined application of X-ray and neutron reflectivity measurements represents a key milestone in the deduction of the interfacial structure and potential with respect to two different lipophilic ligands. Indeed, we show for the first time that hard trivalent cations can be repelled or attracted by the extractant-enriched interface according to the nature of the ligand.

  12. Enrichment of antioxidant compounds from lemon balm (Melissa officinalis) by pressurized liquid extraction and enzyme-assisted extraction

    OpenAIRE

    2013-01-01

    In this work enzyme-assisted extraction (EAE) and pressurized liquid extraction (PLE) are applied for extraction of natural compounds from lemon balm (Melissa officinalis). Cellulase, endo-β-1,4 xylanase and pectinase were studied in order to degrade cell wall of lemon balm leaves and to release phenolic compounds. On the other hand, in order to compare the performance obtained with EAE, PLE using water and ethanol was employed maintaining 150°C as extraction temperature. The obtained extract...

  13. Selective Extraction of Organic Contaminants from Soil Using Pressurised Liquid Extraction

    Directory of Open Access Journals (Sweden)

    Rozita Osman

    2013-01-01

    Full Text Available This study focuses on the application of sorbents in pressurised liquid extraction (PLE cell to establish a selective extraction of a variety of organic contaminants (polycyclic aromatic hydrocarbons (PAHs, chlorpyrifos, phenol, pentachlorophenol, and sterols from soil. The selectivity and efficiency of each sorbent depend on the properties of the material, extracting solvent, capacity factor, organic compounds of interest, and PLE operating parameters (temperature, pressure, and extraction time. Several sorbents (silica, alumina, and Florisil were evaluated and with the proper choice of solvents, polar and nonpolar compounds were successfully separated in two fractions. Nonpolar compounds (PAHs, chlorpyrifos, and pentachlorophenol were recovered in the first fraction using a polar sorbent such as Florisil or alumina, and n-hexane as eluting solvent, while more polar compounds (phenol and sterols were recovered in the second fraction using methanol. Silica (5 g was found to be effective for selective extraction with the satisfactory recoveries for all compounds (PAHs from 87.1–96.2%, chlorpyrifos 102.9%, sterols from 93.7–100.5%, phenol 91.9%, and pentachlorophenol 106.2%. The efficiency and precision of this extraction approach and the existing EPA Method 3545 were compared.

  14. Extraction of bioactive carbohydrates from artichoke (Cynara scolymus L.) external bracts using microwave assisted extraction and pressurized liquid extraction.

    Science.gov (United States)

    Ruiz-Aceituno, Laura; García-Sarrió, M Jesús; Alonso-Rodriguez, Belén; Ramos, Lourdes; Sanz, M Luz

    2016-04-01

    Microwave assisted extraction (MAE) and pressurized liquid extraction (PLE) methods using water as solvent have been optimized by means of a Box-Behnken and 3(2) composite experimental designs, respectively, for the effective extraction of bioactive carbohydrates (inositols and inulin) from artichoke (Cynara scolymus L.) external bracts. MAE at 60 °C for 3 min of 0.3 g of sample allowed the extraction of slightly higher concentrations of inositol than PLE at 75 °C for 26.7 min (11.6 mg/g dry sample vs. 7.6 mg/g dry sample). On the contrary, under these conditions, higher concentrations of inulin were extracted with the latter technique (185.4 mg/g vs. 96.4 mg/g dry sample), considering two successive extraction cycles for both techniques. Both methodologies can be considered appropriate for the simultaneous extraction of these bioactive carbohydrates from this particular industrial by-product. To the best of our knowledge this is the first time that these techniques are applied for this purpose.

  15. Kinetic of liquid-liquid extraction for uranyl nitrate and actinides (III) and lanthanides (III) nitrates by amide extractants; Cinetique d`extraction liquide-liquide du nitrate d`uranyle et des nitrates d`actinides (III) et de lanthanides (III) par des extractants a fonction amide

    Energy Technology Data Exchange (ETDEWEB)

    Toulemonde, V. [CEA Centre d`Etudes Nucleaires de Saclay, 91 -Gif-sur-Yvette (France)]|[CEA Centre d`Etudes de la Vallee du Rhone, 30 -Marcoule (France). Dept. d`Exploitation du Retraitement et de Demantelement

    1995-12-20

    The kinetics of liquid-liquid extraction by amide extractants have been investigated for uranyl nitrate (monoamide extractants), actinides (III) and lanthanides (III) nitrates (diamide extractants). The transfer of the metallic species from the aqueous phase to the organic phase was studied using two experimental devices: ARMOLLEX (Argonne Modified Lewis cell for Liquid Liquid Extraction) and RSC (Rotating Stabilized Cell). The main conclusions are: for the extraction of uranyl nitrate by DEHDMBA monoamide, the rate-controlling step is the complexation of the species at the interface of the two liquids. Thus, an absorption-desorption (according to Langmuir theory) reaction mechanism was proposed; for the extraction of actinides (III) and lanthanides (III) nitrates in nitric acid media by DMDBTDMA diamide, the kinetic is also limited by interfacial reactions. The behavior of Americium and Europium is very similar as fare as their reaction kinetics are concerned. (author). 89 refs.

  16. Removal and upgrading of lignocellulosic fermentation inhibitors by in situ biocatalysis and liquid-liquid extraction.

    Science.gov (United States)

    Tomek, Kyle J; Saldarriaga, Carlos Rafael Castillo; Velasquez, Fernando Peregrino Cordoba; Liu, Tongjun; Hodge, David B; Whitehead, Timothy A

    2015-03-01

    Hydroxycinnamic acids are known to inhibit microbial growth during fermentation of lignocellulosic biomass hydrolysates, and the ability to diminish hydroxycinnamic acid toxicity would allow for more effective biological conversion of biomass to fuels and other value-added products. In this work, we provide a proof-of-concept of an in situ approach to remove these fermentation inhibitors through constituent expression of a phenolic acid decarboxylase combined with liquid-liquid extraction of the vinyl phenol products. As a first step, we confirmed using simulated fermentation conditions in two model organisms, Escherichia coli and Saccharomyces cerevisiae, that the product 4-vinyl guaiacol is more inhibitory to growth than ferulic acid. Partition coefficients of ferulic acid, p-coumaric acid, 4-vinyl guaiacol, and 4-ethyl phenol were measured for long-chain primary alcohols and alkanes, and tetradecane was identified as a co-solvent that can preferentially extract vinyl phenols relative to the acid parent and additionally had no effect on microbial growth rates or ethanol yields. Finally, E. coli expressing an active phenolic acid decarboxylase retained near maximum anaerobic growth rates in the presence of ferulic acid if and only if tetradecane was added to the fermentation broth. This work confirms the feasibility of donating catabolic pathways into fermentative microorganisms in order to ameliorate the effects of hydroxycinnamic acids on growth rates, and suggests a general strategy of detoxification by simultaneous biological conversion and extraction. © 2014 Wiley Periodicals, Inc.

  17. Mathematical modelling of Liquid -Liquid extraction in the slug flow regime in a microchannel

    Science.gov (United States)

    Ramji, Sundari; Bhagavatula, Dinesh; Rakesh, Arjun; Pushpavanam, S.

    2016-11-01

    Mixing in the slug flow regime in microchannels is enhanced by the presence of internal circulations induced by shear due to wall. This helps improve mass transfer in this flow regime. We exploit the low Re characteristic of the flow and seek a numerical solution to understand the structure of the vortex patterns formed in the two phases in the slug flow regime. We study liquid-liquid extraction in the system to determine the improvement in mass transfer. The system was analyzed for two cases when there is (i) no film surrounding the slug (ii) a thin film surrounding the slug. The 2D governing equations for fluid flow are solved using two approaches: a) a stream function formulation based on finite differences b) primitive variable formulation with the Chebyshev collocation method. The effect of viscosity ratio, slug length and film thickness on the vortex structure were studied. While secondary vortices were induced in the less viscous phase in the case where the thin film is absent, they are always generated in the slug irrespective of the viscosity ratio in the case where the film is present. The species balance equation was then solved numerically using two approaches: a) an Alternating Direction Explicit method and b) the Locally One Dimensional splitting technique. The effect of varying Peclet number from 0 to 104 on the solute transfer from the slug to the continuous phase was studied. The extraction performance is analyzed in terms of extraction efficiency and mass transfer coefficient.

  18. Use of experimental design in the investigation of stir bar sorptive extraction followed by ultra-high-performance liquid chromatography-tandem mass spectrometry for the analysis of explosives in water samples.

    Science.gov (United States)

    Schramm, Sébastien; Vailhen, Dominique; Bridoux, Maxime Cyril

    2016-02-12

    A method for the sensitive quantification of trace amounts of organic explosives in water samples was developed by using stir bar sorptive extraction (SBSE) followed by liquid desorption and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The proposed method was developed and optimized using a statistical design of experiment approach. Use of experimental designs allowed a complete study of 10 factors and 8 analytes including nitro-aromatics, amino-nitro-aromatics and nitric esters. The liquid desorption study was performed using a full factorial experimental design followed by a kinetic study. Four different variables were tested here: the liquid desorption mode (stirring or sonication), the chemical nature of the stir bar (PDMS or PDMS-PEG), the composition of the liquid desorption phase and finally, the volume of solvent used for the liquid desorption. On the other hand, the SBSE extraction study was performed using a Doehlert design. SBSE extraction conditions such as extraction time profiles, sample volume, modifier addition, and acetic acid addition were examined. After optimization of the experimental parameters, sensitivity was improved by a factor 5-30, depending on the compound studied, due to the enrichment factors reached using the SBSE method. Limits of detection were in the ng/L level for all analytes studied. Reproducibility of the extraction with different stir bars was close to the reproducibility of the analytical method (RSD between 4 and 16%). Extractions in various water sample matrices (spring, mineral and underground water) have shown similar enrichment compared to ultrapure water, revealing very low matrix effects.

  19. Functionalized ionic liquids: new agents for the extraction of actinides/lanthanides

    Energy Technology Data Exchange (ETDEWEB)

    Ouadi, A.; Hesemann, P.; Billard, I.; Gaillard, C.; Gadenne, B.; Moreau, Joel J.E; Moutiers, G.; Mariet, C.; Labet, A

    2004-07-01

    The potentialities of hydrophobic ionic liquids BumimPF{sub 6} and BumimTf{sub 2}N for their use in the nuclear fuel cycle were investigated, in particular for the liquid liquid extraction. We demonstrate that the use of RTILs in replacement of the organic diluents for actinides partitioning is promising. In our contribution, we present the synthesis of several task-specific ionic liquids. Our results show that grafting metal complexing groups increases the affinity of metals to the IL phase and gives rise to suitable media for the liquid-liquid extraction of actinides. (authors)

  20. Kinetic aspects of hollow fiber liquid-phase microextraction and electromembrane extraction

    DEFF Research Database (Denmark)

    Gjelstad, Astrid; Jensen, Henrik; Rasmussen, Knut Einar

    2012-01-01

    In this paper, extraction kinetics was investigated experimentally and theoretically in hollow fiber liquid-phase microextraction (HF-LPME) and electromembrane extraction (EME) with the basic drugs droperidol, haloperidol, nortriptyline, clomipramine, and clemastine as model analytes. In HF...

  1. Non-aqueous phase liquid spreading during soil vapor extraction

    Science.gov (United States)

    Kneafsey, Timothy J.; Hunt, James R.

    2004-02-01

    Many non-aqueous phase liquids (NAPLs) are expected to spread at the air-water interface, particularly under non-equilibrium conditions. In the vadose zone, this spreading should increase the surface area for mass transfer and the efficiency of volatile NAPL recovery by soil vapor extraction (SVE). Observations of spreading on water wet surfaces led to a conceptual model of oil spreading vertically above a NAPL pool in the vadose zone. Analysis of this model predicts that spreading can enhance the SVE contaminant recovery compared to conditions where the liquid does not spread. Experiments were conducted with spreading volatile oils hexane and heptane in wet porous media and capillary tubes, where spreading was observed at the scale of centimeters. Within porous medium columns up to a meter in height containing stagnant gas, spreading was less than ten centimeters and did not contribute significantly to hexane volatilization. Water film thinning and oil film pinning may have prevented significant oil film spreading, and thus did not enhance SVE at the scale of a meter. The experiments performed indicate that volatile oil spreading at the field scale is unlikely to contribute significantly to the efficiency of SVE.

  2. Selective extraction of copper, mercury, silver and palladium ionsfrom water using hydrophobic ionic liquids.

    Energy Technology Data Exchange (ETDEWEB)

    Papaiconomou, Nicolas; Lee, Jong-Min; Salminen, Justin; VonStosch, Moritz; Prausnitz, John M.

    2007-06-25

    Extraction of dilute metal ions from water was performed near room temperature with a variety of ionic liquids. Distribution coefficients are reported for fourteen metal ions extracted with ionic liquids containing cations 1-octyl-4-methylpyridinium [4MOPYR]{sup +}, 1-methyl-1-octylpyrrolidinium [MOPYRRO]{sup +} or 1-methyl-1-octylpiperidinium [MOPIP]{sup +}, and anions tetrafluoroborate [BF{sub 4}]{sup +}, trifluoromethyl sulfonate [TfO]{sup +} or nonafluorobutyl sulfonate [NfO]{sup +}. Ionic liquids containing octylpyridinium cations are very good for extracting mercury ions. However, other metal ions were not significantly extracted by any of these ionic liquids. Extractions were also performed with four new task-specific ionic liquids. Such liquids containing a disulfide functional group are efficient and selective for mercury and copper, whereas those containing a nitrile functional group are efficient and selective for silver and palladium.

  3. Selective extraction and separation of oxymatrine from Sophora flavescens Ait. extract by silica-confined ionic liquid.

    Science.gov (United States)

    Bi, Wentao; Tian, Minglei; Row, Kyung Ho

    2012-01-01

    This study highlighted the application of a two-stepped extraction method for extraction and separation of oxymatrine from Sophora flavescens Ait. extract by utilizing silica-confined ionic liquids as sorbent. The optimized silica-confined ionic liquid was firstly mixed with plant extract to adsorb oxymatrine. Simultaneously, some interference, such as matrine, was removed. The obtained suspension was then added to a cartridge for solid phase extraction. Through these two steps, target compound was adequately separated from interferences with 93.4% recovery. In comparison with traditional solid phase extraction, this method accelerates loading and reduces the use of organic solvents during washing. Moreover, the optimization of loading volume was simplified as optimization of solid/liquid ratio.

  4. Ionic liquids and deep eutectic solvents in natural products research: mixtures of solids as extraction solvents.

    Science.gov (United States)

    Dai, Yuntao; van Spronsen, Jaap; Witkamp, Geert-Jan; Verpoorte, Robert; Choi, Young Hae

    2013-11-22

    Mixtures of solid chemicals may become liquid under certain conditions. These liquids are characterized by the formation of strong ionic (ionic liquids) or hydrogen bonds (deep eutectic solvents). Due to their extremely low vapor pressure, they are now widely used in polymer chemistry and synthetic organic chemistry, yet little attention has been paid to their use as extraction solvents of natural products. This review summarizes the preparation of ionic liquids and deep eutectic solvents with natural product components and recent progress in their applications to the extraction and analysis of natural products as well as the recovery of extracted compounds from their extracts. Additionally, various factors affecting extraction features of ionic liquids and deep eutectic solvents, as well as potential useful technologies including microwave and ultrasound to increase the extraction efficiency, are discussed.

  5. Predictive model for ionic liquid extraction solvents for rare earth elements

    Science.gov (United States)

    Grabda, Mariusz; Oleszek, Sylwia; Panigrahi, Mrutyunjay; Kozak, Dmytro; Eckert, Franck; Shibata, Etsuro; Nakamura, Takashi

    2015-12-01

    The purpose of our study was to select the most effective ionic liquid extraction solvents for dysprosium (III) fluoride using a theoretical approach. Conductor-like Screening Model for Real Solvents (COSMO-RS), based on quantum chemistry and the statistical thermodynamics of predefined DyF3-ionic liquid systems, was applied to reach the target. Chemical potentials of the salt were predicted in 4,400 different ionic liquids. On the base of these predictions set of ionic liquids' ions, manifesting significant decrease of the chemical potentials, were selected. Considering the calculated physicochemical properties (hydrophobicity, viscosity) of the ionic liquids containing these specific ions, the most effective extraction solvents for liquid-liquid extraction of DyF3 were proposed. The obtained results indicate that the COSMO-RS approach can be applied to quickly screen the affinity of any rare earth element for a large number of ionic liquid systems, before extensive experimental tests.

  6. Fluorous ionic liquids as solvents for the liquid-liquid extraction of metal ions by macrocyclic polyethers.

    Science.gov (United States)

    Heitzman, Holly; Young, Blake A; Rausch, David J; Rickert, Paul; Stepinski, Dominique C; Dietz, Mark L

    2006-04-15

    The predominant mode of strontium ion transfer from aqueous nitrate media into a series of 1-fluoroalkyl-3-methylimidazolium bis[(trifluoromethylsulfonyl)]imides containing dicyclohexano-18-crown-6 (DCH18C6) is shown to shift from cation exchange to strontium nitrato-crown ether complex partitioning as the length of the fluoroalkyl substituent is increased. Fluoroalkyl substituents are shown to be only slightly more effective than their non-fluorous analogs at inducing this shift. At the same time, the fluorinated ionic liquids (ILs) yield strontium distribution ratios as much as an order of magnitude lower than the corresponding 1-alkyl-3-methylimidazolium (C(n)mim(+)) salts. Fluorous ILs thus appear to offer no compelling advantages over C(n)mim(+) ionic liquids as extraction solvents.

  7. Ionic-liquid-impregnated resin for the microwave-assisted solid-liquid extraction of triazine herbicides in honey.

    Science.gov (United States)

    Wu, Lijie; Song, Ying; Hu, Mingzhu; Yu, Cui; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

    2015-09-01

    Microwave-assisted ionic-liquid-impregnated resin solid-liquid extraction was developed for the extraction of triazine herbicides, including cyanazine, metribuzin, desmetryn, secbumeton, terbumeton, terbuthylazine, dimethametryn, and dipropetryn in honey samples. The ionic-liquid-impregnated resin was prepared by immobilizing 1-hexyl-3-methylimidazolium hexafluorophosphate in the microspores of resin. The resin was used as the extraction adsorbent. The extraction and enrichment of analytes were performed in a single step. The extraction time can be shortened greatly with the help of microwave. The effects of experimental parameters including type of resin, type of ionic liquid, mass ratio of resin to ionic liquid, extraction time, amount of the impregnated resin, extraction temperature, salt concentration, and desorption conditions on the extraction efficiency, were investigated. A Box-Behnken design was applied to the selection of the experimental parameters. The recoveries were in the range of 80.1 to 103.4% and the relative standard deviations were lower than 6.8%. The present method was applied to the analysis of honey samples.

  8. Liquid-liquid extraction assisted by a carbon nanoparticles interface. Electrophoretic determination of atrazine in environmental samples.

    Science.gov (United States)

    Caballero-Díaz, Encarnación; Simonet, Bartolomé; Valcárcel, Miguel

    2013-10-21

    A novel method for the determination of atrazine, using liquid-liquid extraction assisted by a nanoparticles film formed in situ and composed of organic solvent stabilized-carbon nanoparticles, is described. The presence of nanoparticles located at the liquid-liquid interface reinforced the extraction of analyte from matrix prior to capillary electrophoresis (CE) analysis. Some influential experimental variables were optimized in order to enhance the extraction efficiency. The developed procedure confirmed that carbon nanoparticles, especially multi-walled carbon nanotubes, are suitable to be used in sample treatment processes introducing new mechanisms of interaction with the analyte. The application of the proposed preconcentration method followed by CE detection enabled the determination of atrazine in spiked river water providing acceptable RSD values (11.6%) and good recoveries (about 87.0-92.0%). Additionally, a similar extraction scheme was tested in soil matrices with a view to further applications in real soil samples.

  9. Enhancing extraction ability by rational design of phosphoryl functionalized ionic liquids and mechanistic investigation on neodymium (III) extraction

    Institute of Scientific and Technical Information of China (English)

    王君平; 赵洁莹; 冯达; 康鑫淳; 孙云雨; 赵玲玲; 梁洪泽

    2016-01-01

    Four ionic liquids (ILs): 3-(diethoxyphosphoryl)propyl triphenylphosphinium hexafluorophosphate [Ph3PC3P(OEt)2][PF6] (IL-1), 3-(ethoxyphenylphosphoryl)propyl triphenylphosphinium hexafluorophosphate [Ph3PC3PPh(OEt)][PF6] (IL-2), 3-(diphenyl-phosphoryl)propyl triphenylphosphinium hexafluorophosphate [Ph3PC3P(Ph)2][PF6] (IL-3), and 3-(diethoxyphosphoryl)propyl triphenylphosphinium bis(trifluoromethanesulfonyl)imide [Ph3PC3P(OEt)2][NTf2] (IL-4) were synthesized and characterized by IR and31P,1H,13C NMR spectroscopy. The liquid-liquid extraction of neodymium(III) by these phosphorus functionalized ionic liquids (PFILs) diluted with common room temperature ionic liquid 1-hexyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide [C6mim][NTf2] was studied. The extraction percentage of Nd(III) was measured as a function of various parameters, such as the ini-tial pH of aqueous phase, equilibrium time, temperature, and concentration of PFIL extractant. The influence of the nature of diluents and salting-out reagents on extraction was also investigated. The results indicated that the extraction process was exothermical and the extraction percentage of Nd(III) by IL-1 was the highest among the PFILs investigated. A possible metal complexation mechanism was proposed for the present PFIL/IL extraction system. And the loaded Nd(III) ions by PFIL could be stripped completely from the ionic liquid phase by 1 mol/L nitric acid.

  10. Simultaneous Distillation Extraction of Some Volatile Flavor Components from Pu-erh Tea Samples—Comparison with Steam Distillation-Liquid/Liquid Extraction and Soxhlet Extraction

    Science.gov (United States)

    Gu, Xungang; Zhang, Zhengzhu; Wan, Xiaochun; Ning, Jingming; Yao, Chengcheng; Shao, Wanfang

    2009-01-01

    A simutaneous distillation extraction (SDE) combined GC method was constructed for determination of volatile flavor components in Pu-erh tea samples. Dichloromethane and ethyl decylate was employed as organic phase in SDE and internal standard in determination, respectively. Weakly polar DB-5 column was used to separate the volatile flavor components in GC, 10 of the components were quantitatively analyzed, and further confirmed by GC-MS. The recovery covered from 66.4%–109%, and repeatability expressed as RSD was in range of 1.44%–12.6%. SDE was most suitable for the extraction of the anlytes by comparing with steam distillation-liquid/liquid extraction and Soxhlet extraction. Commercially available Pu-erh tea samples, including Pu-erh raw tea and ripe tea, were analyzed by the constructed method. the high-volatile components, such as benzyl alcohol, linalool oxide, and linalool, were greatly rich in Pu-erh raw teas, while the contents of 1,2,3-Trimethoxylbenzene and 1,2,4-Trimethoxylbenzene were much high in Pu-erh ripe teas. PMID:20169174

  11. Development of a new extraction method based on counter current salting-out homogenous liquid-liquid extraction followed by dispersive liquid-liquid microextraction: Application for the extraction and preconcentration of widely used pesticides from fruit juices.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Feriduni, Behruz; Mogaddam, Mohammad Reza Afshar

    2016-01-01

    In this paper, a new extraction method based on counter current salting-out homogenous liquid-liquid extraction (CCSHLLE) followed by dispersive liquid-liquid microextraction (DLLME) has been developed for the extraction and preconcentration of widely used pesticides in fruit juice samples prior to their analysis by gas chromatography-flame ionization detection (GC-FID). In this method, initially, sodium chloride as a separation reagent is filled into a small column and a mixture of water (or fruit juice) and acetonitrile is passed through the column. By passing the mixture sodium chloride is dissolved and the fine droplets of acetonitrile are formed due to salting-out effect. The produced droplets go up through the remained mixture and collect as a separated layer. Then, the collected organic phase (acetonitrile) is removed with a syringe and mixed with 1,1,2,2-tetrachloroethane (extraction solvent at µL level). In the second step, for further enrichment of the analytes the above mixture is injected into 5 mL de-ionized water placed in a test tube with conical bottom in order to dissolve acetonitrile into water and to achieve a sedimented phase at µL-level volume containing the enriched analytes. Under the optimal extraction conditions (extraction solvent, 1.5 mL acetonitrile; pH, 7; flow rate, 0.5 mL min(-1); preconcentration solvent, 20 µL 1,1,2,2-tetrachloroethane; NaCl concentration; 5%, w/w; and centrifugation rate and time, 5000 rpm and 5 min, respectively), the extraction recoveries and enrichment factors ranged from 87% to 96% and 544 to 600, respectively. Repeatability of the proposed method, expressed as relative standard deviations, ranged from 2% to 6% for intra-day (n=6, C=250 or 500 µg L(-1)) and inter-days (n=4, C=250 or 500 µg L(-1)) precisions. Limits of detection are obtained between 2 and 12 µg L(-1). Finally, the proposed method is applied for the determination of the target pesticide residues in the juice samples.

  12. Scalable enantioseparation of amino acid derivatives using continuous liquid-liquid extraction in a cascade of centrifugal contactor separators

    NARCIS (Netherlands)

    Schuur, Boelo; Hallett, Andrew J.; Winkelman, Jozef G.M.; Vries, Johannes G. de; Heeres, Hero J.

    2009-01-01

    Using a cascade of six centrifugal contactor separators in a countercurrent liquid-liquid extraction mode allowed the separation of one of the enantiomers of 3,5-dinitrobenzoyl-leucine in 55% yield and 98% ee using a catalytic amount of a chiral host compound based on a cinchona alkaloid, This metho

  13. Ultrapreconcentration and determination of organophosphorus pesticides in water by solid-phase extraction combined with dispersive liquid-liquid microextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Chen, Junhua; Zhou, Guangming; Deng, Yongli; Cheng, Hongmei; Shen, Jie; Gao, Yi; Peng, Guilong

    2016-01-01

    Solid-phase extraction coupled with dispersive liquid-liquid microextraction was developed as an ultra-preconcentration method for the determination of four organophosphorus pesticides (isocarbophos, parathion-methyl, triazophos and fenitrothion) in water samples. The analytes considered in this study were rapidly extracted and concentrated from large volumes of aqueous solutions (100 mL) by solid-phase extraction coupled with dispersive liquid-liquid microextraction and then analyzed using high performance liquid chromatography. Experimental variables including type and volume of elution solvent, volume and flow rate of sample solution, salt concentration, type and volume of extraction solvent and sample solution pH were investigated for the solid-phase extraction coupled with dispersive liquid-liquid microextraction with these analytes, and the best results were obtained using methanol as eluent and ethylene chloride as extraction solvent. Under the optimal conditions, an exhaustive extraction for four analytes (recoveries >86.9%) and high enrichment factors were attained. The limits of detection were between 0.021 and 0.15 μg/L. The relative standard deviations for 0.5 μg/L of the pesticides in water were in the range of 1.9-6.8% (n = 5). The proposed strategy offered the advantages of simple operation, high enrichment factor and sensitivity and was successfully applied to the determination of four organophosphorus pesticides in water samples.

  14. Macrocyclic polyamine-functionalized silica as a solid-phase extraction material coupled with ionic liquid dispersive liquid-liquid extraction for the enrichment of polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Liu, Longhui; He, Lijun; Jiang, Xiuming; Zhao, Wenjie; Xiang, Guoqiang; Anderson, Jared L

    2014-04-01

    In this study, silica modified with a 30-membered macrocyclic polyamine was synthesized and first used as an adsorbent material in SPE. The SPE was further combined with ionic liquid (IL) dispersive liquid-liquid microextraction (DLLME). Five polycyclic aromatic hydrocarbons were employed as model analytes to evaluate the extraction procedure and were determined by HPLC combined with UV/Vis detection. Acetone was used as the elution solvent in SPE as well as the dispersive solvent in DLLME. The enrichment of analytes was achieved using the 1,3-dibutylimidazolium bis[(trifluoromethyl)sulfonyl]imide IL/acetone/water system. Experimental conditions for the overall macrocycle-SPE-IL-DLLME method, such as the amount of adsorbent, sample solution volume, sample solution pH, type of elution solvent as well as addition of salt, were studied and optimized. The developed method could be successfully applied to the analysis of four real water samples. The macrocyclic polyamine offered higher extraction efficiency for analytes compared with commercially available C18 cartridge, and the developed method provided higher enrichment factors (2768-5409) for model analytes compared with the single DLLME. Good linearity with the correlation coefficients ranging from 0.9983 to 0.9999 and LODs as low as 0.002 μg/L were obtained in the proposed method.

  15. Determination of diflubenzuron and chlorbenzuron in fruits by combining acetonitrile-based extraction with dispersive liquid-liquid microextraction followed by high-performance liquid chromatography.

    Science.gov (United States)

    Ruan, Chunqiang; Zhao, Xiang; Liu, Chenglan

    2015-09-01

    In this study, a simple and low-organic-solvent-consuming method combining an acetonitrile-partitioning extraction procedure followed by "quick, easy, cheap, effective, rugged and safe" cleanup with ionic-liquid-based dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic-liquid-based dispersive liquid-liquid microextraction was performed using the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid-liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples.

  16. Use of liquid/supercritical CO2 extraction process for butanol recovery from fermentation broth

    Science.gov (United States)

    In order for butanol fermentation to be a viable option, it is essential to recover it from fermentation broth using economical alternate in-situ product recovery techniques such as liquid/supercritical CO2 extraction as compared to distillation. This technique (liquid CO2 extraction & supercritical...

  17. Determination of Roxarsone in feeds using solid phase extraction and liquid chromatography with ultraviolet detection.

    Science.gov (United States)

    Sapp, R E; Davidson, S

    1993-01-01

    A method is presented for detection and quantitation of Roxarsone in poultry feed by liquid chromatography. The drug is extracted by phosphate buffer and determined by solid phase extraction and reversed-phase liquid chromatography. Recoveries of the sample spikes and fortified field samples agree closely with those obtained by the standard spectrophotometric method.

  18. Ionic liquid pre-treatment of microalgae and extraction of biomolecules

    NARCIS (Netherlands)

    Desai, Rupali K.

    2016-01-01

    Liquid-liquid extraction (LLE) techniques are widely used in separation primarily due to ease of scale up. Conventional (LLE) systems based on organic solvents are not suitable for extraction of fragile molecules such as proteins as it would result in denaturation. On the other hand aqueous biphasic

  19. Quantification of four ionophores in soil, sediment and manure using pressurised liquid extraction

    DEFF Research Database (Denmark)

    Bak, Søren Alex; Hansen, Martin; Pedersen, Kenneth Munk

    2013-01-01

    A multi-residue pressurised liquid extraction (PLE) methodology has been established for the determination of the four ionophores: lasalocid, monensin, salinomycin and narasin in solid environmental matrices. The PLE methodology is combined with solid phase extraction as clean-up using liquid...

  20. Application of ionic liquids based enzyme-assisted extraction of chlorogenic acid from Eucommia ulmoides leaves

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Tingting; Sui, Xiaoyu, E-mail: suixiaoyu@outlook.com; Li, Li; Zhang, Jie; Liang, Xin; Li, Wenjing; Zhang, Honglian; Fu, Shuang

    2016-01-15

    A new approach for ionic liquid based enzyme-assisted extraction (ILEAE) of chlorogenic acid (CGA) from Eucommia ulmoides is presented in which enzyme pretreatment was used in ionic liquids aqueous media to enhance extraction yield. For this purpose, the solubility of CGA and the activity of cellulase were investigated in eight 1-alkyl-3-methylimidazolium ionic liquids. Cellulase in 0.5 M [C6mim]Br aqueous solution was found to provide better performance in extraction. The factors of ILEAE procedures including extraction time, extraction phase pH, extraction temperatures and enzyme concentrations were investigated. Moreover, the novel developed approach offered advantages in term of yield and efficiency compared with other conventional extraction techniques. Scanning electronic microscopy of plant samples indicated that cellulase treated cell wall in ionic liquid solution was subjected to extract, which led to more efficient extraction by reducing mass transfer barrier. The proposed ILEAE method would develope a continuous process for enzyme-assisted extraction including enzyme incubation and solvent extraction process. In this research, we propose a novel view for enzyme-assisted extraction of plant active component, besides concentrating on enzyme facilitated cell wall degradation, focusing on improvement of bad permeability of ionic liquids solutions. - Highlights: • An ionic liquid based enzyme-assisted extraction method of natural product was explored. • ILEAE utilizes enzymatic treatment to improve permeability of ionic liquids solution. • Enzyme incubation and solvent extraction process were ongoing simultaneously. • ILEAE process simplified operating process and suitable for more complete extraction.

  1. Application of ionic liquids based enzyme-assisted extraction of chlorogenic acid from Eucommia ulmoides leaves.

    Science.gov (United States)

    Liu, Tingting; Sui, Xiaoyu; Li, Li; Zhang, Jie; Liang, Xin; Li, Wenjing; Zhang, Honglian; Fu, Shuang

    2016-01-15

    A new approach for ionic liquid based enzyme-assisted extraction (ILEAE) of chlorogenic acid (CGA) from Eucommia ulmoides is presented in which enzyme pretreatment was used in ionic liquids aqueous media to enhance extraction yield. For this purpose, the solubility of CGA and the activity of cellulase were investigated in eight 1-alkyl-3-methylimidazolium ionic liquids. Cellulase in 0.5 M [C6mim]Br aqueous solution was found to provide better performance in extraction. The factors of ILEAE procedures including extraction time, extraction phase pH, extraction temperatures and enzyme concentrations were investigated. Moreover, the novel developed approach offered advantages in term of yield and efficiency compared with other conventional extraction techniques. Scanning electronic microscopy of plant samples indicated that cellulase treated cell wall in ionic liquid solution was subjected to extract, which led to more efficient extraction by reducing mass transfer barrier. The proposed ILEAE method would develope a continuous process for enzyme-assisted extraction including enzyme incubation and solvent extraction process. In this research, we propose a novel view for enzyme-assisted extraction of plant active component, besides concentrating on enzyme facilitated cell wall degradation, focusing on improvement of bad permeability of ionic liquids solutions.

  2. Predictive model for ionic liquid extraction solvents for rare earth elements

    Energy Technology Data Exchange (ETDEWEB)

    Grabda, Mariusz; Oleszek, Sylwia [Institute of Multidisciplinary Research for Advanced Materials (IMRAM), Tohoku University, 2,1-Katahira, 2-Chome, 980-8577 Sendai (Japan); Institute of Environmental Engineering of the Polish Academy of Sciences, ul. M. Sklodowskiej-Curie 34, 41-819, Zabrze (Poland); Panigrahi, Mrutyunjay; Kozak, Dmytro; Shibata, Etsuro; Nakamura, Takashi [Institute of Multidisciplinary Research for Advanced Materials (IMRAM), Tohoku University, 2,1-Katahira, 2-Chome, 980-8577 Sendai (Japan); Eckert, Franck [COSMOlogic GmbH & Co KG, Imbacher Weg 46, 50379 Leverkusen (Germany)

    2015-12-31

    The purpose of our study was to select the most effective ionic liquid extraction solvents for dysprosium (III) fluoride using a theoretical approach. Conductor-like Screening Model for Real Solvents (COSMO-RS), based on quantum chemistry and the statistical thermodynamics of predefined DyF{sub 3}-ionic liquid systems, was applied to reach the target. Chemical potentials of the salt were predicted in 4,400 different ionic liquids. On the base of these predictions set of ionic liquids’ ions, manifesting significant decrease of the chemical potentials, were selected. Considering the calculated physicochemical properties (hydrophobicity, viscosity) of the ionic liquids containing these specific ions, the most effective extraction solvents for liquid-liquid extraction of DyF{sub 3} were proposed. The obtained results indicate that the COSMO-RS approach can be applied to quickly screen the affinity of any rare earth element for a large number of ionic liquid systems, before extensive experimental tests.

  3. Application of ionic liquids in the microwave-assisted extraction of proanthocyanidins from Larix gmelini bark.

    Science.gov (United States)

    Yang, Lei; Sun, Xiaowei; Yang, Fengjian; Zhao, Chunjian; Zhang, Lin; Zu, Yuangang

    2012-01-01

    Ionic liquid based, microwave-assisted extraction (ILMAE) was successfully applied to the extraction of proanthocyanidins from Larix gmelini bark. In this work, in order to evaluate the performance of ionic liquids in the microwave-assisted extraction process, a series of 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were evaluated for extraction yield, and 1-butyl-3-methylimidazolium bromide was selected as the optimal solvent. In addition, the ILMAE procedure for the proanthocyanidins was optimized and compared with other conventional extraction techniques. Under the optimized conditions, satisfactory extraction yield of the proanthocyanidins was obtained. Relative to other methods, the proposed approach provided higher extraction yield and lower energy consumption. The Larix gmelini bark samples before and after extraction were analyzed by Thermal gravimetric analysis, Fourier-transform infrared spectroscopy and characterized by scanning electron microscopy. The results showed that the ILMAE method is a simple and efficient technique for sample preparation.

  4. Supported Liquid Membrane Extraction Technology and Its Application in Detection of Meat Security

    Institute of Scientific and Technical Information of China (English)

    LIU Jia; LI Weijin

    2010-01-01

    As a novel technology, supported liquid membrane extraction has gradually become the direction of the research of extraction, for the advantages of using little organic solvents, good selectivity and repeatability. This paper is based on describing the working principle, structure and influencing factors of supported liquid membrane, and research in domestic and foreign literatures which are in the same period, and give a review on the application of supported liquid membrane in meat security determination.

  5. [Determination of 23 antibiotics and 3 β-agonists in livestock drinking water by ultra performance liquid chromatography-tandem mass spectrometry coupled with solid-phase extraction].

    Science.gov (United States)

    Shi, Ao

    2016-02-01

    A method has been developed for the simultaneous determination of 23 antibiotics (four categories) and 3 β-agonists in livestock drinking water using solid-phase extraction and ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI MS/MS). The samples were adjusted pH to 5. 0, added Na2EDTA, enriched and cleaned-up by an HLB solid-phase extraction cartridge. The target compounds were confirmed and quantified by UPLC-ESI MS/MS with external standard method for the anti- biotics and internal standard method for the β-agonists. The recoveries were assessed by using lab tap water as matrix. The average recoveries of the 23 antibiotics and the 3 β-agonists were in the range of 50. 7%-104. 6% and the relative standard deviations (RSDs) were 2. 6%-8. 8% (n= 3). Under the optimal conditions, the calibration curves of the 23 antibiotics and the 3 β-agonists showed good linearity with the correlation coefficients better than 0. 994. The limits of detection (LODs, S/N≥3) ranged from 0. 01-0. 20 ng/L. The developed method was applied to analyze the livestock drinking waters in 36 Beijing intensive livestock farms. The results showed that some antibiotics were detected.

  6. On-line anion exchange solid-phase extraction coupled to liquid chromatography with fluorescence detection to determine quinolones in water and human urine.

    Science.gov (United States)

    Lara, Francisco J; Del Olmo-Iruela, Monsalud; García-Campaña, Ana M

    2013-10-04

    An analytical method based on on-line solid-phase extraction coupled to liquid chromatography with fluorescence detection has been developed to determine quinolones in tap water and human urine. A home-made setup was used to percolate 10 mL of sample through a solid-phase extraction column. Analytes were retained onto the sorbent by an anion exchange mechanism which ensures an optimum compatibility with the subsequent chromatographic separation. A C-18 column containing core-shell particles (2.6 μm) was used to achieve peak efficiencies up to 200,000 plates/m, at a flow rate of 1.2 mL/min and without the need for special pumps. The method allowed the determination of 11 quinolones directly in tap water samples in less than 20 min and with limits of detection ranging between 7 and 110 ng/L. The sensitivity achieved made possible the direct determination of 9 quinolones in human urine without any sample treatment, just dilution with water. Relative recoveries between 94 and 109% were obtained meaning that the matrix effect in human urine is negligible after dilution. Satisfactory results were also obtained in terms of precision since relative standard deviations were always below 13%.

  7. Combination of counter current salting-out homogenous liquid-liquid extraction and dispersive liquid-liquid microextraction as a novel microextraction of drugs in urine samples.

    Science.gov (United States)

    Akramipour, Reza; Fattahi, Nazir; Pirsaheb, Meghdad; Gheini, Simin

    2016-02-15

    The counter current salting-out homogenous liquid-liquid extraction (CCSHLLE) joined with the dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) has been developed as a high preconcentration technique for the determination of different drugs in urine samples. Amphetamines were employed as model compounds to assess the extraction procedure and were determined by high performance liquid chromatography-ultraviolet detection (HPLC-UV). In this method, initially, NaCl as a separation reagent is filled into a small column and a mixture of urine and acetonitrile is passed through the column. By passing the mixture, NaCl is dissolved and the fine droplets of acetonitrile are formed due to salting-out effect. The produced droplets go up through the remained mixture and collect as a separated layer. Then, the collected acetonitrile is removed with a syringe and mixed with 30.0μL 1-undecanol (extraction solvent). In the second step, the 5.00mLK2CO3 solution (2% w/v) is rapidly injected into the above mixture placed in a test tube for further DLLME-SFO. Under the optimum conditions, calibration curves are linear in the range of 1-3000μgL(-1) and limit of detections (LODs) are in the range of 0.5-2μgL(-1). The extraction recoveries and enrichment factors ranged from 78 to 84% and 157 to 168, respectively. Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 100μgL(-1) of amphetamines were in the range of 3.5-4.5% and 4-5%, respectively. The method was successfully applied for the determination of amphetamines in the actual urine samples. The relative recoveries of urine samples spiked with amphetamine and methamphetamine are 90-108%.

  8. Determination of Zinc Ions in Environmental Samples by Dispersive Liquid- Liquid Micro Extraction and Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    F. Arabi

    2012-11-01

    Full Text Available In this work preconcentration of the Zn ions was investigated in water sample by Dispersive liquid- liquid micro extraction (DLLME using chloroform as an extraction solvent, methanol as a disperser solvent and 8-Hydroxyquinoline as a chelating agent. The determination of extracted ions was done by graphite furnace atomic absorption spectrometry. The influence of various analytical parameters including pH, extraction and disperser solvent type and volume and concentration of the chelating agent on the extraction efficiency of analyses was investigated. After extraction, the enrichment factor was 26 and the detection limit of the method was 0.0033 µg l-1 and the relative standard deviations (R.S.D for five determinations of 1 ng/ml Zn were 7.41%. 

  9. Study of 3-Ethylamino-but-2-enoic acid phenylamide as a new ligand for preconcentration of lanthanides from aqueous media by liquid-liquid extraction prior to ICP-MS analysis.

    Science.gov (United States)

    Varbanova, Evelina K; Angelov, Plamen A; Stefanova, Violeta M

    2016-11-01

    In the present work the potential of a new ligand 3-Ethylamino-but-2-enoic acid phenylamide (representing the class of enaminones) for selective preconcentration of lanthanides (La, Ce, Eu, Gd and Er) from aqueous medium is examined. Liquid-liquid extraction parameters, such as pH of the water phase, type and volume of organic solvent, quantity of ligand and reaction time are optimized on model solutions. Recovery of lanthanides by re-extraction with nitric acid makes the LLE procedure compatible with Inductively Coupled Plasma Mass Spectrometry. Spectral and non-spectral interferences are studied. Two isotopes per element are measured (with exception of La) for dynamic evaluation of the potential risk of spectral interference in variable real samples. The selectivity of complex formation reaction towards concomitant alkali and alkali-earth elements eliminates the interferences from sample matrix. Subjecting the standards to the optimized extraction procedure in combination with Re as internal standard is recommended as calibration strategy. The accuracy of developed method is approved by analysis of CRM Bush branches and leaves (NCS DC 73348) and recovery of spiked water and plant samples. The method's limits of detection for both studied objects are in the ranges from 0.2 ((158)Gd) to 3.7 ((139)La) ngl(-1) and 0.02 ((158)Gd) to 0.37((139)La) ngg(-1) for waters and plants respectively. The studied compound is an effective new ligand for preconcentration/separation of lanthanides from aqueous medium by LLE and subsequent determination by ICP-MS. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Functionalized ionic liquids. New agents for the extraction of actinides/lanthandies

    Energy Technology Data Exchange (ETDEWEB)

    Ouadi, A.; Billard, I.; Gaillard, C. [CNRS/IN2P3 and Univ. L. Pasteur, Strasbourg (France). Inst. de Recherches Subatomiques; Hesemann, P.; Gadenne, B.; Moreau, J. [CNRS UMR 5076, Heterochimie Moleculaire et Macromoleculaire, Lab. de Chimie Organometallique, Montpellier (France); Moutiers, G.; Mariet, C.; Labet, A.; Mekki, S. [CEA-Institut National des Sciences et Techniques Nucleaires (INSTN), Centre d' Etudes Nucleaires de Saclay, 91 - Gif-sur-Yvette (France). UECCC

    2004-07-01

    Room-temperature ionic liquids (RTILs) are promising solvent alternatives in organic synthesis, catalysis, electrochemistry and separation processes. They appear as interesting media for the elaboration of separation processes in the nuclear fuel cycle. However, the partitioning of metallic species in liquid-liquid extraction is largely limited by the low complexation properties of the hydrophobia ionic liquids: in general, hydrophobic RTILs are non-coordinating, and the highly hydrated metal ions remain in the aqueous phase. (orig.)

  11. The removal of dinitrochlorobenzene from industrial residuals by liquid-liquid extraction with chemical reaction

    Directory of Open Access Journals (Sweden)

    G. C. M. Ferreira

    2007-09-01

    Full Text Available Nitrochlorobenzenes (NCBs are very important in the chemical industry since they have been used as raw material for the manufacture of crop protection products, as active ingredients in the pharmaceutical industry, as pigments and as antioxidants as well as for other uses. In industrial processes, NCBs are produced by monochlorobenzene (MCB nitration reactions and one of the main residuals formed is dinitrochlorobenzene (DNCB, which is mainly composed of the isomer 2,4DNCB. This subproduct, although of commercial interest when in its pure state, is generally incinerated due to the high costs of recovery treatment and purification. The objective of this study is to present an alternative to the treatment of industrial residuals containing DNCB. The technique consists of converting DNCB into sodium dinitrophenolate, which is very soluble in water and is also easy to reuse. For this purpose, liquid-liquid extraction with chemical reaction (alkaline hydrolysis with a rotating disc contactor (RDC is used. Experimental data on MCB nitration reactions as well as alkaline hydrolysis using a rotating disc contactor are presented.

  12. Electromembrane extraction of peptides - fundamental studies on the supported liquid membrane

    DEFF Research Database (Denmark)

    Seip, Knut Fredrik; Stigsson, Jeanette; Gjelstad, Astrid;

    2011-01-01

    A large screening of different components in the supported liquid membrane (SLM) in electromembrane extraction (EME) was performed to test the extraction efficiency on eight model peptides. Electromembrane extraction from a 500 µL acidified aqueous sample containing the model peptides in the conc...

  13. Extraction of ranitidine and nizatidine with using imidazolium ionic liquids prior spectrophotometric and chromatographic detection.

    Science.gov (United States)

    Kiszkiel, Ilona; Starczewska, Barbara; Leśniewska, Barbara; Późniak, Patrycja

    2015-03-15

    A new extraction medium was proposed for liquid-liquid extraction of the histamine H2 receptor antagonists ranitidine (RNT) and nizatidine (NZT). The ionic liquids with low vapor pressure and favorable solvating properties for a range of compounds such as 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6] and 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide [C4mim][Tf2N] were tested for isolation of analytes. The extraction parameters of RNT and NZT, namely, amount of ionic liquid, pH of sample solution, shaking and centrifugation time were optimized. The isolation processes were performed with 1 mL of the ionic liquids. The extracted samples (pH values near 4) were shaken at 1750 rpm. The influence of interfering substances on the efficiency of extraction process was also studied. Methods for the histamine H2 receptor antagonists (ranitidine and nizatidine) determination after their separation using imidazolium ionic liquids by high performance liquid chromatography (HPLC) combined with UV spectrophotometry were developed. The application of ionic liquids in extraction step allows for selective isolation of analytes from aqueous matrices and their preconcentration. The above methods were applied to the determination of RNT and NZT in environmental samples (river water and wastewater after treatment).

  14. Determination of bisphenols in beverages by mixed-mode solid-phase extraction and liquid chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Regueiro, Jorge; Wenzl, Thomas

    2015-11-27

    Facing growing restrictions on the use of bisphenol A in food contact materials, several bisphenol analogs are arising as major alternatives to replace this chemical in most of its applications. This work reports a simple and robust method based on mixed-mode solid-phase extraction and stable-isotope dilution liquid chromatography-tandem mass spectrometry for the analysis of bisphenol A and its main analogs - bisphenol S, 4,4'-sulfonylbis(2-methylphenol), bisphenol F, bisphenol E, bisphenol B, bisphenol Z, bisphenol AF, bisphenol AP, tetrabromobisphenol A and bisphenol P - in alcoholic and non-alcoholic beverages. Mixed-mode solid-phase extraction, combining cationic exchange and reversed-phase mechanisms, was optimized to provide a selective extraction and purification of the target analytes. Derivatization of bisphenols with pyridine-3-sulfonyl chloride allowed increasing their ionization efficiency by electrospray ionization. Validation of the proposed method was performed in terms of selectivity, matrix effects, linearity, precision, measurement uncertainty, trueness and limits of detection. Satisfactory repeatability and intermediate precision were obtained; the related relative standard deviations were ≤9% and ≤12%, respectively. The relative expanded uncertainty (k=2) was below 20% for all bisphenol analogs and the trueness of the method was demonstrated by recovery experiments. Limits of detection (LOD) ranged from 1.6ngL(-1) to 27.9ngL(-1) for all compounds. Finally, several canned and non-canned beverages were analyzed to demonstrate the applicability of the method. Only bisphenol A and three bisphenol F isomers were detected in any of the samples. Bisphenol A concentration ranged from

  15. Screening and quantitative determination of twelve acidic and neutral pharmaceuticals in whole blood by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Simonsen, Kirsten Wiese; Steentoft, Anni; Buck, Maike

    2010-01-01

    . The method was fully validated for salicylic acid, paracetamol, phenobarbital, carisoprodol, meprobamate, topiramate, etodolac, chlorzoxazone, furosemide, ibuprofen, warfarin, and salicylamide. The method also tentatively includes thiopental, theophylline, piroxicam, naproxen, diclophenac, and modafinil......We describe a multi-method for simultaneous identification and quantification of 12 acidic and neutral compounds in whole blood. The method involves a simple liquid-liquid extraction, and the identification and quantification are performed using liquid chromatography-tandem mass spectrometry...

  16. A novel liquid/liquid extraction process composed of surfactant and acetonitrile for purification of polygalacturonase enzyme from Durio zibethinus.

    Science.gov (United States)

    Amid, Mehrnoush; Manap, Yazid; Azmira, Farhana; Hussin, Muhaini; Sarker, Zaidul Islam

    2015-07-01

    Polygalacturonase is one of the important enzymes used in various industries such as food, detergent, pharmaceutical, textile, pulp and paper. A novel liquid/liquid extraction process composed of surfactant and acetonitrile was employed for the first time to purify polygalacturonase from Durio zibethinus. The influences of different parameters such as type and concentration of surfactants, concentrations of acetonitrile and composition of surfactant/acetonitrile on partitioning behavior and recovery of polygalacturonase was investigated. Moreover, the effect of pH of system and crude load on purification fold and yield of purified polygalacturonase were studied. The results of the experiment indicated the polygalacturonase was partitioned into surfactant top rich phase with impurities being partitioned into acetonitrile bottom rich phase in the novel method of liquid/liquid process composed of 23% (w/w) Triton X-100 and 19% (w/w) acetonitrile, at 55.6% of TLL (tie line length) crude load of 25% (w/w) at pH 6.0. Recovery and recycling of components also was measured in each successive step of liquid/liquid extraction process. The enzyme was successfully recovered by the method with a high purification factor of 14.3 and yield of 97.3% while phase components were also recovered and recycled above 95%. This study demonstrated that the novel method of liquid/liquid extraction process can be used as an efficient and economical extraction method rather than the traditional methods of extraction for the purification and recovery of the valuable enzyme.

  17. Sorptive extraction using polydimethylsiloxane/metal-organic framework coated stir bars coupled with high performance liquid chromatography-fluorescence detection for the determination of polycyclic aromatic hydrocarbons in environmental water samples.

    Science.gov (United States)

    Hu, Cong; He, Man; Chen, Beibei; Zhong, Cheng; Hu, Bin

    2014-08-22

    In this work, metal-organic frameworks (MOFs, Al-MIL-53-NH₂) were synthesized via the hydrothermal method, and novel polydimethylsiloxane/metal-organic framework (PDMS/MOFs, PDMS/Al-MIL-53-NH₂)-coated stir bars were prepared by the sol-gel technique. The preparation reproducibility of the PDMS/MOFs-coated stir bar was good, with relative standard deviations (RSDs) ranging from 4.8% to 14.9% (n=7) within one batch and from 6.2% to 16.9% (n=6) among different batches. Based on this fact, a new method of PDMS/MOFs-coated stir bar sorptive extraction (SBSE) and ultrasonic-assisted liquid desorption (UALD) coupled with high performance liquid chromatography-fluorescence detection (HPLC-FLD) was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. To obtain the best extraction performance for PAHs, several parameters affecting SBSE, such as extraction time, stirring rate, and extraction temperature, were investigated. Under optimal experimental conditions, wide linear ranges and good RSDs (n=7) were obtained. With enrichment factors (EFs) of 16.1- to 88.9-fold (theoretical EF, 142-fold), the limits of detection (LODs, S/N=3) of the developed method for the target PAHs were found to be in the range of 0.05-2.94 ng/L. The developed method was successfully applied to the analysis of PAHs in Yangtze River and East Lake water samples.

  18. Dynamic headspace time-extended helix liquid-phase microextraction.

    Science.gov (United States)

    Huang, Shih-Pin; Chen, Pai-Shan; Huang, Shang-Da

    2009-05-15

    Liquid-phase microextraction (LPME) has been proved to be a fast, inexpensive and effective sample pre-treatment technique for the analyses of pesticides and many other compounds. In this investigation, a new headspace microextraction technique, dynamic headspace time-extended helix liquid-phase microextraction (DHS-TEH-LPME), is presented. In this work, use of a solvent cooling system, permits the temperature of the extraction solvent to be lowered. Lowering the temperature of the extraction solvent not only reduces solvent loss but also extends the feasible extraction time, thereby improving extraction efficiency. Use of a larger volume of the solvent not only extends the feasible extraction time but also, after extraction, leaves a larger volume to be directly injected into the gas chromatography (GC) to increase extraction efficiency and instrument signal. The DHS-TEH-LPME technique was used to extract six organochlorine pesticides (OCPs) from 110ml water samples that had been spiked with the analytes at ng/l levels, and stirred for 60min. The proposed method attained enrichments up to 2121 fold. The effects of extraction solvent identity, sample agitation, extraction time, extraction temperature, and salt concentration on extraction performance were also investigated. The method detection limits (MDLs) varied from 0.2 to 25ng/l. The calibration curves were linear for at least 2 orders of magnitude with R(2)>==0.996. Relative recoveries in river water were more than 86%.

  19. Double-salting out assisted liquid-liquid extraction (SALLE) HPLC method for estimation of temozolomide from biological samples.

    Science.gov (United States)

    Jain, Darshana; Athawale, Rajani; Bajaj, Amrita; Shrikhande, Shruti

    2014-11-01

    The role of temozolomide (TMZ) in treatment of high grade gliomas, melanomas and other malignancies is being defined by the current clinical developmental trials. Temozolomide belongs to the group of alkylating agents and is prescribed to patients suffering from most aggressive forms of brain tumors. The estimation techniques for temozolomide from the extracted plasma or biological samples includes high-performance liquid chromatography with UV detection (HPLC-UV), micellar electrokinetic capillary chromatography (MKEC) and liquid chromatography coupled to mass spectroscopy (LC-MS). These methods suffer from disadvantages like low resolution, low sensitivity, low recovery or cost involvement. An analytical method possessing capacity to estimate low quantities of TMZ in plasma samples with high extraction efficiency (%) and high resolution with cost effectiveness needs to be developed. Cost effective, robust and low plasma component interfering HPLC method using salting out liquid-liquid extraction (SALLE) technique was developed and validated for estimation of drug from plasma samples. The extraction efficiency (%) with conventional LLE technique with methanol, ethyl acetate, dichloromethane and acetonitrile was found to be 5.99±2.45, 45.39±4.56, 46.04±1.14 and 46.23±3.67 respectively. Extraction efficiency (%) improved with SALLE where sodium chloride was used as an electrolyte and was found to be 6.80±5.56, 52.01±3.13, 62.69±2.11 and 69.20±1.18 with methanol, ethyl acetate, dichloromethane and acetonitrile as organic solvent. Upon utilization of two salts for extraction (double salting liquid-liquid extraction) the extraction efficiency (%) was further improved and was twice of LLE. It was found that double salting liquid-liquid extraction technique yielded extraction efficiency (%) of 11.71±5.66, 55.62±3.44, 77.28±2.89 and 87.75±0.89. Hence a method based on double SALLE was developed for quantification of TMZ demonstrating linearity in the range of

  20. Recovery of steroidal alkaloids from potato peels using pressurized liquid extraction.

    Science.gov (United States)

    Hossain, Mohammad B; Rawson, Ashish; Aguiló-Aguayo, Ingrid; Brunton, Nigel P; Rai, Dilip K

    2015-05-13

    A higher yield of glycoalkaloids was recovered from potato peels using pressurized liquid extraction (1.92 mg/g dried potato peels) compared to conventional solid-liquid extraction (0.981 mg/g dried potato peels). Response surface methodology deduced the optimal temperature and extracting solvent (methanol) for the pressurized liquid extraction (PLE) of glycoalkaloids as 80 °C in 89% methanol. Using these two optimum PLE conditions, levels of individual steroidal alkaloids obtained were of 597, 873, 374 and 75 µg/g dried potato peel for α-solanine, α-chaconine, solanidine and demissidine respectively. Corresponding values for solid liquid extraction were 59%, 46%, 40% and 52% lower for α-solanine, α-chaconine, solanidine and demissidine respectively.

  1. Recovery of Steroidal Alkaloids from Potato Peels Using Pressurized Liquid Extraction

    Directory of Open Access Journals (Sweden)

    Mohammad B. Hossain

    2015-05-01

    Full Text Available A higher yield of glycoalkaloids was recovered from potato peels using pressurized liquid extraction (1.92 mg/g dried potato peels compared to conventional solid–liquid extraction (0.981 mg/g dried potato peels. Response surface methodology deduced the optimal temperature and extracting solvent (methanol for the pressurized liquid extraction (PLE of glycoalkaloids as 80 °C in 89% methanol. Using these two optimum PLE conditions, levels of individual steroidal alkaloids obtained were of 597, 873, 374 and 75 µg/g dried potato peel for α-solanine, α-chaconine, solanidine and demissidine respectively. Corresponding values for solid liquid extraction were 59%, 46%, 40% and 52% lower for α-solanine, α-chaconine, solanidine and demissidine respectively.

  2. Comparison of solid phase- and liquid/liquid-extraction for the purification of hair extract prior to multi-class pesticides analysis.

    Science.gov (United States)

    Duca, Radu-Corneliu; Salquebre, Guillaume; Hardy, Emilie; Appenzeller, Brice M R

    2014-04-01

    The present study focuses on the influence of a purification step - after extraction of pesticides from hair and before analysis of the extract - on the sensitivity of analytical methods including compounds from different chemical classes (both parent and metabolites). Sixty-seven pesticides and metabolites from different chemical classes were tested here: organochlorines, organophosphates, carbamates, pyrethroids, ureas, azoles, phenylpyrazoles and neonicotinoids. Two gas chromatography-negative chemical ionization-tandem mass spectrometry methods and one based on ultra-performance liquid chromatography-electrospray tandem mass spectrometry were used. Seven solid-phase extraction cartridges: C18, S-DVB, PS-DVB, GCB, GCB/PSA, SAX/PSA and Florisil/PSA were tested and compared to more classical liquid-liquid extraction procedures using ethyl acetate, hexane and dichloromethane. Although LLE allowed obtaining good results for some compounds, on the whole, SPE clearly provided better recovery for the majority of the pesticide residues tested in the present study. GCB/PSA was clearly the best suited to non-polar compounds such as organochlorines, pyrethroids and organophosphates, with recovery ranging from 45.9% (diflufenican) to 117.1% (parathion methyl). For hydrophilic metabolites (e.g. dialkyl phosphates and other organophosphate metabolites, pyrethroid metabolites, phenols and carbamate metabolites), the best results were obtained with PS-DVB, with recovery ranged from 10.3% (malathion monocarboxylic acid) to 93.1% (para-nitrophenol). For hydrophilic parent pesticides (e.g. neonicotinoids, carbamates, azoles) and metabolites without nucleophilic functions, the best recovery was obtained with SAX/PSA, with recovery ranging from 52.1% (3-hydroxycarbofuran) to 100.9% (3,4-dichloroaniline). Solid phase extraction was found to be more suitable than the liquid-liquid extraction for pesticides and their metabolites determination in terms of number of extracted compounds

  3. Modelling of an industrial NGL-Recovery unit considering environmental and economic impacts

    Energy Technology Data Exchange (ETDEWEB)

    Sharratt, P. N.; Hernandez-Enriquez, A.; Flores-Tlacuahuac, A.

    2009-07-01

    In this work, an integrated model is presented that identifies key areas in the operation of a cryogenic NGL-recovery unit. This methodology sets out to provide deep understanding of various interrelationship across multiple plant operating factors including reliability, which could be essential for substantial improvement of process performance. The integrated model has been developed to predict the economic and environmental impacts of a real cryogenic unit (600 MMCUF/D) during normal operation, and has been built in Aspen TM. (Author)

  4. ANALISIS TRAFIK SUARA JARINGAN KOMUNIKASI TELEPON PT. BADAK NGL BONTANG – KALIMANTAN TIM

    Directory of Open Access Journals (Sweden)

    Ajub Ajulian Zahra

    2012-02-01

    Full Text Available In time being, the user of telecommunication provider is growing up, both of voice and datatelecommunication, so it is needed to design a good and accurate telecommunication tools to avoidproblem’s user. In this case, PT. Badak NGL Bontang needs to review the telecommunication tools(number of trunk because of reducing the number of employee for re-organization.In this paper, application programme is made to analyze voice traffic data with the result that to determineoptimalization number of trunk. Work and condition of system in traffic analysis is influenced by trafficparameters, like ASR (Answered Seizure Ratio, SCH (Seizure per Circuit per Hour, MHTS (MeanHolding Time per Seizure, dan GOS (Grade of Service.From traffic analysis, optimalization number of trunk is 33 trunks with the value of grade of service is 0,1%., so the efficiency number of trunk in PT. Badak NGL is 41,25 % which is determined from comparisonthe number of trunk in traffic analysis (33 trunks and the number of trunk in PT. Badak NGL Bontang (80trunks, so with 33 trunks, the probability of blocking is still low. In traffic analysis, the condition of systemwill be busy if the value of real grade of service is higher than the value of grade of service which isdetermined, and the condition of system will be normal if the value of real grade of service is lower thanthe value of grade of service which is determined.

  5. Determination of methylphenidate in Calliphorid larvae by liquid-liquid extraction and liquid chromatography mass spectrometry - Forensic entomotoxicology using an in vivo rat brain model

    DEFF Research Database (Denmark)

    Bushby, Sarah K.; Thomas, Nicky; Priemel, Petra A.;

    2012-01-01

    and Calliphorid larvae) by liquid-liquid extraction with recovery of >80%, and quantified using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The LC-MS/MS assay was validated for entomotoxicological use and initially applied to male Sprague-Dawley rats (n=6) that were dosed with MPH (20mg/kg) ante......The aim of this study was to examine the potential forensic utilisation of blowfly larvae (Diptera: Calliphoridae) as an alternative toxicological specimen for the detection of the psychotropic model drug methylphenidate (MPH). MPH was extracted from biological matrices (rat brain, serum...

  6. Parallel microwave-assisted synthesis of ionic liquids and screening for denitrogenation of straight-run diesel feed by liquid-liquid extraction.

    Science.gov (United States)

    Ceron, Miguel A; Guzman-Lucero, Diego J; Palomeque, Jorge F; Martínez-Palou, Rafael

    2012-06-01

    Fifty-six ionic liquids were efficiently synthesized in parallel format under one-pot, solvent-free microwave-assisted synthesis. These compounds were evaluated as extracting agents of nitrogen-containing compounds from a real Diesel feed before being submitted to the hydrodesulfurization process to obtain ultralow sulfur Diesel. Our results showed that halogenated ionic liquids are an excellent alternative due to these ionic liquids are relatively inexpensive, presenting a high selectivity for the extraction of nitrogen-containing compounds and can be regenerated and recycled.

  7. Pressurized liquid extraction and HPLC quantification of folic acid in fortified wheat flours.

    Science.gov (United States)

    Araújo, Michel Mozeika; Marchioni, Eric; Villavicencio, Anna Lucia Casañas Haasis; Zhao, Minjie; Zimmermann, Pierre; El-Khoury, Etienne; Bergaentzle, Martine

    2012-08-01

    A pressurized liquid extraction (PLE) method using phosphate buffer as solvent was applied for folic acid (FA) extraction from fortified wheat flours and was compared to a standard solid-liquid extraction (SLE) method. Extracted FA was quantified by reverse phase high-performance liquid chromatography (RP-HPLC) hyphenated with a phenyl column and an absorption photometric detector (λ = 280 nm). Detection and quantification limits were 0.12 and 0.4 ng, respectively, corresponding to 0.06 and 0.2 μg g(-1) of analyzed wheat flour. Equivalent FA contents were found by both extraction methods, but a single PLE allowed a total recovery of FA content, whereas at least three successive SLEs were needed to achieve a total recovery of FA. The obtained results indicated that PLE is a rapid and efficient technique for FA extraction from fortified wheat flour.

  8. Lipid extraction from microalgae using a single ionic liquid

    Science.gov (United States)

    Salvo, Roberto Di; Reich, Alton; Dykes, Jr., H. Waite H.; Teixeira, Rodrigo

    2013-05-28

    A one-step process for the lysis of microalgae cell walls and separation of the cellular lipids for use in biofuel production by utilizing a hydrophilic ionic liquid, 1-butyl-3-methylimidazolium. The hydrophilic ionic liquid both lyses the microalgae cell walls and forms two immiscible layers, one of which consists of the lipid contents of the lysed cells. After mixture of the hydrophilic ionic liquid with a suspension of microalgae cells, gravity causes a hydrophobic lipid phase to move to a top phase where it is removed from the mixture and purified. The hydrophilic ionic liquid is recycled to lyse new microalgae suspensions.

  9. Recovery of Scandium from Leachate of Sulfation-Roasted Bayer Red Mud by Liquid-Liquid Extraction

    Science.gov (United States)

    Liu, Zhaobo; Li, Hongxu; Jing, Qiankun; Zhang, Mingming

    2017-08-01

    The leachate obtained from sulfation-roasted Bayer red mud is suitable for extraction of scandium by liquid-liquid solvent extraction because it contains trace amounts of Fe3+ and Si4+. In this study, a completely new metallurgical process for selective recovery of scandium from Bayer red mud was proposed. The extraction performances of Sc3+, Fe3+, Al3+, Si4+, Ca2+, and Na+ from synthetic leachate of sulfation-roasted red mud were first investigated using organophosphorus extractants (di-2-ethylhexyl phosphoric acid P204 and 2-ethylhexyl phosphoric acid mono-2-ethylhexyl ester P507) and carboxylic acid extractant (Versatic acid 10). It shows that P204 has an excellent extraction ability and that it can be applied to the scandium recovery. P507 and Versatic acid 10 are much poorer in performance for selective extraction of scandium. In the leachate of sulfation-roasted red mud, approximately 97% scandium can be recovered using a P204/sulfonated kerosene (1% v/v) extraction system under the condition of an organic-to-aqueous phase ratio of 10:1 and with an extraction temperature of 15°C.

  10. Solvent extraction in the treatment of acidic high-level liquid waste : where do we stand?

    Energy Technology Data Exchange (ETDEWEB)

    Horwitz, E. P.; Schulz, W. W.

    1998-06-18

    During the last 15 years, a number of solvent extraction/recovery processes have been developed for the removal of the transuranic elements, {sup 90}Sr and {sup 137}Cs from acidic high-level liquid waste. These processes are based on the use of a variety of both acidic and neutral extractants. This chapter will present an overview and analysis of the various extractants and flowsheets developed to treat acidic high-level liquid waste streams. The advantages and disadvantages of each extractant along with comparisons of the individual systems are discussed.

  11. Synthesis of mimic molecularly imprinted ordered mesoporous silica adsorbent by thermally reversible semicovalent approach for pipette-tip solid-phase extraction-liquid chromatography fluorescence determination of estradiol in milk.

    Science.gov (United States)

    Wang, Lu; Yan, Hongyuan; Yang, Chunliu; Li, Zan; Qiao, Fengxia

    2016-07-22

    A mimic molecularly imprinted ordered mesoporous silica (MIOMS) adsorbent was prepared utilizing a thermally reversible semicovalent approach. The thermally reversible covalent template-monomer complex was firstly synthesized by employing 4,4'-sulfonyldiphenol (BPS) and (3-isocyanatopropyl) triethoxysilane (ICPTES) as template and monomer, respectively. The template-monomer complex was incorporated into ordered mesoporous silica via a simple self-assembly process. The adsorption experiment illustrated that the imprint-removed silica (MIOMS-ir) had higher special recognition ability (250μgg(-1)) for estradiol (E2) than the non-imprinted silica (NIOMS-ir) (25μgg(-1)). MIOMS-ir was applied as an adsorbent in pipette-tip solid-phase extraction (PT-SPE) coupled with liquid chromatography-fluorescence detector (LC-FLD) for determination of E2 in milk samples. Under the optimized conditions, only 3mg of the adsorbent, 0.3mL of water as washing solvent, and 0.5mL of acetonitrile-acetic acid (96:4, v/v) as elution solvent were used in the pretreatment procedure of milk samples. Good calibration linearity was obtained in a range of 25ngL(-1) to 1000ngL(-1), and the recoveries at three spiked levels were ranged from 95.4% to 107.0% with relative standard deviations (RSDs) ≤3.1% (n=3). The proposed MIOMS-ir-PT-SPE-LC-FLD method combined the advantages of PT-SPE and ordered mesoporous material such as ease assembly, low cost, high extraction efficiency and large specific surface area, so it is a potential pretreatment strategy for the extraction and determination of E2 in complex milk samples.

  12. Determination of fenvalerate in tomato by ultrasound-assisted solvent extraction combined with dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Pirsaheb, Meghdad; Ahmadi-Jouibari, Toraj; Fattahi, Nazir; Shamsipur, Mojtaba

    2014-09-01

    Ultrasound-assisted solvent extraction (UASE) combined with dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) has been developed for extraction and determination of fenvalerate from tomato samples. Fenvalerate was determined by high-performance liquid-liquid chromatography-ultraviolet detector. Effects of parameters such as type and volume of extraction solvent in the UASE stage, sonication time, type and volume of extraction solvent and disperser solvent in the DLLME-SFO stage, salt addition and pH effect on extraction were studied and optimized. Under the optimum conditions, the calibration graph was linear in the range of 5-500 µg kg(-1) with a detection limit of 0.6 µg kg(-1). The relative standard deviation for five replicate measurements of 100 µg kg(-1) of fenvalerate was 6.5%. The relative recovery of fenvalerate in different tomato samples at a spiking level of 10, 20 and 50 µg kg(-1) is in the range of 93.5-108%. The obtained results show that UASE-DLLME-SFO is a sensitive, fast and simple method for the determination of fenvalerate in tomato samples.

  13. The influence of purge times on the yields of essential oil components extracted from plants by pressurized liquid extraction.

    Science.gov (United States)

    Wianowska, Dorota

    2014-01-01

    The influence of different purge times on the yield of the main essential oil constituents of rosemary (Rosmarinus officinalis L.), thyme (Thymus vulgaris L.), and chamomile (Chamomilla recutita L.) was investigated. The pressurized liquid extraction process was performed by applying different extraction temperatures and solvents. The results presented in the paper show that the estimated yield of essential oil components extracted from the plants in the pressurized liquid extraction process is purge time-dependent. The differences in the estimated yields are mainly connected with the evaporation of individual essential oil components and the applied solvent during the purge; the more volatile an essential oil constituent is, the greater is its loss during purge time, and the faster the evaporation of the solvent during the purge process is, the higher the concentration of less volatile essential oil components in the pressurized liquid extraction receptacle. The effect of purge time on the estimated yield of individual essential oil constituents is additionally differentiated by the extraction temperature and the extraction ability of the applied solvent.

  14. Review of algorithms for modeling metal distribution equilibria in liquid-liquid extraction processes

    Directory of Open Access Journals (Sweden)

    Lozano, L. J.

    2005-10-01

    Full Text Available This work focuses on general guidelines to be considered for application of least-squares routines and artificial neural networks (ANN in the estimation of metal distribution equilibria in liquid-liquid extraction process. The goal of the procedure in the statistical method is to find the values of the equilibrium constants (Kj for the reactions involved in the metal extraction which minimizes the differences between experimental distribution coefficient (Dexp and theoretical distribution coefficients according to the mechanism proposed (Dtheor- In the first part of the article, results obtained with the most frequently routine reported in the bibliography are compared with those obtained using the algorithms previously discussed. In the second part, the main features of a single back-propagation neural network for the same purpose are discussed, and the results obtained are compared with those obtained with the classical methods.

    El trabajo presenta las líneas generales a considerar para la estimación del equilibrio de distribución de metales en procesos de extracción líquido-líquido, según dos métodos: algoritmo clásico de mínimos cuadrados y redes neuronales artificiales. El objetivo del procedimiento, en el caso del método estadístico, es encontrar los valores de las constantes de equilibrio (Kj para las reacciones involucradas en la extracción del metal, que minimizan las diferencias entre el coeficiente de distribución experimental y el coeficiente de distribución teórico, de acuerdo al mecanismo propuesto. En la primera parte del artículo se comparan los resultados obtenidos a partir de los algoritmos usados más habitualmente en la bibliografía, con los datos obtenidos mediante el algoritmo previamente descrito. En la segunda parte, se presentan las características fundamentales para aplicar una red neuronal sencilla con algoritmo back-propagation y los

  15. Fe3O4@ionic liquid@methyl orange nanoparticles as a novel nano-adsorbent for magnetic solid-phase extraction of polycyclic aromatic hydrocarbons in environmental water samples.

    Science.gov (United States)

    Liu, Xiaofei; Lu, Xin; Huang, Yong; Liu, Chengwei; Zhao, Shulin

    2014-02-01

    A novel nano-adsorbent, Fe3O4@ionic liquid@methyl orange nanoparticles (Fe3O4@IL@MO NPs), was prepared for magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. The Fe3O4@IL@MO NPs were synthesized by self-assembly of the ionic liquid 1-octadecyl-3-methylimidazolium bromide (C18mimBr) and methyl orange (MO) onto the surface of Fe3O4 silica magnetic nanoparticles, as confirmed by infrared spectroscopy, ultraviolet-visible spectroscopy and superconducting quantum interface device magnetometer. The extraction performance of Fe3O4@IL@MO NPs as a nano-adsorbent was evaluated by using five PAHs, fluorene (FLu), anthracene (AnT), pyrene (Pyr), benzo(a)anthracene (BaA) and benzo(a)pyrene (BaP) as model analytes. Under the optimum conditions, detection limits in the range of 0.1-2 ng/L were obtained by high performance liquid chromatography-fluorescence detection (HPLC-FLD). This method has been successfully applied for the determination of PAHs in environmental water samples by using the MSPE-HPLC-FLD. The recoveries for the five PAHs tested in spiked real water samples were in the range of 80.4-104.0% with relative standard deviations ranging from 2.3 to 4.9%.

  16. A simple liquid extraction protocol for overcoming the ion suppression of triacylglycerols by phospholipids in liquid chromatography mass spectrometry studies.

    Science.gov (United States)

    Araujo, Pedro; Tilahun, Ephrem; Breivik, Joar Fjørtoft; Abdulkader, Bashir M; Frøyland, Livar; Zeng, Yingxu

    2016-02-01

    It is well-known that triacylglycerol (TAG) ions are suppressed by phospholipid (PL) ions in regiospecific analysis of TAG by mass spectrometry (MS). Hence, it is essential to remove the PL during sample preparation prior to MS analysis. The present article proposes a cost-effective liquid-liquid extraction (LLE) method to remove PL from TAG in different kinds of biological samples by using methanol, hexane and water. High performance thin layer chromatography confirmed the lack of PL in krill oil and salmon liver samples, submitted to the proposed LLE protocol, and liquid chromatography tandem MS confirmed that the identified TAG ions were highly enhanced after implementing the LLE procedure.

  17. [Determination of eight bisphenol diglycidyl ethers in water by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Zhang, Haijing; Lin, Shaobin

    2014-07-01

    A solid phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry (SPE-HPLC-MS/MS) method was developed for the determination of eight bisphenol diglycidyl ethers, including bisphenol A diglycidyl ether (BADGE), bisphenol A (3-chloro-2-hydroxypropyl) glycidyl ether (BADGE x HCl), bisphenol A bis (3-chloro-2-hydroxypropyl) ether (BADGE x 2HCl), bisphenol A (2, 3-dihydroxypropyl) glycidyl ether (BADGE x H2O), bisphenol A bis(2,3-dihydroxypropyl) ether (BADGE x 2H2O), bisphenol A (3-chloro-2-hydroxypropyl) (2,3-dihydroxypropyl) ether (BADGE x HCl x H2O), bisphenol F diglycidyl ether (BFDGE) and bisphenol F bis (3-chloro-2-hydroxypropyl) ether (BFDGE 2HCl) in water. A total of ten samples were collected from the leaching of the coatings for drinking water supply system. Then, 200 mL exposure water was preconcentrated on C18 solid-phase extraction cartridge. The eight compounds were analyzed by liquid chromatography-tandem mass spectrometry method on a C18 column by the gradient elution with methanol, water and 5 mmol/L ammonium acetate as mobile phases in the multiple reaction monitoring (MRM) scan mode. The external matrix standard solutions were used for the quantitative determination and the calibration curves of the eight compounds showed good linearity in the range of 0.007-5.00 microg/L with the correlation coefficients more than 0.999 0. The limits of quantification (LOQs) of the method were 7-91 ng/L. The spiked recoveries ranged from 79.1% to 101% with the relative standard deviations of 4.0% - 12%. The method is sensitive and accurate, and is applicable to the determination of bisphenol diglycidyl ethers in water.

  18. Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction of herbicides in peanuts.

    Science.gov (United States)

    Li, Na; Wang, Zhibing; Zhang, Liyuan; Nian, Li; Lei, Lei; Yang, Xiao; Zhang, Hanqi; Yu, Aimin

    2014-10-01

    Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction was developed and applied to the extraction of pesticides in high fatty matrices. The herbicides were ultrasonically extracted from peanut using ethyl acetate as extraction solvent. The separation of the analytes from a large amount of co-extractive fat was achieved by dispersive solid-phase extraction using MIL-101(Cr) as sorbent. In this step, the analytes were adsorbed on MIL-101(Cr) and the fat remained in bulk. The herbicides were separated and determined by high-performance liquid chromatography. The experimental parameters, including type and volume of extraction solvent, ultrasonication time, volume of hexane and eluting solvent, amount of MIL-101(Cr) and dispersive solid phase extraction time, were optimized. The limits of detection for herbicides range from 0.98 to 1.9 μg/kg. The recoveries of the herbicides are in the range of 89.5-102.7% and relative standard deviations are equal or lower than 7.0%. The proposed method is simple, effective and suitable for treatment of the samples containing high content of fat.

  19. Determination of Gemfibrozil (Lipitor and Lopid in Water, Biological Fluids and Drug Matrix by Dispersive Liquid-Liquid micro Extraction (DLLME and Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Ghorbani A.

    2014-07-01

    Full Text Available In this study Dispersive liquid-liquid micro extraction (DLLME coupled with High performance liquid chromatography was applied for the determination of Gemfibrozil in water, drug`s matrix and biological liquids (human plasma and urine. In this method, the appropriate mixture of extraction solvent (200 μl chlorophorm and disperser solvent (1 ml methanol are injected rapidly into the aqueous sample (10.0 ml by syringe, cloudy solution is formed that consisted of fine particles of extraction solvent which is dispersed entirely into aqueous phase. The mixture was centrifuged and the extraction solvent is sedimented on the bottom of the conical test tube. 50 μl of the sedimented phase is puted in a vial and it`s solvent is evaporated. Then 1ml methanol injected to vial and 20 μL of it injected into the HPLC for separation and determination of Gemfibrozil. Some important parameters, such as kind of extraction and disperser solvent, volume of them, extraction time, pH and ionic strength of the aqueous feed solution were optimized. Under the optimum conditions, the enrichment factors and extraction recoveries were 10 and 93.64%. The linear range was (0.1-100.0 mgl-1, limit of detection was 12.3 mgl-1. The relative standard deviations (RSD for 2 mgl-1 of Gemfibrozil in water were 1.3%, (n=10.

  20. Separation-preconcentration of nickel and lead in food samples by a combination of solid-liquid-solid dispersive extraction using SiO2 nanoparticles, ionic liquid-based dispersive liquid-liquid micro-extraction.

    Science.gov (United States)

    Jalbani, Nusrat; Soylak, Mustafa

    2015-01-01

    A microextraction method for the determination of nickel and lead using solid-liquid-solid dispersive extraction followed by ionic liquid-based dispersive liquid-liquid microextraction (SLSDE-ILDLLME) was presented. It was applied to the extraction of nickel and lead from food samples. Ammonium pyrrolidine dithiocarbamate (APDC) as complexing agent, [C4MIM][PF6] as ionic liquid, SiO2 as nanoparticles and 2 mol L(-1) HNO3 as eluent were used. Several important parameters such as amount of IL, extraction time, pH and volume of the complexing agent were investigated. The quantitative recoveries were obtained at pH 7.0 for analytes. Under the optimum conditions, the limits of detection (LODs) calculated using 3(Sd)blank/m were 0.17 for Ni(II) and 0.79 µg L(-1) for Pb(II) for aqueous solutions with 125 enrichment factor (EF). The limit of detections of the analyte ions (3(Sd)blank/m) for solid samples were 0.09 µg g(-1) (Ni) and 0.40 µg g(-1) (Pb). The accuracy of the proposed method was confirmed by the analysis of standard reference material (1577c bovine liver) and spiked recovery test. The proposed method was applied to determine nickel and lead levels in chicken, fish and meat samples.

  1. Determination of non-ionic polyethoxylated surfactants in wastewater and river water by mixed hemimicelle extraction and liquid chromatography-ion trap mass spectrometry.

    Science.gov (United States)

    Cantero, Manuel; Rubio, Soledad; Pérez-Bendito, Dolores

    2005-03-04

    The capability of hemimicelles-based solid phase extraction (SPE)/liquid chromatography/atmospheric pressure chemical ionisation in positive mode, ion trap mass spectrometry (LC/(APCl+-IT)-MS) for the concentration, separation and quantitation of non-ionic surfactants has been investigated. Concentration was based on the formation of mixed aggregates of analytes [alkylphenol ethoxylates (APE, octyl and nonyl) and alkyl ethoxylates (AE, C12-C16)] with the anionic surfactant sodium dodecyl sulphate (SDS) that is adsorbed on alumina. Parameters affecting SPE were investigated on the basis that hemimicelles are dynamic entities in equilibrium with the aqueous phase. The performance of ion trap mass spectrometry for MS and MS/MS quantitation of non-ionic homologues was assessed. Recoveries of analytes from wastewater influent and effluent and river water samples ranged between 91 and 98% and were found independent on the length of the alkyl chain under the optimised conditions. Anionic surfactants did not interfere to the levels found in environmental samples. The detection limits ranged between 14 and 111 ng/l for wastewater influent, 10 and 40 for wastewater effluent and 4 and 35 for river water, after concentration of 250, 500 and 750 ml of sample, respectively. The approach was applied to the determination of AE and APE in influent and effluent samples from four wastewater treatment plants and four river samples. The concentrations of individual non-ionic surfactants found ranged between 0.3 and 373 microg/l.

  2. Determination of palladium in human urine by high-performance liquid chromatography and ultraviolet detection after ultraviolet photolysis and selective solid-phase extraction.

    Science.gov (United States)

    Philippeit, G; Angerer, J

    2001-09-05

    The high-performance liquid chromatographic method with UV detection described below permits the selective determination of traces of palladium in human urine. After UV photolysis, during which the complete organic matrix was destroyed, the palladium was selectively enriched by solid-phase extraction (SPE). The reversed-phase C18 SPE column material was loaded with the ligand N,N-diethyl-N'-benzoylthiourea (DEBT) which shows an excellent complexing capacity for palladium in acidic solutions and at room temperature. The Pd(DEBT)2 complex was eluted with ethanol. After isocratic separation on the analytical column (MeOH/H2O 98:2 (v/v)), the complex was detected at 274 nm. The detection limit was 10 ng Pd/l. The relative standard deviations (RSD) of the within-series imprecision were in the range between 11% (75 ng Pd/l) and 7% (180 ng Pd/l). The between-day imprecision was 11% (75 ng Pd/l) and 5% (180 ng Pd/l). The recovery rates ranged between 94 and 96%. Using this method, urine samples of 44 persons from the general population were analysed. Only in one urine sample could palladium be detected. For comparison, 10 persons with occupational palladium exposure were examined. The urinary concentrations ranged from <10 to 2,538 ng/l.

  3. Enhancing Extraction and Detection of Veterinary Antibiotics in Solid and Liquid Fractions of Manure.

    Science.gov (United States)

    Wallace, Joshua S; Aga, Diana S

    2016-03-01

    Analysis of veterinary antibiotics in separated liquid and solid fractions of animal manures is vital because of wide variations in the composition of agriculturally applied manure. Differentiation of antibiotic concentrations is important between liquid and solid manures, as their sorption onto the solid fraction depends on physicochemical properties of each antibiotic and manure composition (e.g., organic content, pH) and because each fraction may be treated and reused differently. Here, an efficient and sensitive method for the analysis of 22 veterinary antibiotics in the liquid and solid fractions of manure is reported. Tetracycline (TC), macrolide, and sulfonamide antibiotics were extracted from liquid manure by liquid-liquid extraction (LLE) with methanol following acidification with acetic acid. Extraction from solids was performed by sonication with acetonitrile, methanol, and 0.1 M EDTA-McIlvaine buffer. Cleanup of extracts was achieved by solid-phase extraction with hydrophilic-lipophilic balance (HLB) cartridges or tandem amino (NH2) and HLB cartridges. Quantification of antibiotics was performed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) under wrong-way-round (WWR) ionization for sulfonamides and TCs and right-way-round ionization for macrolides. Recoveries of 58 to 94.7% and 62 to 94.3% were obtained in liquid and solid manure, respectively. Method detection limits range from 1.2 to 12 ng L and 0.5 to 7.9 μg kg dry wt. in liquids and solids, respectively. This method allows for extraction and analysis of both mobile antibiotics in liquid phase and hydrophobic antibiotics adsorbed on the solids. Without separate analysis, antibiotic concentrations may be improperly estimated by analyzing whole manure, as reported in many studies to date.

  4. [Effects of fungi and its liquid extract on seed germination of Dendrobium hancockii Rolf].

    Science.gov (United States)

    Guo, S; Xu, J

    1990-07-01

    The experiment revealed that several species of fungi isolated from the protocorms of Orchidaceae notable promote the seed germination of Dendrobium hancockii. The seed germination rate amounts to over 20% when the seeds are incubated with fungi, but zero without incubation. Seed germination rate ranges from 40 to 70% when the incubation is affected in liquid extract of the cultural products of fungi, but the growth of protocorms and seedlings of Dendrobium hancockii is slower in liquid extract of fungi than on mycolia.

  5. Microwave-assisted preparation of poly(ionic liquids)-modified magnetic nanoparticles for pesticide extraction.

    Science.gov (United States)

    Zhang, Ruizhe; Su, Ping; Yang, Lu; Yang, Yi

    2014-06-01

    Novel poly(ionic liquids) were synthesized and immobilized on prepared magnetic nanoparticles, which were used to extract pesticides from fruit and vegetable samples by dispersive solid-phase extraction prior to high-performance liquid chromatography analysis. Compared with monomeric ionic liquids, poly(ionic liquids) have a larger effective contact area and higher viscosity, so they can achieve higher extraction efficiency and be used repeatedly without a decrease in analyte recovery. The immobilized poly(ionic liquids) were rapidly separated from the sample matrix, providing a simple approach for sample pretreatment. The nature and volume of the desorption solvent and amount of poly(ionic liquid)-modified magnetic material were optimized for the extraction process. Under optimum conditions, calibration curves were linear (R(2) > 0.9988) for pesticide concentrations in the range of 0.100-10.000 μg/L. The relative standard deviations for repeated determinations of the four analytes were 2.29-3.31%. The limits of detection and quantification were 0.29-0.88 and 0.97-2.93 μg/L, respectively. Our results demonstrate that the developed poly(ionic liquid)-modified material is an effective absorbent to extract pesticides from fruit and vegetable samples.

  6. Coupling of homogeneous liquid-liquid extraction and dispersive liquid-liquid microextraction for the extraction and preconcentration of polycyclic aromatic hydrocarbons from aqueous samples followed by GC with flame ionization detection.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Khiavi, Elahe Behboudi; Khorram, Parisa; Mogaddam, Mohammad Reza Afshar

    2017-01-01

    In the present study, a simple and rapid method for the extraction and preconcentration of some polycyclic aromatic hydrocarbons in water samples has been developed. In this method, two sample preparation methods were combined to obtain high extraction recoveries and enrichment factors for sensitive analysis of the selected analytes. In the first stage of the method, a homogeneous solution containing an aqueous solution and cyclohexyl amine is broken by the addition of a salt. After centrifugation, the upper collected phase containing the extracted analytes is subjected to the following dispersive liquid-liquid microextraction method. Rapid injection of the mixture of cyclohexyl amine resulted from the first stage and 1,1,2-trichloroethane (as an extraction solvent) into an acetic acid solution is led to form a cloudy solution. After centrifuging, the fine droplets of the extraction solvent are settled down in the bottom of the test tube, and an aliquot of it is analyzed by gas chromatography. Under the optimum extraction conditions, enrichment factors and limits of detection for the studied analytes were obtained in the ranges of 616-752 and 0.08-0.20 μg/L, respectively. The simplicity, high extraction efficiency, short sample preparation time, low cost, and safety demonstrated the efficiency of this method relative to other approaches.

  7. Aromatics extraction from pyrolytic sugars using ionic liquid to enhance sugar fermentability

    NARCIS (Netherlands)

    Li, X.; Luque-Moreno, L.C.; Oudenhoven, S.R.G; Rehmann, L.; Kersten, S.R.A.; Schuur, B.

    2016-01-01

    Fermentative bioethanol production from pyrolytic sugars was improved via aromatics removal by liquid–liquid extraction. As solvents, the ionic liquid (IL) trihexyltetradecylphosphonium dicyanamide (P666,14[N(CN)2]) and ethyl acetate (EA) were compared. Two pyrolytic sugar solutions were created fro

  8. Ionic Liquid-Based Microwave-Assisted Extraction of Flavonoids from Bauhinia championii (Benth. Benth.

    Directory of Open Access Journals (Sweden)

    Wei Xu

    2012-12-01

    Full Text Available An ionic liquids (IL-based microwave-assisted approach for extraction and determination of flavonoids from Bauhinia championii (Benth. Benth. was proposed for the first time. Several ILs with different cations and anions and the microwave-assisted extraction (MAE conditions, including sample particle size, extraction time and liquid-solid ratio, were investigated. Two M 1-butyl-3-methylimidazolium bromide ([bmim] Br solution with 0.80 M HCl was selected as the optimal solvent. Meanwhile the optimized conditions a ratio of liquid to material of 30:1, and the extraction for 10 min at 70 °C. Compared with conventional heat-reflux extraction (CHRE and the regular MAE, IL-MAE exhibited a higher extraction yield and shorter extraction time (from 1.5 h to 10 min. The optimized extraction samples were analysed by LC-MS/MS. IL extracts of Bauhinia championii (Benth.Benth consisted mainly of flavonoids, among which myricetin, quercetin and kaempferol, β-sitosterol, triacontane and hexacontane were identified. The study indicated that IL-MAE was an efficient and rapid method with simple sample preparation. LC-MS/MS was also used to determine the chemical composition of the ethyl acetate/MAE extract of Bauhinia championii (Benth. Benth, and it maybe become a rapid method to determine the composition of new plant extracts.

  9. Ionic liquid-based microwave-assisted extraction of rutin from Chinese medicinal plants.

    Science.gov (United States)

    Zeng, Huan; Wang, Yuzhi; Kong, Jinhuan; Nie, Chan; Yuan, Ya

    2010-12-15

    An ionic liquid-based microwave-assisted extraction (ILMAE) method has been developed for the effective extraction of rutin from Chinese medicinal plants including Saururus chinensis (Lour.) Bail. (S. chinensis) and Flos Sophorae. A series of 1-butyl-3-methylimidazolium ionic liquids with different anions were investigated. The results indicated that the characteristics of anions have remarkable effects on the extraction efficiency of rutin and among the investigated ionic liquids, 1-butyl-3-methylimidazolium bromide ([bmim]Br) aqueous solution was the best. In addition, the ILMAE procedures for the two kinds of medicinal herbs were also optimized by means of a series of single factor experiments and an L(9) (3(4)) orthogonal design. Compared with the optimal ionic liquid-based heating extraction (ILHE), marinated extraction (ILME), ultrasonic-assisted extraction (ILUAE), the optimized approach of ILMAE gained higher extraction efficiency which is 4.879 mg/g in S. chinensis with RSD 1.33% and 171.82 mg/g in Flos Sophorae with RSD 1.47% within the shortest extraction time. Reversed phase high performance liquid chromatography (RP-HPLC) with ultraviolet detection was employed for the analysis of rutin in Chinese medicinal plants. Under the optimum conditions, the average recoveries of rutin from S. chinensis and Flos Sophorae were 101.23% and 99.62% with RSD lower than 3%, respectively. The developed approach is linear at concentrations from 42 to 252 mg L(-1) of rutin solution, with the regression coefficient (r) at 0.99917. Moreover, the extraction mechanism of ILMAE and the microstructures and chemical structures of the two researched samples before and after extraction were also investigated. With the help of LC-MS, it was future demonstrated that the two researched herbs do contain active ingredient of rutin and ionic liquids would not influence the structure of rutin.

  10. Ultrasonic-Assisted Extraction of Procyanidins Using Ionic Liquid Solution from Larix gmelinii Bark

    Directory of Open Access Journals (Sweden)

    Xiaowei Sun

    2013-01-01

    Full Text Available An ionic liquid-based ultrasonic-assisted extraction method has been developed for the effective extraction of procyanidins from Larix gmelinii bark. So as to evaluate the performance of ionic liquids in ultrasonic-assisted extraction process, the effects caused by changes in the anion and the alkyl chain length of the cation on the extraction efficiency were investigated in this paper. The results indicated that the characteristics of anions had remarkable effects on the extraction efficiency of procyanidins, and 1-butyl-3-methylimidazolium bromide ([Bmim]Br aqueous solution was the best among the investigated ionic liquids. The optimum conditions for the extraction were as follows: [Bmim]Br concentration 1.25 M, soak time 3 h, solid-liquid ratio 1 : 10, ultrasonic power 150 W, and ultrasonic time 30 min. This work not only introduces a simple, green, and highly efficient sample preparation method for extraction of procyanidins from L. gmelinii bark, but also reveals the tremendous application potential of ionic liquids.

  11. Sensitive spectrophotometric determination of Co(II) using dispersive liquid-liquid micro-extraction method in soil samples.

    Science.gov (United States)

    Hasanpour, Foroozan; Hadadzadeh, Hassan; Taei, Masoumeh; Nekouei, Mohsen; Mozafari, Elmira

    2016-05-01

    Analytical performance of conventional spectrophotometer was developed by coupling of effective dispersive liquid-liquid micro-extraction method with spectrophotometric determination for ultra-trace determination of cobalt. The method was based on the formation of Co(II)-alpha-benzoin oxime complex and its extraction using a dispersive liquid-liquid micro-extraction technique. During the present work, several important variables such as pH, ligand concentration, amount and type of dispersive, and extracting solvent were optimized. It was found that the crucial factor for the Co(II)-alpha benzoin oxime complex formation is the pH of the alkaline alcoholic medium. Under the optimized condition, the calibration graph was linear in the ranges of 1.0-110 μg L(-1) with the detection limit (S/N = 3) of 0.5 μg L(-1). The preconcentration operation of 25 mL of sample gave enhancement factor of 75. The proposed method was applied for determination of Co(II) in soil samples.

  12. Ionic liquid-based dispersive liquid-liquid microextraction with back-extraction coupled with capillary electrophoresis to determine phenolic compounds.

    Science.gov (United States)

    Zhou, Caihong; Tong, Shanshan; Chang, Yunxia; Jia, Qiong; Zhou, Weihong

    2012-04-01

    Ionic liquid (IL) based dispersive liquid-liquid microextraction (DLLME) with back-extraction coupled with capillary electrophoresis ultraviolet detection was developed to determine four phenolic compounds (bisphenol-A, β-naphthol, α-naphthol, 2, 4-dichlorophenol) in aqueous cosmetics. The developed method was used to preconcentrate and clean up the four phenolic compounds including two steps. The analytes were transferred into room temperature ionic liquid (1-octyl-3-methylimidazolium hexafluorophosphate, [C(8) MIM][PF(6) ]) rich-phase in the first step. In the second step, the analytes were back-extracted into the alkaline aqueous phase. The effects of extraction parameters, such as type and volume of extraction solvent, type and volume of disperser, extraction and centrifugal time, sample pH, salt addition, and concentration and volume of NaOH in back-extraction were investigated. Under the optimal experimental conditions, the preconcentration factors were 60.1 for bisphenol-A, 52.7 for β-naphthol, 49.2 for α-naphthol, and 18.0 for 2, 4-dichlorophenol. The limits of detection for bisphenol-A, β-naphthol, α-naphthol and 2, 4-dichlorophenol were 5, 5, 8, and 100 ng mL(-1), respectively. Four kinds of aqueous cosmetics including toner, soften lotion, make-up remover, and perfume were analyzed and yielded recoveries ranging from 81.6% to 119.4%. The main advantages of the proposed method are quick, easy, cheap, and effective.

  13. Extraction of S- and N-Compounds from the Mixture of Hydrocarbons by Ionic Liquids as Selective Solvents

    OpenAIRE

    Beata Gabrić; Aleksandra Sander; Marina Cvjetko Bubalo; Dejan Macut

    2013-01-01

    Liquid-liquid extraction is an alternative method that can be used for desulfurization and denitrification of gasoline and diesel fuels. Recent approaches employ different ionic liquids as selective solvents, due to their general immiscibility with gasoline and diesel, negligible vapor pressure, and high selectivity to sulfur- and nitrogen-containing compounds. For that reason, five imidazolium-based ionic liquids and one pyridinium-based ionic liquid were selected for extraction of thiophene...

  14. Determination of trace amount of lead in industrial and municipal effluent water samples based on dispersive liquid-liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Shirkhanloo, H. [Iranian Petroleum Industry Health Research Institute, Occupational and Environmental Health Research Center, Tehran (Iran, Islamic Republic of); Sedighi, K.; Mousavi, H. Z., E-mail: hzmousavi@semnan.ac.ir [Semnan University, College of Science, Department of Chemistry, Semnan (Iran, Islamic Republic of)

    2014-10-01

    In this study, a simple, sensitive and accurate method was developed for the determination of lead ion by combining ionic liquid dispersive liquid-liquid extraction (Il-DLL E) with flame atomic absorption spectrometry. Tetraethyl thiuram disulfide (Tetd), acetone and 1-octyl-3m ethylimidazolium hexafluorophosphate [(C{sub 8}MIM) (PF{sub 6})] were used as the chelating agent, dispersive and extraction solvent, respectively. Under the optimal conditions, the calibration graph was linear in the range of 5-190 μg L{sup -1} of lead and the detection limit was 0.8 μg L{sup -1} with a sample volume of 200 ml. The proposed method was validated by the analysis of one certified reference material and applied successfully to the determination of lead in real water samples. (Author)

  15. New methods and materials for solid phase extraction and high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Dumont, Philip John [Iowa State Univ., Ames, IA (United States)

    1996-04-23

    This paper describes methods for solid phase extraction and high performance liquid chromatography (HPLC). The following are described: Effects of Resin Sulfonation on the Retention of Polar Organic Compounds in Solid Phase Extraction; Ion-Chromatographic Separation of Alkali Metals In Non-Aqueous Solvents; Cation-Exchange Chromatography in Non-Aqueous Solvents; and Silicalite As a Stationary Phase For HPLC.

  16. Parallel artificial liquid membrane extraction of acidic drugs from human plasma

    DEFF Research Database (Denmark)

    Roldan-Pijuan, Mercedes; Pedersen-Bjergaard, Stig; Gjelstad, Astrid

    2015-01-01

    The new sample preparation concept “Parallel artificial liquid membrane extraction (PALME)” was evaluated for extraction of the acidic drugs ketoprofen, fenoprofen, diclofenac, flurbiprofen, ibuprofen, and gemfibrozil from human plasma samples. Plasma samples (250 μL) were loaded into individual...

  17. Determination of tocopherols and tocotrienols in cereals by pressurized liquid extraction-liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Bustamante-Rangel, M; Delgado-Zamarreño, M M; Sánchez-Pérez, A; Carabias-Martínez, R

    2007-03-28

    A rapid analytical method including pressurized liquid extraction (PLE) and liquid chromatography-electrospray ionisation-mass spectrometry (LC-ESI-MS) has been developed for the determination of tocopherols and tocotrienols in cereals. The pressurized liquid extraction parameters were optimized in order to maximize the extraction efficiency. The use of methanol as extraction solvent at a temperature of 50 degrees C and a pressure of 110 bar, using one cycle of extraction with a static time of 5 min, provided the best results. A good LC separation was achieved using a C(18) column and a solution of 6.0 mM ammonia in methanol/water (97:3, v/v) as the mobile phase at a flow rate of 0.2 mL min(-1). MS coupling with an ESI interface in the negative ion mode was used as the detection technique. In the present work, it is shown that the addition of a base to the mobile phase is required to enhance the ionization of tocopherols and tocotrienols in negative ion mode electrospray ionization. The applicability of the method to cereal samples was confirmed. The reproducibility of the procedure was good, with relative standard deviations in the 6-10% range. The recoveries of added tocopherols from cereal samples ranged from 91 to 109%.

  18. Liquid-liquid reductive extraction in molten fluoride salt/liquid aluminium as a core of process for the An/Ln group separation

    Energy Technology Data Exchange (ETDEWEB)

    Conocar, O

    2007-06-15

    This report concerns a pyrochemical process based on liquid-liquid extraction in a molten fluoride/liquid aluminium system as a core process for actinide (An)/lanthanide (Ln) group separation, studied at CEA. The basic and demonstrative experiments have established the feasibility of the An/Ln group separation in the molten fluoride/liquid aluminium system (U, Pu, Np, Am, Cm traces from Nd, Ce, Eu, Sm, Eu, La - An/Ln separation factors over 1000 - An recovery yield over 98 % in one batch). The main experimental efforts must now be targeted on the recovery of actinides from the Al matrix. A thermodynamic and bibliographical survey has been done. It shows that back-extraction in a molten chloride melt could be a promising technique for this purpose.

  19. Thermal stability of liquid antioxidative extracts from pomegranate peel

    Science.gov (United States)

    This research was carried out to assess the potential of using the natural antioxidants in pomegranate peel extracts as replacement for synthetic antioxidants. As a result the thermal stability of pomegranate peel extract products during sterilization and storage, and its effect on industrial, color...

  20. Storage stability of sterilized liquid extracts from pomegranate peel

    Science.gov (United States)

    Pomegranate marc, a byproduct of commercial juice production, has shown promise as a starting material for the recovery of health promoting phenolic compounds. The stability of aqueous extracts prepared from pomegranate marc was evaluated in preparation to directly using these extracts as nutraceuti...

  1. Extraction and determination of hormones in cosmetics by homogeneous ionic liquid microextraction high-performance liquid chromatography.

    Science.gov (United States)

    Kang, Mingqin; Sun, Shuo; Li, Na; Zhang, Daihui; Chen, Mingyan; Zhang, Hanqi

    2012-08-01

    The homogeneous ionic liquid microextraction was applied to the extraction of hormones from cosmetics and the hormones were determined by high-performance liquid chromatography. 1-Hexyl-3-methylimidazolium tetrafluoroborate was used as extraction solvent. Ammonium hexafluorophosphate as used as ion-pairing agent. Several experimental parameters, including the volume of 1-hexyl-3-methylimidazolium tetrafluoroborate, amount of ammonium hexafluorophosphate and sodium chloride, extraction and centrifuge time, and the pH value, were optimized. The limits of detection and quantification for the analytes ranged from 0.03 to 0.24 ng/mL and from 0.10 to 0.79 ng/mL, respectively. The precision for determining the hormones was lower than 5.2%. The proposed method was successfully developed for the determination of hormones in real cosmetic samples.

  2. Liquid-liquid extraction of ion-association complexes of cobalt(II-4-(2-pyridylazoresorcinol with ditetrazolium salts

    Directory of Open Access Journals (Sweden)

    Divarova Vidka V.

    2015-01-01

    Full Text Available The formation and liquid-liquid extraction of ion-association complexes between Co(II-4-(2-Pyridylazoresorcinol (PAR anionic chelates and cations of three ditetrazolium chlorides were studied: Blue Tetrazolium chloride (BTC, Neotetrazolium chloride (NTC and Nitro Blue Tetrazolium chloride (NBT. The optimum conditions for the formation and solvent extraction of the ion-association comlpex chelates were determined. It has been found that in the systems of Co(II-PAR-DTS, the reactants are reacted in molar ratios 1:2:1 and the general formula of complexes was suggested. The extraction equilibria were investigated and quantitatively characterized by the equilibrium constants and the recovery factors. The analytical characteristics of the complexes were calculated.

  3. Lignin extraction from straw by ionic liquids and enzymatic hydrolysis of the cellulosic residues.

    Science.gov (United States)

    Fu, Dongbao; Mazza, Giuseppe; Tamaki, Yukihiro

    2010-03-10

    Lignocellulose is a promising starting material for bioproducts, ranging from biofuels to specialty chemicals; however, lignocellulose is resistant to enzymatic degradation. Overcoming this resistance is therefore an important priority for the development of the lignocellulosic biorefinery concept. In this work, 1-ethyl-3-methylimidazolium acetate ([emim]Ac) was selected from six ionic liquid candidates for the extraction of lignin from triticale and wheat straw and flax shives. Lignin extractability, composition, and cellulose enzymatic digestibility of the residues after extraction by [emim]Ac were determined at various temperatures (70-150 degrees C) and time intervals (0.5-24 h). The optimal result (52.7% of acid insoluble lignin in triticale straw) was obtained at 150 degrees C after 90 min, yielding >95% cellulose digestibility of the residue. Little cellulose was extracted, and the extracted lignin was recovered by acid precipitation. Selective extraction of lignin by ionic liquids is a potentially efficient technique for the comprehensive utilization of lignocellulose.

  4. Application of ionic liquids in the microwave-assisted extraction of pectin from lemon peels.

    Science.gov (United States)

    Guolin, Huang; Jeffrey, Shi; Kai, Zhang; Xiaolan, Huang

    2012-01-01

    Microwave-assisted extraction of pectin from lemon peels by using ionic liquid as alternative solvent was investigated. The extracted pectin was detected by Fourier transform infrared spectra. The extraction conditions were optimized through the different experiments in conjunction with the response surface methodology. A pectin yield of 24.68 % was obtained under the optimal parameters: the extraction temperature of 88°C, the extraction time of 9.6 min, and a liquid-solid ratio of 22.7 ml · g(-1). The structure of the pretreated lemon peel samples and the samples after microwave-assisted extraction were characterized by a field emission scanning electron microscope.

  5. Application of Ionic Liquids in the Microwave-Assisted Extraction of Pectin from Lemon Peels

    Directory of Open Access Journals (Sweden)

    Huang Guolin

    2012-01-01

    Full Text Available Microwave-assisted extraction of pectin from lemon peels by using ionic liquid as alternative solvent was investigated. The extracted pectin was detected by Fourier transform infrared spectra. The extraction conditions were optimized through the different experiments in conjunction with the response surface methodology. A pectin yield of 24.68 % was obtained under the optimal parameters: the extraction temperature of 88°C, the extraction time of 9.6 min, and a liquid-solid ratio of 22.7 ml⋅g-1. The structure of the pretreated lemon peel samples and the samples after microwave-assisted extraction were characterized by a field emission scanning electron microscope.

  6. Liquid Phase Micro-Extraction of Linear Alkylbenzene Sulfonate Anionic Surfactants in Aqueous Samples

    OpenAIRE

    2011-01-01

    Hollow fiber liquid phase micro-extraction (LPME) of linear alkylbenzene sulfonates (LAS) from aqueous samples was studied. Ion pair extraction of C10, C11, C12 and C13 homologues was facilitated with trihexylamine as ion-pairing agent, using di-n-hexylether as solvent for the supported liquid membrane (SLM). Effects of extraction time, acceptor buffer concentration, stirring speed, sample volume, NaCl and humic acids were studied. At 10–50 μg L−1 linear R2-coefficients were 0.99 for C10 and ...

  7. Determination of furfurals in Manuka honey using piston-cylinder liquid-liquid extraction and gas chromatography.

    Science.gov (United States)

    Gras, K; Luong, J; Gras, R; Cortes, H J; Shellie, R A

    2014-10-03

    A rapid analytical approach for the direct measurement of furfurals such as 2-furfural and 5-methyl-2-furfural at parts-per-billion level in Manuka honey is described. The approach employs a piston-cylinder based liquid-liquid extraction device using chloroform extraction solvent. This device substantially reduces extraction time by a factor of 120 times compared to solid phase micro-extraction and reduces solvent consumption by a factor of 25 times compared to liquid-liquid extraction with mechanical agitation. A recently commercialised capillary column offering a high degree of inertness permits separation and detection of the analytes at ultra-trace level without derivatisation. A three-port planar microfluidic device with a mid-point pressure is also incorporated to back-flush heavier compounds in the matrix to improve column longevity and overall system cleanliness. With this approach, analysis is conducted in less than 7min. Repeatability of retention times for all compounds is less than 0.1% (n=20). The compounds cited can be analysed over a range from 1ng/g to 10μg/g in honey with a 5ng/g limit of quantification (LOQ) and correlation coefficients of at least 0.999. Relative precision is less than 2.8% RSD (n=20) at 50ng/g level with analyte extraction efficiency of greater than 99% (n=3) over a range from 5ng/g to 10μg/g in the matrix described. The analytical system requires only minimal maintenance and is suitable for remote site deployment. Under the analytical conditions established and with a practical LOQ of 5ng/g, 100 samples can be analysed before septum/liner/o-ring replacements are needed. As a preventive measure, the pre-column can be replaced once every six months to maintain chromatographic fidelity.

  8. Liquid membrane extraction techniques for trace metal analysis and speciation in environmental and biological matrices

    Energy Technology Data Exchange (ETDEWEB)

    Ndungu, Kuria

    1999-04-01

    In this thesis, liquid-membrane-based methods for the analysis of trace metal species in samples of environmental and biological origin were developed. By incorporating extracting reagents in the membrane liquid, trace metal ions were selectively separated from humic-rich natural waters and urine samples, prior to their determination using various instrumental techniques. The extractions were performed in closed flow systems thus allowing easy automation of both the sample clean-up and enrichment. An acidic organophosphorus reagent (DEHPA) and a basic tetraalkylammonium reagent (Aliquat-336) were used as extractants in the membrane liquid to selectively extract and enrich cationic and anionic metal species respectively. A speciation method for chromium species was developed that allowed the determination of cationic Cr(III) species and anionic CR(VI) species in natural water samples without the need of a chromatographic separation step prior to their detection. SLM was also coupled on-line to potentiometric stripping analysis providing a fast and sensitive method for analysis of Pb in urine samples. A microporous membrane liquid-liquid extraction (MMLLE) method was developed for the determination of organotin compounds in natural waters that reduced the number of manual steps involved in the LLE of organotin compounds prior to their CC separation. Clean extracts obtained after running unfiltered humic-rich river water samples through the MMLLE flow system allowed selective determination of all the organotin compounds in a single run using GC-MS in the selected ion monitoring mode (SIM) 171 refs, 9 figs, 4 tabs

  9. Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

    Science.gov (United States)

    Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko

    2016-04-01

    Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

  10. U(VI) extraction by 8-hydroxyquinoline. A comparison study in ionic liquid and in dichloromethane

    Energy Technology Data Exchange (ETDEWEB)

    Yuan, Li-Yong; Shi, Wei-Qun [Chinese Academy of Sciences, Beijing (China). Lab. of Nuclear Energy Chemistry; Liao, Xiang-Hong [Chinese Academy of Sciences, Beijing (China). Lab. of Nuclear Energy Chemistry; East China Institute of Technology, Nanchang (China). School of Nuclear Engineering and Geophysics; Liu, Zhi-Rong [East China Institute of Technology, Nanchang (China). School of Nuclear Engineering and Geophysics; Chai, Zhi-Fang [Chinese Academy of Sciences, Beijing (China). Lab. of Nuclear Energy Chemistry; Soochow Univ., Suzhou (China). School of Radiological and Interdisciplinary Sciences and Collaborative Innovation Center of Radiation Medicine

    2017-08-01

    Room temperature ionic liquids (RTILs) represent a recent new class of solvents with potential application in liquid/liquid extraction based nuclear fuel reprocessing due to their unique physical and chemical properties. The work herein provides a comparison of U(VI) extraction by 8-hydroxyquinoline (HOX) in a commonly used RTIL, i.e. 1-butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}mim][PF{sub 6}]) and in conventional solvent, i.e. dichloromethane (CH{sub 2}Cl{sub 2}). The effect of HOX concentration, solution acidity and nitrate ions on the extraction were discussed in detail, and the speciation analyses of the extracted U(VI) were performed. One of the main emphasis of this work is the extraction mechanism of U(VI) extracted from aqueous phase into RTILs and conventional solvent. In CH{sub 2}Cl{sub 2}, the extraction occurs through a combination of ion change and neutral complexation, and the extracted complex is proposed as UO{sub 2}(OX){sub 2}HOX. In [C{sub 4}mim][PF{sub 6}], although a cation-change mechanism as previously reported for RTILs-based system was involved, the extracted complex of UO{sub 2}(OX){sub 1.5}(HOX){sub 1.5}(PF6){sub 0.5} gave a clear indication that the usage of HOX as an acidic extractant markedly inhibited the solubility loss of [C{sub 4}mim][PF{sub 6}] during the extraction by leaching H{sup +} to aqueous phase. Moreover, the extracted U(VI) in [C{sub 4}mim][PF{sub 6}] can be easily stripped by using 0.01 M nitric acid, which provides a simple way of the ionic liquid recycling.

  11. Direct Sampling and Analysis from Solid Phase Extraction Cards using an Automated Liquid Extraction Surface Analysis Nanoelectrospray Mass Spectrometry System

    Energy Technology Data Exchange (ETDEWEB)

    Walworth, Matthew J [ORNL; ElNaggar, Mariam S [ORNL; Stankovich, Joseph J [ORNL; WitkowskiII, Charles E. [Protein Discovery, Inc.; Norris, Jeremy L [ORNL; Van Berkel, Gary J [ORNL

    2011-01-01

    Direct liquid extraction based surface sampling, a technique previously demonstrated with continuous flow and autonomous pipette liquid microjunction surface sampling probes, has recently been implemented as the Liquid Extraction Surface Analysis (LESA) mode on the commercially available Advion NanoMate chip-based infusion nanoelectrospray ionization system. In the present paper, the LESA mode was applied to the analysis of 96-well format custom solid phase extraction (SPE) cards, with each well consisting of either a 1 or 2 mm diameter monolithic hydrophobic stationary phase. These substrate wells were conditioned, loaded with either single or multi-component aqueous mixtures, and read out using the LESA mode of a TriVersa NanoMate or a Nanomate 100 coupled to an ABI/Sciex 4000QTRAPTM hybrid triple quadrupole/linear ion trap mass spectrometer and a Thermo LTQ XL linear ion trap mass spectrometer. Extraction conditions, including extraction/nanoESI solvent composition, volume, and dwell times, were optimized in the analysis of targeted compounds. Limit of detection and quantitation as well as analysis reproducibility figures of merit were measured. Calibration data was obtained for propranolol using a deuterated internal standard which demonstrated linearity and reproducibility. A 10x increase in signal and cleanup of micromolar Angiotensin II from a concentrated salt solution was demonstrated. Additionally, a multicomponent herbicide mixture at ppb concentration levels was analyzed using MS3 spectra for compound identification in the presence of isobaric interferences.

  12. Determination of pharmaceuticals in environmental and biological matrices using pressurised liquid extraction--are we developing sound extraction methods?

    DEFF Research Database (Denmark)

    Runnqvist, Hannah; Bak, Søren Alex; Hansen, Martin

    2010-01-01

    Pressurised liquid extraction (PLE) is now a well established and extensively applied extraction technique in environmental analysis for pollutants such as persistent organic pollutants (POPs). During the past decade, an emerging group of environmentally interesting analytes are pharmaceuticals...... that are continuingly released into the environment. This class is comprised with compounds of various properties. As the field of the analysis of these compounds grows, an increasing number of PLE methods for pharmaceuticals of varying quality are developed and published. This review summarises the critical PLE...... parameters during PLE method development and highlight them with examples from recently published papers utilising pressurised liquid extraction for the determination of pharmaceuticals in environmental and biological matrices. These recent methods are summarised and critically discussed with the aim...

  13. Influence of the ionic liquid cation on the solvent extraction of trivalent rare-earth ions by mixtures of Cyanex 923 and ionic liquids.

    Science.gov (United States)

    Rout, Alok; Binnemans, Koen

    2015-01-21

    Trivalent rare-earth ions were extracted from nitric acid medium by the neutral phosphine oxide extractant Cyanex 923 into ionic liquid phases containing the bis(trifluoromethylsulfonyl)imide anion. Five different cations were considered: 1-butyl-3-methylimidazolium, 1-decyl-3-methylimidazolium, methyltributylammonium, methyltrioctylammonium and trihexyl(tetradecyl)phosphonium. The extraction behavior of neodymium(iii) was investigated as a function of various parameters: pH, extractant concentration, concentration of the neodymium(iii) ion in the aqueous feed and concentration of the salting-out agent. The loading capacity of the ionic liquid phase was studied. The extraction efficiency increased with increasing pH of the aqueous feed solution. The extraction occurred for all ionic liquids via an ion-exchange mechanism and the extraction efficiency could be related to the solubility of the ionic liquid cation in the aqueous phase: high distribution ratios for hydrophilic cations and low ones for hydrophobic cations. Addition of nitrate ions to the aqueous phase resulted in an increase in extraction efficiency for ionic liquids with hydrophobic cations due to extraction of neutral complexes. Neodymium(iii) could be stripped from the ionic liquid phase by 0.5-1.0 M nitric acid solutions and the extracting phase could be reused. The extractability of other rare earths present in the mixture was compared for the five ionic liquids.

  14. Supervising Model of Independent Enterprise Group (Study of Community Development PT Badak NGL

    Directory of Open Access Journals (Sweden)

    Hermansyah Hermansyah

    2016-06-01

    Full Text Available This research aims to arrange an empowerment model of enterprise group through the program of Community Development in order to be independent and ready to compete, which is begun from the empirical study of the success of Cipta Busana Cooperative.. This research uses the descriptive analysis by using a case study on one enterprise supervised by PT Badak NGL that is Koperasi Cipta Busana (Kocibu. Kocibu is chosen to be the object of research due to its success to achieve the target to be the independent supervised enterprise in the fourth year. The data analysis method used in this research is the explorative analysis. Based on the research, there are some results such as that Kocibu is one of the supervised Micro, Small and Medium Enterprises of PT Badak NGL that could develop and be independent through several supporting programs. Some of key successes of Kocibu are as follows: a high commitment, a good leader, and intensive supervising programs. Besides, a good marketing system also contributes to the key of success. There are some aspects that naturally contribute to the Kocibu improvement and emerge naturally as follows: the leader figure and the high commitment from the stakeholders. While, the aspects emerged by design are: the supervising and training programs, the evaluation, the determination of rules, and the business targets. Hopefully, after this research has been conducted, the aspects appeared naturaly would be realized so early that the success of the public empowerment program will be able to increase. 

  15. TREES VEGETATION DIVERSITY IN PT ARUN NGL HOUSING, LHOKSEUMAWE, ACEH PROVINCE

    Directory of Open Access Journals (Sweden)

    Iqbar Iqbar

    2016-03-01

    Full Text Available The research about trees vegetation diversity in PT Arun NGL area had been done in December 2012. The objective of the research was to calculate the trees vegetation diversity index. The data had been collected in nine belt transects by length 400 m and  400 m2  (10 m x 40 m plots  for each belt transect. The collecting data was  including name of species, family, density, frequency and  dominancy.  The data was analyzed to get important value and diversity index. The result showed that there were 39 tree species belongs to 23 families found in the research area.  There were three dominant species namely; Pterocarpus indicus,  Pithecelobium dulce, dan Leucaena leucocephala which had higher important value than others species that lead  influencing the ecosystem. The trees diversity index in this area was about 3,3 which interpreted this area has high diversity index. Moreover, the plants were planted in PT Arun NGL Housing Area have another function as reducing pollutant material in the air.

  16. Ionic liquids for improving the extraction of NSAIDs in water samples using dispersive liquid-liquid microextraction by high performance liquid chromatography-diode array-fluorescence detection.

    Science.gov (United States)

    Toledo-Neira, Carla; Álvarez-Lueje, Alejandro

    2015-03-01

    A rapid, sensitive and efficient analytical method based on the use of ionic liquids for determination of non-steroidal anti-inflammatory drugs (NSAIDs) in water samples was developed. High-performance liquid chromatography equipped with a diode array and fluorescence detector was used for quantification of ketoprofen, ibuprofen and diclofenac in tap and river water samples. This new method relies on the use of two ionic liquids with multiple functionalities: one functions as an extraction solvent (1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM][PF6]), and the other changes the polarity in the aqueous medium (1-butyl-3-methylimidazolium tetrafluoroborate, ([BMIM][BF4]). Factors such as the type and volume of the ILs and dispersive solvent, sample volume, and centrifugation time were investigated and optimized. The optimized method exhibited good precision, with relative standard deviation values between 2% and 3%, for the three NSAIDs. Limits of detection achieved for all of the analytes were between 17 and 95 ng mL(-1), and the recoveries ranged from 89% to 103%. Furthermore, the enrichment factors ranged from 49 to 57. The proposed method was successfully applied to the analysis of NSAIDs in tap and river water samples.

  17. Combination of dispersive solid-phase extraction and salting-out homogeneous liquid-liquid extraction for the determination of organophosphorus pesticides in cereal grains.

    Science.gov (United States)

    Jia, Chunhong; Zhu, Xiaodan; Wang, Jihua; Zhao, Ercheng; He, Min; Chen, Li; Yu, Pingzhong

    2014-07-01

    A new analytical method for the determination of organophosphorus pesticides in cereal samples was developed by combining dispersive SPE (d-SPE) and salting-out homogeneous liquid-liquid extraction (SHLLE). The pesticides were first extracted from cereal grains with acetonitrile, followed by d-SPE cleanup. A 2 mL aliquot of the extract was then added to a centrifuge tube containing 9.2 mL water and 3.3 g NaCl for SHLLE. Analysis of the extract was carried out by gas chromatography coupled with flame photometric detection. The d-SPE procedure effectively provides the necessary cleanup of the extract while SHLLE is used as an efficient concentration technique. Experimental parameters influencing the extraction efficiency including amounts of added water and salt were investigated. Recovery studies were carried out at three fortification levels, yielding recoveries in the range of 57.7-98.1% with the RSD from 3.7 to 10.9%. The reported limits of determination obtained from this study were 1 μg/kg, which is better than the conventional methods. In the analysis of 40 wheat and corn samples taken from Beijing suburbs, only two wheat samples have chlorpyrifos residue over the limits of determination.

  18. Enrichment of antioxidant compounds from lemon balm (Melissa officinalis) by pressurized liquid extraction and enzyme-assisted extraction.

    Science.gov (United States)

    Miron, T L; Herrero, M; Ibáñez, E

    2013-05-03

    In this work enzyme-assisted extraction (EAE) and pressurized liquid extraction (PLE) are applied for extraction of natural compounds from lemon balm (Melissa officinalis). Cellulase, endo-β-1,4 xylanase and pectinase were studied in order to degrade cell wall of lemon balm leaves and to release phenolic compounds. On the other hand, in order to compare the performance obtained with EAE, PLE using water and ethanol was employed maintaining 150°C as extraction temperature. The obtained extracts were characterized in terms of antioxidant capacity by using DPPH (1,1-diphenyl-2-picrylhydrazyl) radical scavenging and trolox equivalent antioxidant capacity (TEAC) in vitro assays, whereas the Folin-Ciocalteu procedure was employed to estimate the total phenols content. On the other hand, extracts were chemically characterized by liquid chromatography tandem mass spectrometry (LC-MS/MS). The results showed that EAE enhanced the total phenolic content and the antioxidant capacity compared to a non-enzymatic control. PLE extracts presented higher amount of phenols and antioxidant capacity than enzyme-assisted extracts, reaching the highest values on water extracts (193.18mggallicacid/gextract and EC50=6.81μg/mL). Among the bioactive phenolic compounds identified in lemon balm, rosmarinic acid was the main component, although other important compounds were also identified, such as caffeic acid derivatives (salvianolic acids, lithospermic acid) and rosmarinic acid derivatives (rosmarinic acid hexoside, sagerinic acid, sulfated rosmarinic acid). The present study confirms that EAE and PLE can be considered alternative methods for the extraction of natural compounds with biological activity from natural sources. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Miniaturized salting-out liquid-liquid extraction in a coupled-syringe system combined with HPLC-UV for extraction and determination of sulfanilamide.

    Science.gov (United States)

    Sereshti, Hassan; Khosraviani, Marzieh; Sadegh Amini-Fazl, Mohammad

    2014-04-01

    In salting-out liquid-liquid extraction (SALLE) technique, water-miscible organic solvents are used for extraction of polar analytes from saline solutions. In this study, for the first time, a coupled 1-mL syringes system was utilized to perform a miniaturized SALLE method. Sulfanilamide antibiotic was extracted and determined via the developed method followed by high performance liquid chromatography-ultraviolet detection (HPLC-UV). The extraction process was carried out by rapid shooting of acetonitrile as extraction solvent (syringe B) into saline aqueous sample solution (syringe A), and then the shooting was repeated several times at a rate of 1 cycles(-1). Thereby, an extremely large contact surface area was created between phases and led to a rapid equilibrium and mass transfer. In order to improve the efficiency of the method, the effect of extraction solvent (type and volume), shooting times, salt concentration, and pH on the extraction efficiency was investigated. The best performance of the method was achieved with 250 µL of acetonitrile, salt concentration of 250 mg mL(-1), pH of 7, and shooting times of 5. The linear dynamic range was 0.001-10 µg mL(-1) with the determination coefficient of 0.9999. The relative standard deviation (RSD; n=3, C=5 µg mL(-1)), and the limit of detection (LOD) were 1.55% and 0.3 ng mL(-1), respectively. The developed technique was successfully applied to genuine samples of tea, water, milk, honey, human urine, plasma and blood.

  20. Application of ionic liquid for extraction and separation of bioactive compounds from plants.

    Science.gov (United States)

    Tang, Baokun; Bi, Wentao; Tian, Minglei; Row, Kyung Ho

    2012-09-01

    In recent years, ionic liquids (ILs), as green and designer solvents, have accelerated research in analytical chemistry. This review highlights some of the unique properties of ILs and provides an overview of the preparation and application of IL or IL-based materials to extract bioactive compounds in plants. IL or IL-based materials in conjunction with liquid-liquid extraction (LLE), ultrasonic-assisted extraction (UAE), microwave-assisted extraction (MAE), high performance liquid chromatography (HPLC) and solid-phase extraction (SPE) analytical technologies etc., have been applied successfully to the extraction or separation of bioactive compounds from plants. This paper reviews the available data and references to examine the advantages of IL and IL-based materials in these applications. In addition, the main target compounds reviewed in this paper are bioactive compounds with multiple therapeutic effects and pharmacological activities. Based on the importance of the targets, this paper reviews the applications of ILs, IL-based materials or co-working with analytical technologies. The exploitation of new applications of ILs on the extraction of bioactive compounds from plant samples is expected to increase.

  1. Optimal Extraction of Gallic Acid from Suaeda glauca Bge. Leaves and Enhanced Efficiency by Ionic Liquids

    Directory of Open Access Journals (Sweden)

    Xin-Hong Wang

    2016-01-01

    Full Text Available The ultrasound-assisted extraction (UAE was initially applied to extract gallic acid from Suaeda glauca Bge. using 70% ethanol as extraction solvent. Temperature, liquid-solid ratio, and extraction time were optimized by response surface methodology (RSM, obtaining maximum levels of gallic acid (6.30 mg·g−1 at 51°C, 19.52 mL·g−1, and 42.68 min, respectively. The obtained model was statistically significant (p<0.0001. The verification experiments at the optimum conditions yielded gallic acid for 6.21 mg·g−1. Subsequently, under optimal conditions, four ionic liquids were used to extract gallic acid from Suaeda glauca Bge. The results indicated that the presence of 1-hexyl-3-methylimidazolium chloride allowed increasing the EE of gallic acid up to 8.90 mg·g−1. This might be interpreted in terms of the molecular interaction between ionic liquid and gallic acid. The use of ionic liquids involves a stronger gallic acid extraction capacity than conventional organic volatile solvents. A promising alternative process is proposed for the extraction of gallic acid of Suaeda glauca Bge.

  2. Development of an Analytical Method Based on Temperature Controlled Solid-Liquid Extraction Using an Ionic Liquid as Solid Solvent

    Directory of Open Access Journals (Sweden)

    Zhongwei Pan

    2015-12-01

    Full Text Available At the present paper, an analytical method based on temperature controlled solid-liquid extraction (TC-SLE utilizing a synthesized ionic liquid, (N-butylpyridinium hexafluorophosphate, [BPy]PF6, as solid solvent and phenanthroline (PT as an extractant was developed to determine micro levels of Fe2+ in tea by PT spectrophotometry. TC-SLE was carried out in two continuous steps: Fe2+ can be completely extracted by PT-[BPy]PF6 or back-extracted at 80 °C and the two phases were separated automatically by cooling to room temperature. Fe2+, after back-extraction, needs 2 mol/L HNO3 as stripping agent and the whole process was determined by PT spectrophotometry at room temperature. The extracted species was neutral Fe(PTmCl2 (m = 1 according to slope analysis in the Fe2+-[BPy]PF6-PT TC-SLE system. The calibration curve was Y = 0.20856X − 0.000775 (correlation coefficient = 0.99991. The linear calibration range was 0.10–4.50 μg/mL and the limit of detection for Fe2+ is 7.0 × 10−2 μg/mL. In this method, the contents of Fe2+ in Tieguanyin tea were determined with RSDs (n = 5 3.05% and recoveries in range of 90.6%–108.6%.

  3. Alkaline extraction of polonium from liquid lead bismuth eutectic

    Science.gov (United States)

    Heinitz, S.; Neuhausen, J.; Schumann, D.

    2011-07-01

    The production of highly radiotoxic polonium isotopes poses serious safety concerns for the development of future nuclear systems cooled by lead bismuth eutectic (LBE). In this paper it is shown that polonium can be extracted efficiently from LBE using a mixture of alkaline metal hydroxides (NaOH + KOH) in a temperature range between 180 and 350 °C. The extraction ratio was analyzed for different temperatures, gas blankets and phase ratios. A strong dependence of the extraction performance on the redox properties of the cover gas was found. While hydrogen facilitates the removal of polonium, oxygen has a negative influence on the extraction. These findings open new possibilities to back up the safety of future LBE based nuclear facilities.

  4. Aluminium sensitized spectrofluorimetric determination of fluoroquinolones in milk samples coupled with salting-out assisted liquid-liquid ultrasonic extraction

    Science.gov (United States)

    Xia, Qinghai; Yang, Yaling; Liu, Mousheng

    2012-10-01

    An aluminium sensitized spectrofluorimetric method coupled with salting-out assisted liquid-liquid ultrasonic extraction for the determination of four widely used fluoroquinolones (FQs) namely norfloxacin (NOR), ofloxacin (OFL), ciprofloxacin (CIP) and gatifloxacin (GAT) in bovine raw milk was described. The analytical procedure involves the fluorescence sensitization of aluminium (Al3+) by complexation with FQs, salting-out assisted liquid-liquid ultrasonic extraction (SALLUE), followed by spectrofluorometry. The influence of several parameters on the extraction (the salt species, the amount of salt, pH, temperature and phase volume ratio) was investigated. Under optimized experimental conditions, the detection limits of the method in milk varied from 0.009 μg/mL for NOR to 0.016 μg/mL for GAT (signal-to-noise ratio (S/N) = 3). The relative standard deviations (RSD) values were found to be relatively low (0.54-2.48% for four compounds). The calibration graph was linear from 0.015 to 2.25 μg/mL with coefficient of determinations not less than 0.9974. The methodology developed was applied to the determination of FQs in bovine raw milk samples. The main advantage of this method is simple, accurate and green. The method showed promising applications for analyzing polar analytes especially polar drugs in various sample matrices.

  5. Recovery of zinc and manganese from spent alkaline batteries by liquid-liquid extraction with Cyanex 272

    Science.gov (United States)

    Salgado, Aline L.; Veloso, Aline M. O.; Pereira, Daniel D.; Gontijo, Glayson S.; Salum, Adriane; Mansur, Marcelo B.

    A hydrometallurgical route based on the liquid-liquid extraction technique using Cyanex 272 as extractant is investigated for the selective separation of metal values, in particular, zinc and manganese from spent alkaline batteries. The recycling route consists of following steps: (1) cryogenic dismantling of the spent batteries, (2) pre-treatment of the internal material consisting of drying, grinding and screening steps in order to produce a dry homogeneous powder, (3) leaching of the powder with sulphuric acid and (4) metal separation by liquid-liquid extraction. Bench scale experiments have shown that zinc and manganese are easily separated (ΔpH 1/2≈2.0) using 20% (v/v) Cyanex 272 dissolved in Escaid 110 at 50 °C. Therefore, the proposed route can treat residues from both zinc-carbon and alkaline batteries because metal composition of these batteries is quite similar. The metal content of other batteries such as Ni-Cd and nickel-metal hydride (NiMH) has been also determined in order to include them in future investigations.

  6. Development of a new sample preparation method based on liquid-liquid-liquid extraction combined with dispersive liquid-liquid microextraction and its application on unfiltered samples containing high content of solids.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Abbaspour, Maryam

    2017-11-01

    A new sample preparation method based on liquid-liquid-liquid extraction combined with dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection has been reported for the extraction/preconcentration and determination of trace levels of twelve pesticide residues from different samples with high content of solids without filtration. This method consists of a three-phase system including an aqueous phase (sample solution), acetonitrile, and hexane. The extraction mechanism is based on different affinities of the substances from the sample matrices towards each of the involved phase, which provides a high selectivity to the process. In other words, interfering hydrophobic compounds are transferred into hexane and will not be present in the final extract. Furthermore, ionic and polar compounds are retained in the aqueous phase. Therefore, only semi-polar compounds such as the studied pesticides are extracted into acetonitrile. In this method, a homogeneous solution of the aqueous phase and acetonitrile (a water-soluble extraction solvent) forms two clearly separated phases in the presence of sodium sulfate (as a phase separation agent) and simultaneously the analytes are extracted into the fine droplets of the acetonitrile collected on the surface of the aqueous phase. To achieve high enrichment factors, the acetonitrile phase is mixed with 1,2-dibromoethane (as a preconcentration solvent) at µL-level to perform the following dispersive liquid-liquid microextraction procedure. Several parameters that can affect extraction efficiency including kind and volume of extraction solvent, type and concentration of phase separation agent, hexane volume, kind of preconcentration solvent, and ionic strength were studied and optimized. Under the optimal conditions, extraction recoveries were obtained in the range of 53-93% and the calibration curves were linear in wide ranges with correlation coefficients ≥ 0.9983. Intra- (n = 6) and

  7. Application of ionic liquid-based microwave-assisted extraction of flavonoids from Scutellaria baicalensis Georgi.

    Science.gov (United States)

    Zhang, Qin; Zhao, San-Hu; Chen, Jue; Zhang, Li-Wei

    2015-10-01

    In the present work, a rapid ionic liquid-based microwave-assisted extraction (ILMAE) method was successfully applied to simultaneous extraction of baicalin, wogonoside, baicalein and wogonin from Scutellaria baicalensis Georgi. A series of 1-alkyl-3-methylirnidazolium ionic liquids with different anions and cations were assessed for extraction efficiency, and 1-octyl-3-methylimidazolium bromide was selected as the optimal solvent. In addition, the parameters of ILMAE procedure for the four flavonoids were optimized, and the optimal ILMAE method was validated in the linearity, stability, precision and recovery. Meanwhile, the microstructures of S. baicalensis powders were observed before and after extraction with the help of a scanning electron microscope (SEM) in order to explore the extraction mechanism, and the activity of the crude enzyme solution from S. baicalensis was determined through the hydrolysis of baicalin. Finally, the extraction yields and extraction time of WaterHRE, WaterMAE, ILHRE and Chp were 5.18% (30min), 8.77% (90s), 16.94% (30min) and 18.58% (3h), respectively. The results indicated that compared with the conventional extraction approaches, ILMAE possessed great advantages in extracting flavonoids, such as the highest extraction yield (22.28%), the shortest extraction time (90s), etc.

  8. Ionic liquids based microwave-assisted extraction of lichen compounds with quantitative spectrophotodensitometry analysis.

    Science.gov (United States)

    Bonny, Sarah; Paquin, Ludovic; Carrié, Daniel; Boustie, Joël; Tomasi, Sophie

    2011-11-30

    Ionic liquids based extraction method has been applied to the effective extraction of norstictic acid, a common depsidone isolated from Pertusaria pseudocorallina, a crustose lichen. Five 1-alkyl-3-methylimidazolium ionic liquids (ILs) differing in composition of alkyl chain and anion were investigated for extraction efficiency. The extraction amount of norstictic acid was determined after recovery on HPTLC with a spectrophotodensitometer. The proposed approaches (IL-MAE and IL-heat extraction (IL-HE)) have been evaluated in comparison with usual solvents such as tetrahydrofuran in heat-reflux extraction and microwave-assisted extraction (MAE). The results indicated that both the characteristics of the alkyl chain and anion influenced the extraction of polyphenolic compounds. The sulfate-based ILs [C(1)mim][MSO(4)] and [C(2)mim][ESO(4)] presented the best extraction efficiency of norstictic acid. The reduction of the extraction times between HE and MAE (2 h-5 min) and a non-negligible ratio of norstictic acid in total extract (28%) supports the suitability of the proposed method. This approach was successfully applied to obtain additional compounds from other crustose lichens (Pertusaria amara and Ochrolechia parella).

  9. Extraction of aromatics from naphtha with ionic liquids

    NARCIS (Netherlands)

    Meindersma, G.W.

    2005-01-01

    The objective of this study was the development of a separation technology for the selective recovery and purification of aromatic compounds benzene, toluene, ethylbenzene and xylenes (BTEX) from liquid ethylene cracker feeds. Most ethylene cracker feeds contain 10 ¿ 25% of aromatic components,

  10. An AIL/IL-based liquid/liquid extraction system for the purification of His-tagged proteins.

    Science.gov (United States)

    Xu, Weiyuan; Cao, Huazhen; Ren, Guangwei; Xie, Hujun; Huang, Jianying; Li, Shijun

    2014-06-01

    A sorbent based on affinity ionic liquid (AIL), triazacyclononane-ionic liquid, was synthesized, characterized, and applied to the extraction of histidine (His)-tagged proteins from aqueous buffer to ionic liquid (IL) phase. The adsorbed His-tagged proteins could be back-extracted from the IL phase to the aqueous buffer with an imidazole solution. The specific binding of His-tagged proteins with AIL/IL could be affected by a few factors including the ionic strength and coordinated metal ions. In the case of His-tagged enhanced green fluorescent protein (EGFP), the maximum binding capacity of Cu(2+)-AIL/IL reached 2.58 μg/μmol under the optimized adsorption conditions. The eluted His-tagged EGFP kept fluorescent and remained active through the purification process. Moreover, a tandem extraction process successively using Cu(2+)-AIL/IL and Zn(2+)-AIL/IL systems was developed, which was proven very efficient to obtain the ultimate protein with a purity of about 90 %. An effective reclamation method for the AIL/IL extraction system was further established. The sorbent could be easily regenerated by removing metal ions with EDTA and the followed reimmobilization of metal ions. Easy handling of the presented M(2+)-AIL/IL system and highly specific ability to absorb His-tagged proteins make it attractive and potentially applicable in biomolecular separation.

  11. Optimization and validation of liquid-liquid extraction with low temperature partitioning for determination of carbamates in water

    Energy Technology Data Exchange (ETDEWEB)

    Machado Goulart, Simone; Domingos Alves, Renata; Neves, Antonio Augusto; Queiroz, Jose Humberto de; Conde de Assis, Tamires [Departamento de Quimica, Universidade Federal de Vicosa, Vila Gianetti, Casa 24, 36 570-000 Vicosa, MG (Brazil); Queiroz, Maria Eliana L.R. de, E-mail: meliana@ufv.br [Departamento de Quimica, Universidade Federal de Vicosa, Vila Gianetti, Casa 24, 36 570-000 Vicosa, MG (Brazil)

    2010-06-25

    Using a 2{sup 3} experimental design, liquid-liquid extraction with low temperature partitioning (LLE-LTP) was optimized and validated for analysis of three carbamates (aldicarb, carbofuran and carbaryl) in water samples. In this method, 2.0 mL of sample is placed in contact with 4.0 mL of acetonitrile. After agitation, the sample is placed in a freezer for 3 h for phase separation. The organic extract is analyzed by high performance liquid chromatography with ultraviolet detection (HPLC-UV). For validation of the technique, the following figures of merit were evaluated: accuracy, precision, detection and quantification limits, linearity, sensibility and selectivity. Extraction recovery percentages of the carbamates aldicarb, carbofuran and carbaryl were 90%, 95% and 96%, respectively. Even though extremely low volumes of sample and solvent were used, the extraction method was selective and the detection and quantification limits were between 5.0 and 10.0 {mu}g L{sup -1}, and 17.0 and 33.0 {mu}g L{sup -1}, respectively.

  12. Rapid extraction and determination of amphetamines in human urine samples using dispersive liquid-liquid microextraction and solidification of floating organic drop followed by high performance liquid chromatography.

    Science.gov (United States)

    Ahmadi-Jouibari, Toraj; Fattahi, Nazir; Shamsipur, Mojtaba

    2014-06-01

    A novel, rapid, simple and sensitive dispersive liquid-liquid microextraction method based on the solidification of floating organic drop (DLLME-SFO) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was used to determine amphetamine and methamphetamine in urine samples. The factors affecting the extraction efficiency of DLLME-SFO such as the kind and volume of the extraction and the disperser solvents, effect of concentration of K2CO3 and extraction time were investigated and the optimal extraction conditions were established. Under the optimum conditions (extraction solvent: 30.0μl 1-undecanol; disperser solvent: 300μl acetonitrile; buffer concentration: 2% (w/v) K2CO3 and extraction time: 1min), calibration curves are linear in the range of 10-3000μgl(-1) and limit of detections (LODs) are in the range of 2-8μgl(-1). The relative standard deviations (RSDs) for 100μgl(-1) of amphetamine and methamphetamine in diluted urine are in the range of 6.2-7.8% (n=7). The method was successfully applied for the determination of amphetamine and methamphetamine in the actual urine samples. The relative recoveries of urine samples spiked with amphetamine and methamphetamine are 87.8-113.2%. The obtained results show that DLLME-SFO combined with HPLC-UV is a fast and simple method for the determination of amphetamine and methamphetamine in urine.

  13. Optimization of pressurized liquid extraction of carotenoids and chlorophylls from Chlorella vulgaris.

    Science.gov (United States)

    Cha, Kwang Hyun; Lee, Hee Ju; Koo, Song Yi; Song, Dae-Geun; Lee, Dong-Un; Pan, Cheol-Ho

    2010-01-27

    Pressurized liquid extraction (PLE) was applied to the extraction of carotenoids and chlorophylls from the green microalga Chlorella vulgaris. Four extraction techniques such as maceration (MAC), Soxhlet extraction (SOX), ultrasound assisted extraction (UAE), and PLE were compared, and both the extraction temperature (50, 105, and 160 degrees C) and the extraction time (8, 19, and 30 min), which are the two main factors for PLE, were optimized with a central composite design to obtain the highest extraction efficiency. The extraction solvent (90% ethanol/water) could adequately extract the functional components from C. vulgaris. PLE showed higher extraction efficiencies than MAC, SOX, and UAE. Temperature was the key parameter having the strongest influence on the extraction of carotenoids and chlorophylls from chlorella. In addition, high heat treatment (>110 degrees C) by PLE minimized the formation of pheophorbide a, a harmful chlorophyll derivative. These results indicate that PLE may be a useful extraction method for the simultaneous extraction of carotenoids and chlorophylls from C. vulgaris.

  14. Novel materials and methods for solid-phase extraction and liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Ambrose, Diana [Iowa State Univ., Ames, IA (United States)

    1997-06-24

    This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

  15. Actinide ion extraction using room temperature ionic liquids: opportunities and challenges for nuclear fuel cycle applications.

    Science.gov (United States)

    Mohapatra, Prasanta Kumar

    2017-02-14

    Studies on the extraction of actinide ions from radioactive feeds have great relevance in nuclear fuel cycle activities, mainly in the back end processes focused on reprocessing and waste management. Room temperature ionic liquid (RTIL) based diluents are becoming increasingly popular due to factors such as more efficient extraction vis-à-vis molecular diluents, higher metal loading, higher radiation resistance, etc. The fascinating chemistry of the actinide ions in RTIL based solvent systems due to complex extraction mechanisms makes it a challenging area of research. By the suitable tuning of the cationic and anionic parts of the ionic liquids, their physical properties such as density, dielectric constant and viscosity can be changed which are considered key parameters in metal ion extraction. Aqueous solubility of the RTILs, which can lead to significant loss in the solvent inventory, can be avoided by appending the extractant moieties onto the ionic liquid. While the low vapour pressure and non-flammability of the ionic liquids make them appear as 'green' diluents, their aqueous solubility raises concerns of environmental hazards. The present article gives a summary of studies carried out on actinide ion extraction and presents perspectives of its applications in the nuclear fuel cycle. The article discusses various extractants used for actinide ion extraction and at many places, comparison is made vis-à-vis molecular diluents which includes the nature of the extracted species and the mechanism of extraction. Results of studies on rare earth elements are also included in view of their similarities with the trivalent minor actinides.

  16. Graphene based solid phase extraction combined with ultra high performance liquid chromatography-tandem mass spectrometry for carbamate pesticides analysis in environmental water samples.

    Science.gov (United States)

    Shi, Zhihong; Hu, Junda; Li, Qi; Zhang, Shulan; Liang, Yuhuan; Zhang, Hongyi

    2014-08-15

    In this paper, graphene, a new sorbent material, was synthesized and used for solid-phase extraction (SPE) of the six carbamate pesticides (pirimicarb, baygon, carbaryl, isoprocarb, baycarb and diethofencarb) in environmental water samples. The target analytes can be extracted on the graphene-packed SPE cartridge, and then eluted with acetone. The eluate was collected and dried by high purity nitrogen gas at room temperature. 1mL of 20% (v/v) acetonitrile aqueous solution was used to redissolve the residue. The final sample solution was analyzed by ultra performance liquid chromatography-tandem quadrupole mass spectrometry (UPLC-MS/MS) system. Under optimum conditions, good linearity was obtained for the carbamates with correlation coefficient in the range of 0.9992-0.9998. The limits of detection (S/N=3) for the six carbamate pesticides were in the range of 0.5-6.9ngL(-1). Relative standard deviations (RSD) for five replicate determinations were below 5.54%. RSD values for cartridge-to-cartridge precision (n=7) were in the range of 1.27-8.13%. After proper regeneration, the graphene-packed SPE cartridge could be re-used over 100 times for standard solution without significant loss of performance. The enrichment factors for the target analytes were in the range of 34.2-51.7. The established method has been successfully applied to the determination of carbamate pesticide residues in environmental water samples such as river water, well water and lake water. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Optimization of pressurized liquid extraction of inositols from pine nuts (Pinus pinea L.).

    Science.gov (United States)

    Ruiz-Aceituno, L; Rodríguez-Sánchez, S; Sanz, J; Sanz, M L; Ramos, L

    2014-06-15

    Pressurized liquid extraction (PLE) has been used for the first time to extract bioactive inositols from pine nuts. The influence of extraction time, temperature and cycles of extraction in the yield and composition of the extract was studied. A quadratic lineal model using multiple linear regression in the stepwise mode was used to evaluate possible trends in the process. Under optimised PLE conditions (50°C, 18 min, 3 cycles of 1.5 mL water each one) at 10 MPa, a noticeable reduction in extraction time and solvent volume, compared with solid-liquid extraction (SLE; room temperature, 2h, 2 cycles of 5 mL water each one) was achieved; 5.7 mg/g inositols were extracted by PLE, whereas yields of only 3.7 mg/g were obtained by SLE. Subsequent incubation of PLE extracts with Saccharomyces cerevisiae (37°C, 5h) allowed the removal of other co-extracted low molecular weight carbohydrates which may interfere in the bioactivity of inositols.

  18. Focused ultrasound solid-liquid extraction and selective pressurised liquid extraction to determine bisphenol A and alkylphenols in sewage sludge by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Martínez-Moral, María P; Tena, María T

    2011-09-01

    A new method for determining endocrine disrupter compounds (EDCs) in sewage sludge is described in this paper. EDCs studied were bisphenol A (BPA) and alkylphenols (APs). In order to obtain a fast and simple method, selective pressurised liquid extraction (SPLE) and focused ultrasound solid-liquid extraction (FUSLE) were tested. Best results for SPLE were obtained using Florisil as clean-up sorbent and dichloromethane as extraction solvent, while temperature was the only significant variable. Analyte extraction by SPLE was completed in only one extraction cycle of 1 min at 130 °C. FUSLE was carried out in one step of 20 s at 75% power (0.5 cycles) and with 8 mL of ethyl acetate. Although the optimised FUSLE process was faster, simpler and cheaper, SPLE provided higher recovery values (ranging from 81 to 105%) and therefore SPLE-based method was selected and validated. The SPLE and GC-MS method showed an LOD of 10.7 ng/g for BPA and LODs between 1.2 and 41.6 ng/g for APs. Relative standard deviation values lower than 6% were obtained for all analytes. As a result, an efficient, fast and simple method based on SPLE and GC-MS for the determination of BPA and APs in sewage sludge is proposed.

  19. Microstructure-Enhanced Liquid–Liquid Extraction in a Real-Time Fluorescence Detection Microfluidic Chip

    Directory of Open Access Journals (Sweden)

    Penghui Xiong

    2016-03-01

    Full Text Available Microfluidic system is widely employed in the detection of environmental contaminants and biological specimens. One of the critical issues which limits the applications of microfluidic chips is the limit of detection of trace specimens. Liquid–liquid extraction is of great importance in the preprocessing in microfluidic devices. In this paper, we developed a real-time fluorescence detection microfluidic chip combined with a microstructure-enhanced liquid–liquid laminar extraction technique, which concentrated the trace compound and realized real-time monitoring. Auxiliary microstructures integrated in the microfluidic chip were applied to increase the extraction efficiency, which was proved by the FEM (finite element method simulation as well. A common fluorescence probe, Rhodamine 6G (Rh6g, was used in the experiment to demonstrate the performance of the microfluidic system. It revealed that the liquid–liquid laminar extraction combined with auxiliary microstructures of a cross shape was an effective method for enrichment. The efficiency of microstructure-enhanced liquid–liquid extraction was increased by 350% compared to the traditional laminar flow extraction.

  20. Liquid CO2 extraction of Jasminum grandiflorum and comparison with conventional processes.

    Science.gov (United States)

    Prakash, Om; Sahoo, Deeptanjali; Rout, Prasant Kumar

    2012-01-01

    The concrete (0.35%) of Jasminum grandiflorum L. flowers was prepared by extraction in n-pentane, and the absolute (0.27%) by fractionation of the n-pentane extract (concrete) with cold methanol. Direct extraction of flowers with liquid CO2 gave a relatively fat-free product in 0.26% yield. The liquid CO2 extract was enriched with terpenoids and benzenoids, thus providing the organoleptically accepted product. The major compounds, such as benzyl acetate, (E,E)-alpha-farnesene and (Z)-3-hexenyl benzoate, along with compounds like indole, methyl anthranilate, (Z)-jasmone, (Z)-methyl jasmonoate and (Z)-methyl epi-jasmonoate, are responsible for the high diffusivity of the jasmine fragrance. These compounds have been obtained with improved recoveries in the liquid CO2 extract. On the other hand, the yield of the essential oil was poor (0.05%), and some polar compounds (oxygenated terpenoids) were recovered in less amounts in comparison with either the n-pentane or liquid CO2 extract.

  1. On-line high speed lipid extraction for nanoflow liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Lee, Ju Yong; Yang, Joon Seon; Park, Se Mi; Byeon, Seul Kee; Moon, Myeong Hee

    2016-09-16

    An on-line lipid extraction method is introduced by utilizing a short capillary extraction column using HILIC and C4 particles prior to nanoflow liquid chromatography-tandem mass spectrometry (nLC-MS/MS). The on-line extraction using a urine sample spiked with PL standards showed similar or slightly higher recovery values (86%-96%) of phospholipids (PLs) compared to those obtained by the conventional off-line extraction based on the Folch method with or without using the air-exposed drying process. In this study, we demonstrated that PL oxidation can occur during the air-exposed drying process of lipid extracts in standard liquid-liquid extraction procedures, which was confirmed by the oxidized PL (OxPL) molecules that were generated from an off-line extraction using a few PL standards. Quantitative comparison of these OxPL species between on- and off-line extraction followed by nLC-MS/MS with multiple reaction monitoring (MRM) analysis showed a significant decrease (2-10 fold) in unwanted OxPL species when on-line extraction was employed. While the number of identified PLs from a urine sample was somewhat lower than those by off-line extraction, the number of OxPLs was significantly reduced (from 70 to 22) with on-line extraction. The new method offers high speed (∼5min) automated extraction of PLs with nLC-MS/MS analysis and presents the possibility of handling a biological sample with a very limited amount of lipids.

  2. High-throughput salting-out-assisted homogeneous liquid-liquid extraction with acetonitrile for determination of baicalin in rat plasma with high-performance liquid chromatography.

    Science.gov (United States)

    Li, Tingting; Zhang, Lei; Tong, Ling; Liao, Qiongfeng

    2014-05-01

    Baicalin is the main indicator for qualitative and quantitative analysis of Scutellaria baicalensis Georgi and its prescription in vivo and in vitro. Owing to its insolubility and instability, the analysis of baicalin in biological samples is analytically challenging. Although there have been many pharmacokinetic or metabolism studies on baicalin, the current reported sample pretreatment methods are not the optimal choice with regard to absolute recovery and operation procedure. Here we report a high-throughput salting-out-assisted homogeneous liquid-liquid extraction method with acetonitrile and ammonium sulfate. Eight kinds of commonly used salts, preferred salt concentration and auxiliary solvents were investigated. The extraction efficiency in the presence of ammonium salt and auxiliary solvent (methanol) in comparison to that from the salt-free aqueous increased to above 90%. The performance of the developed pretreatment method was further evaluated through testing specificity, linearity, precision, accuracy, extraction recovery and stability. In particular, the stability investigation results proved that the operation at low temperature would no longer necessary be for salting-out-assisted homogeneous liquid-liquid extraction compared with protein precipitation, and the pretreatment method would be valuable if the compounds were unstable within matrices.

  3. Liquid-Liquid Equilibrium data for mono ethylene glycol extraction from water with the new ionic liquid tetraoctyl ammonium 2-methyl-1-naphtoate as solvent

    NARCIS (Netherlands)

    Garcia Chavez, L.Y.; Schuur, Boelo; de Haan, A.B.

    2012-01-01

    Thermal recovery of mono ethylene glycol (MEG) from aqueous streams is one of the most energy demanding operations in industry, because of the large amount of water that needs to be evaporated. The use of alternative technologies such as liquid–liquid extraction could save energy. A new tailor made

  4. Feasibility of corona discharge ion mobility spectrometry for direct analysis of samples extracted by dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Jafari, Mohammad T; Riahi, Farhad

    2014-05-23

    The capability of corona discharge ionization ion mobility spectrometry (CD-IMS) for direct analysis of the samples extracted by dispersive liquid-liquid microextraction (DLLME) was investigated and evaluated, for the first time. To that end, an appropriate new injection port was designed and constructed, resulting in possibility of direct injection of the known sample volume, without tedious sample preparation steps (e.g. derivatization, solvent evaporation, and re-solving in another solvent…). Malathion as a test compound was extracted from different matrices by a rapid and convenient DLLME method. The positive ion mobility spectra of the extracted malathion were obtained after direct injection of carbon tetrachloride or methanol solutions. The analyte responses were compared and the statistical results revealed the feasibility of direct analysis of the extracted samples in carbon tetrachloride, resulting in a convenient methodology. The coupled method of DLLME-CD-IMS was exhaustively validated in terms of sensitivity, dynamic range, recovery, and enrichment factor. Finally, various real samples of apple, river and underground water were analyzed, all verifying the feasibility and success of the proposed method for the easy extraction of the analyte using DLLME separation before the direct analysis by CD-IMS.

  5. Parallel artificial liquid membrane extraction of acidic drugs from human plasma.

    Science.gov (United States)

    Roldán-Pijuán, Mercedes; Pedersen-Bjergaard, Stig; Gjelstad, Astrid

    2015-04-01

    The new sample preparation concept "Parallel artificial liquid membrane extraction (PALME)" was evaluated for extraction of the acidic drugs ketoprofen, fenoprofen, diclofenac, flurbiprofen, ibuprofen, and gemfibrozil from human plasma samples. Plasma samples (250 μL) were loaded into individual wells in a 96-well donor plate and diluted with HCl to protonate the acidic drugs. The acidic drugs were extracted as protonated species from the individual plasma samples, through corresponding artificial liquid membranes each comprising 2 μL of dihexyl ether, and into corresponding acceptor solutions each comprising 50 μL of 25 mM ammonia solution (pH 10). The liquid membranes and the acceptor solutions were located in a 96-well filter plate, which was sandwiched with the 96-well donor plate during extraction. Parallel extraction of several samples was performed for 15 to 60 min, followed by high-performance liquid chromatography-ultraviolet detection of the individual acceptor solutions. Important PALME parameters including the chemical composition of the liquid membrane, extraction time, and sample pH were optimized, and the extraction performance was evaluated. Except for flurbiprofen, exhaustive extraction was accomplished from plasma. Linearity was obtained for all six drugs in the range 0.025-10 μg/mL, with r (2) values ranging between 0.998 and 1.000. Precision data were in the range 3-22% RSD, and accuracy data were within 72-130% with spiked plasma samples. Based on the current experiences, PALME showed substantial potential for future high-throughput bioanalysis of non-polar acidic drugs.

  6. Extraction of Lutein Diesters from Tagetes Erecta using Supercritical CO2 and Liquid Propane.

    Science.gov (United States)

    Skerget, Mojca; Bezjak, Miran; Makovšek, Katja; Knez, Zeljko

    2010-03-01

    The efficiency of high pressure extraction of lutein diesters from marigold (Tagetes erecta) flower petals has been investigated. The solvents used for extraction were supercritical carbon dioxide and liquid propane. Operating parameters were 300 bar and 40, 60 and 80 °C for CO2 and 100, 150, 200 bar and 40 and 60 °C for propane, respectively. The influence of process parameters on the total yield of extraction and content of lutein diesters in the extracts was investigated. The results show, that solvent power of propane for lutein diesters is approximately 3.5 times higher than of CO2. The calculation procedure based on the Fick's second law was applied to determine the diffusivities of lutein diesters during extraction from marigold flower petals for both extraction stages: a constant rate stage followed by a stage of decreasing rate. The mathematical model based on the Fick's second law well described the experimental extraction results.

  7. RECOVERY OF CARBOXYLIC ACIDS FROM AQUEOUS SOLUTIONS BY LIQUID-LIQUID EXTRACTION WITH A TRIISOOCTYLAMINE DILUENT SYSTEM

    Directory of Open Access Journals (Sweden)

    G. Malmary

    2001-12-01

    Full Text Available Tertiary alkylamines in solution with organic diluents are attractive extractants for the recovery of carboxylic acids from dilute aqueous phases. The aim of this study was to investigate the mechanism for extraction of organic acids from water by a long-chain aliphatic tertiary amine. In order to attain this objective, we studied the liquid-liquid equilibria between the triisooctylamine + 1-octanol + n-heptane system as solvent and an aqueous solution of an individual carboxylic acid such as citric, lactic and malic acids. The experiments showed that the partition coefficient for a particular organic acid depends on the kind of solute, notably when the acid concentration in the aqueous phase is low. A mathematical model, where both chemical association and physical distribution are taken into consideration, is proposed. The model suggests that the various complexes obtained between amine and organic acids contribute to the distribution of the solute between the coexisting phases in equilibrium.

  8. Vortex-assisted ionic liquid-based dispersive liquid-liquid microextraction for assessment of chromium species in artificial saliva extract of different chewing tobacco products.

    Science.gov (United States)

    Akhtar, Asma; Kazi, Tasneem Gul; Afridi, Hassan Imran; Musharraf, Syed Ghulam; Talpur, Farah Naz; Khan, Noman; Bilal, Muhammad; Khan, Mustafa

    2016-12-01

    A novel dispersive liquid-liquid microextraction (ILDLLμE) method using an extracting solvent (ionic liquid) and dispersant (Triton X-114) was developed for the separation and preconcentration of hexavalent chromium (Cr(6+)) in artificial saliva extract (ASE) of chewing tobacco products, gutkha, and mainpuri (n = 23). In the proposed method, the extraction of Cr(6+) was accomplished by using ammonium pyrrolidinedithiocarbamate (APDC) as complexing agent and 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM] [PF6] as extracting solvent. The tiny droplet of metal chelate was then dispersed into TX-114 emulsion, using vortex mixer. Various parameters such as concentration of APDC, pH of the solution, volume of [C4MIM] [PF6], and TX-114 as well as extraction time were studied. Under the most favorable conditions, the limit of detection was found to be 0.068 μg/L with the relative standard deviation carcinogenic and noncarcinogenic risks. Estimated daily intake of Cr via chewing 10 g/day of gutkha and mainpuri was found to be below the maximum tolerable daily intake, whereas the calculated risk of cancer for Cr was observed in the acceptable range of 10E(-6)-10E(-4), except some brands of gutkha. Graphical Abstract ᅟ.

  9. Extraction of pyridine derivatives from human urine using electromembrane extraction coupled to dispersive liquid-liquid microextraction followed by gas chromatography determination.

    Science.gov (United States)

    Arjomandi-Behzad, Leila; Yamini, Yadollah; Rezazadeh, Maryam

    2014-08-01

    In the present work, some of pyridine derivatives were analyzed for the first time in complicated biological fluids by coupling electromembrane extraction with dispersive liquid-liquid microextraction (EME-DLLME). 3-Methylpyridine, 2,4-lutidine, quinoline and 4-dimethylaminopyridine (DMAP) were extracted from urine and water samples. Effective parameters on the efficiencies of EME and DLLME were optimized by one variable at a time method and face-centered central composite design (FCCCD), respectively. The supported liquid phase (SLM) employed for the extraction of the analytes was a mixture of 90% 2-nitrophenyl octyl ether (NPOE) and 10% di-(2-ethylhexyl) phosphate (DEHP) which was immobilized in the pores of a piece of hollow fiber. An electric field was applied to carry over the analytes into acceptor solution. The acceptor solution was transferred to 1mL of an alkaline solution (pH=13) and then DLLME procedure was performed. Preconcentration factors in the range of 40-263 and satisfactory repeatabilities (2.3pyridine compounds in smokers׳ urine samples. The proposed technique can be introduced as a simple, fast and inexpensive method for diagnosis of smokers.

  10. Separation by liquid-liquid extraction of actinides(III) from lanthanides(III) using new molecules: the picolinamides; Separation par extraction liquide-liquide des actinides(III) des lanthanides(III) par de nouvelles molecules: les picolinamides

    Energy Technology Data Exchange (ETDEWEB)

    Cordier, P.Y. [CEA Marcoule, Departement de Recherche en Retraitement et en Vitrification, 30 - Bagnols-sur-Ceze (France)]|[Clermont-Ferrand-2 Univ., 63 - Aubiere (France)

    1996-07-01

    In the field of long-lived radionuclides separation from waste generated during spent fuel reprocessing, the picolinamides have been chosen as potential extractants for the selective extraction of actinides (III) from lanthanides (III). The first studies initiated on the most simple molecule of the picolinamide family, namely 2-pyridinecarboxamide, pointed out that in an aqueous media the complexation stability constant between this ligand and Am(III) is roughly 10 times higher than the ones corresponding to Ln(III). The synthesis of lipophilic derivatives of 2-pyridinecarboxamide leaded to extraction experiments. The extraction of metallic cation by lipophilic picolinamides, according to a solvatation mechanism, is strongly dependent on the nature of the amide function: a primary amide function (group I) leads to a good extraction; on the contrary, there is a decrease for secondary (group II) and tertiary (group III) amide functions. From a theoretical point of view, this work leads finally to the following conclusions: confirmation of the importance of the presence of soft donor atoms within the extractants (nitrogen in our case) for An(III)/Ln(III). Also, sensitivity of this soft donor atom regarding the protonation reaction; prevalence in our case of the affinity of the extractant for the metallic cation over the lipophilia of the extractant to ensure good distribution coefficients. The extraction and Am(III)/Ln(III) separation performances of the picolinamides from pertechnetic media leads to the design of a possible flowsheet for the reprocessing of high level liquid waste, with the new idea of an integrated technetium reflux. (author) 105 refs.

  11. Ultrasonication-assisted extraction and preconcentration of medicinal products from herb by ionic liquids.

    Science.gov (United States)

    Bi, Wentao; Tian, Minglei; Row, Kyung Ho

    2011-07-15

    Ionic liquid-based extraction of medicinal or useful compounds from plants was investigated as an alternative to supercritical fluid, cloud point and conventional organic solvent extractions. The method integrated extraction and preconcentration. Medicinal products were first extracted by an ionic liquid solution, part of which was then converted to a hydrophobic form by anion metathesis for preconcentration. The remaining soluble ionic liquid acted as a dispersive agent to enhance the efficiency of preconcentration. Protein in the extract was precipitated spontaneously without addition of further solvents. Ultrasonication assisted this method for extraction and preconcentration of cryptotanshinone, tanshinone I and tanshinone II A from Salvia Miltiorrhiza Bunge. 0.233 mg g(-1), 0.695 mg g(-1) and 0.682 mg g(-1) of each, respectively, were extracted using [OMIM][Cl], and preconcentrated in a [OMIM][PF(6)] phase at respective concentrations of 148.1, 507.1 and 486.1 μg mL(-1). The method exhibited potential applicability with other medicinal products. Copyright © 2011 Elsevier B.V. All rights reserved.

  12. Recovery of Acetic Acid from An Ethanol Fermentation Broth by Liquid-Liquid Extraction (LLE) Using Various Solvents

    Energy Technology Data Exchange (ETDEWEB)

    Pham, Thi Thu Huong; Kim, Tae Hyun [Kongju National University, Cheonan (Korea, Republic of); Um, Byung Hwan [Hankyong National University, Anseong (Korea, Republic of)

    2015-12-15

    Liquid-liquid extraction (LLE) using various solvents was studied for recovery of acetic acid from a synthetic ethanol fermentation broth. The microbial fermentation of sugars presented in hydrolyzate gives rise to acetic acid as a byproduct. In order to obtain pure ethanol for use as a biofuel, fermentation broth should be subjected to acetic acid removal step and the recovered acetic acid can be put to industrial use. Herein, batch LLE experiments were carried out at 25°C using a synthetic fermentation broth comprising 20.0 g l{sup -1} acetic acid and 5.0 g l{sup -1} ethanol. Ethyl acetate (EtOAc), tri-n-octylphosphine oxide (TOPO), tri-n-octylamine (TOA), and tri-n-alkylphosphine oxide (TAPO) were utilized as solvents, and the extraction potential of each solvent was evaluated by varying the organic phase-to-aqueous phase ratios as 0.2, 0.5, 1.0, 2.0, and 4.0. The highest acetic acid extraction yield was achieved with TAPO; however, the lowest ethanol-to-acetic acid extraction ratio was obtained using TOPO. In a single-stage batch extraction, 97.0 % and 92.4 % of acetic acid could be extracted using TAPO and TOPO when the ratio of organic-to-aqueous phases is 4:1 respectively. A higher solvent-to-feed ratio resulted in an increase in the ethanol-to-acetic acid ratio, which decreased both acetic acid purity and acetic acid extraction yield.

  13. Optimization of liquid-liquid extraction of biosurfactants from corn steep liquor.

    Science.gov (United States)

    Vecino, X; Barbosa-Pereira, L; Devesa-Rey, R; Cruz, J M; Moldes, A B

    2015-09-01

    In this work, the optimization of the operational conditions for the chloroform-based extraction of surface-active compounds from corn steep liquor (CSL) was carried out and the nutritional properties of the remnant aqueous phase (CSL-less biosurfactant) was evaluated as microbial fermentation medium. The optimal conditions to obtain biosurfactants from CSL were as follows: chloroform/CSL ratio 2 (v/v), 56 °C at extraction times >30 min. At the optima conditions, 100 % of biosurfactant extract can be obtained from CSL, obtaining 12.0 ± 0.5 g of biosurfactant extract/Kg of CSL. The critical micelle concentration (CMC) of the biosurfactant extract was 399.4 mg L(-1). This value is similar to the CMC of cetrimonium bromide (CTAB), a cationic surfactant used in the formulation of nanoparticles. The extraction of biosurfactant can be also carried out at room temperature although in this case, the extraction yield decreased about 15 %. The extraction of surface-active compounds from agroindustrial streams can suppose important advances for the bio-based surfactants industry. Biosurfactants obtained in this work are not only more eco-friendly than chemical detergents but also can be cost competitive with its chemical counterparts. Furthermore, after the extraction of surface-active compounds, CSL-less biosurfactant was found to be suitable as nutritional supplement for lactic acid bacteria, maintaining its nutritional properties in comparison with regular CSL.

  14. Synthesis, characterization and application of 1-butyl-3-methylimidazolium tetrafluoroborate for extractive desulfurization of liquid fuel

    Directory of Open Access Journals (Sweden)

    Swapnil A. Dharaskar

    2016-07-01

    Full Text Available In the present paper the experimental data of extractive desulfurization of liquid fuel using 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM]BF4 have been presented. The data of FTIR, 1H NMR and 13C NMR have been discussed for the molecular confirmation of synthesized [BMIM]BF4. Further, the thermal properties, conductivity, solubility, and viscosity analysis of the [BMIM]BF4 were carried out. The effects of reaction time, reaction temperature, sulfur compounds, and recycling of ionic liquid without regeneration on dibenzothiophene removal of liquid fuel were presented. In extractive desulfurization process, the removal of dibenzothiophene in n-dodecane was 73.02% for mass ratio of 1:1 in 30 min at 30 °C under the mild reaction conditions. The ionic liquids could be reused four times without a significant decrease in activity. Also, the desulfurizations of real fuels, multistage extraction were presented. The data and results provided in the present paper explore the significant insights of imidazoled ILs for extractive desulfurization of liquid fuels.

  15. Selective extraction of triazine herbicides from food samples based on a combination of a liquid membrane and molecularly imprinted polymers.

    Science.gov (United States)

    Mhaka, Byron; Cukrowska, Ewa; Bui, Bernadette Tse Sum; Ramström, Olof; Haupt, Karsten; Tutu, Hlanganani; Chimuka, Luke

    2009-10-02

    A selective extraction technique based on the combination of liquid membrane (microporous membrane liquid-liquid extraction) and molecularly imprinted polymers (MIP) was applied to triazines herbicides in food samples. Simazine, atrazine and propazine were extracted from aqueous food samples through the hydrophobic porous membrane that was impregnated with toluene, which also formed part of the acceptor phase. In the acceptor phase, the compounds were re-extracted onto MIP particles. The extraction technique was optimised for the amount of molecularly imprinted polymers particles in the organic acceptor phase, extraction time, and type of organic acceptor solvent and desorption solvent. An extraction time of 90 min and 50mg of MIP were found to be optimum parameters. Toluene as the acceptor phase was found to give higher triazines binding onto MIP particles compared to hexane and combinations of diethyl ether and hexane. 90% methanol in water was found to be the best desorption solvent compared to acetonitrile, methanol and water. The selectivity of the technique was demonstrated by extracting spiked lettuce and apple extracts where clean chromatograms were obtained compared to liquid membrane extraction alone or to the microporous membrane liquid-liquid extraction - non-imprinted polymer combination. The MIP showed a certain degree of group specificity and the extraction efficiency in lettuce extract was 79% (0.72) for simazine, 98% (1.55) for atrazine and 86% (3.08) for propazine.

  16. Ultrasound-assisted extraction of carnosic acid and rosmarinic acid using ionic liquid solution from Rosmarinus officinalis.

    Science.gov (United States)

    Zu, Ge; Zhang, Rongrui; Yang, Lei; Ma, Chunhui; Zu, Yuangang; Wang, Wenjie; Zhao, Chunjian

    2012-01-01

    Ionic liquid based, ultrasound-assisted extraction was successfully applied to the extraction of phenolcarboxylic acids, carnosic acid and rosmarinic acid, from Rosmarinus officinalis. Eight ionic liquids, with different cations and anions, were investigated in this work and [C(8)mim]Br was selected as the optimal solvent. Ultrasound extraction parameters, including soaking time, solid-liquid ratio, ultrasound power and time, and the number of extraction cycles, were discussed by single factor experiments and the main influence factors were optimized by response surface methodology. The proposed approach was demonstrated as having higher efficiency, shorter extraction time and as a new alternative for the extraction of carnosic acid and rosmarinic acid from R. officinalis compared with traditional reference extraction methods. Ionic liquids are considered to be green solvents, in the ultrasound-assisted extraction of key chemicals from medicinal plants, and show great potential.

  17. Synthesis, characterization, and application of 1-butyl-3-methylimidazolium thiocyanate for extractive desulfurization of liquid fuel.

    Science.gov (United States)

    Dharaskar, Swapnil A; Wasewar, Kailas L; Varma, Mahesh N; Shende, Diwakar Z

    2016-05-01

    1-Butyl-3-methylimidazolium thiocyanate [BMIM]SCN has been presented on extractive desulfurization of liquid fuel. The FTIR, (1)H-NMR, and C-NMR have been discussed for the molecular confirmation of synthesized [BMIM]SCN. Further, thermal, conductivity, moisture content, viscosity, and solubility analyses of [BMIM]SCN were carried out. The effects of time, temperature, sulfur compounds, ultrasonication, and recycling of [BMIM]SCN on removal of dibenzothiophene from liquid fuel were also investigated. In extractive desulfurization, removal of dibenzothiophene in n-dodecane was 86.5 % for mass ratio of 1:1 in 30 min at 30 °C under the mild process conditions. [BMIM]SCN could be reused five times without a significant decrease in activity. Also, in the desulfurization of real fuels, multistage extraction was examined. The data and results provided in the present paper explore the significant insights of imidazolium-based ionic liquids as novel extractant for extractive desulfurization of liquid fuels.

  18. Ionic liquids based simultaneous ultrasonic and microwave assisted extraction of phenolic compounds from burdock leaves.

    Science.gov (United States)

    Lou, Zaixiang; Wang, Hongxin; Zhu, Song; Chen, Shangwei; Zhang, Ming; Wang, Zhouping

    2012-02-24

    The ionic liquids based simultaneous ultrasonic and microwave assisted extraction (IL-UMAE) technique was first proposed and applied to isolate compounds. The ionic liquids comprising a range of four anions, five 1-alkyl-3-methylimidazolium derivatives were designed and prepared. The results suggested that varying the anion and cation both had apparent effects on the extraction of phenolics. The results also showed that irradiation power, time and solid-liquid ratio significantly affected the yields. The yields of caffeic acid and quercetin obtained by IL-UMAE were higher than those by regular UMAE. Compared with conventional heat-reflux extraction (HRE), the proposed approach exhibited higher efficiency (8-17% enhanced) and shorter extraction time (from 5h to 30s). The results indicated ILUMAE to be a fast and efficient extraction technique. Moreover, the proposed method was validated by the reproducibility and recovery experiments. The ILUMAE method provided good recoveries (from 96.1% to 105.3%) with RSD lower than 5.2%, which indicated that the proposed method was credible. Based on the designable nature of ionic liquids, and the rapid and highly efficient performance of the proposed approach, ILUMAE provided a new alternative for preparation of various useful substances from solid samples.

  19. Ionic liquids based simultaneous ultrasonic and microwave assisted extraction of phenolic compounds from burdock leaves

    Energy Technology Data Exchange (ETDEWEB)

    Lou Zaixiang, E-mail: louzaixiang@126.com [State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China); Wang Hongxin, E-mail: whx200720082009@yahoo.cn [State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China); Zhu Song; Chen Shangwei; Zhang Ming; Wang Zhouping [State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China)

    2012-02-24

    The ionic liquids based simultaneous ultrasonic and microwave assisted extraction (IL-UMAE) technique was first proposed and applied to isolate compounds. The ionic liquids comprising a range of four anions, five 1-alkyl-3-methylimidazolium derivatives were designed and prepared. The results suggested that varying the anion and cation both had apparent effects on the extraction of phenolics. The results also showed that irradiation power, time and solid-liquid ratio significantly affected the yields. The yields of caffeic acid and quercetin obtained by IL-UMAE were higher than those by regular UMAE. Compared with conventional heat-reflux extraction (HRE), the proposed approach exhibited higher efficiency (8-17% enhanced) and shorter extraction time (from 5 h to 30 s). The results indicated ILUMAE to be a fast and efficient extraction technique. Moreover, the proposed method was validated by the reproducibility and recovery experiments. The ILUMAE method provided good recoveries (from 96.1% to 105.3%) with RSD lower than 5.2%, which indicated that the proposed method was credible. Based on the designable nature of ionic liquids, and the rapid and highly efficient performance of the proposed approach, ILUMAE provided a new alternative for preparation of various useful substances from solid samples.

  20. Dispersive liquid-liquid microextraction with little solvent consumption combined with gas chromatography-mass spectrometry for the pretreatment of organochlorine pesticides in aqueous samples.

    Science.gov (United States)

    Tsai, Wan-Chun; Huang, Shang-Da

    2009-07-03

    Dispersive liquid-liquid microextraction with little solvent consumption (DLLME-LSC), a novel dispersive liquid-liquid microextraction (DLLME) technique with few solvent requirements (13 microL of a binary mixture of disperser solvent and extraction solvent in the ratio of 6:4) and short extraction time (90 s), has been developed for extraction of organochlorine pesticides (OCPs) from water samples prior to gas chromatography/mass spectrometry analysis. In DLLME-LSC, much less volume of organic solvent is used as compared to DLLME. The new technique is less harmful to environment and yields a higher enrichment factor (1885-2648-fold in this study). Fine organic droplets were formed in the sample solution by manually shaking the test tube containing the mixture of sample solution and extraction solvent. The large surface area of the organic solvent droplets increases the rate of mass transfer from the water sample to the extractant and produces efficient extraction in a short period of time. DLLME-LSC shows good repeatability (RSD: 4.1-9.7% for reservoir water; 5.6-8.9% for river water) and high sensitivity (limits of detection: 0.8-2.5 ng/L for reservoir water; 0.4-1.3 ng/L for river water). The method can be used on various water samples (river water, tap water, sea water and reservoir water). It can be used for routine work for the investigation of OCPs.

  1. Liquid - liquid extraction of matrine using TRPO/cyclohexane reverse micelles

    Directory of Open Access Journals (Sweden)

    Lichun Dong

    2009-06-01

    Full Text Available Reverse micellar extraction has been widely used in the purification of biomolecules. However, reverse micelles formed by ionic surfactants can only be employed for the extraction of biomolecules that are charged in the extraction system with the electrostatic interaction between surfactants and solutes as the driving force. In this study, the extraction of matrine by using reverse micelles formed by non-ionic TRPO surfactants was studied. Theoretical analysis and experimental results demonstrated that the driving force of the extraction is the coordination forces between matrines and TRPOs. Using this coordination-based reverse micellar extraction, matrine can be efficiently separated from oxymatrine and other components in the raw matrine materials. Experimental studies showed that the factors affecting matrine extraction include pH value and TRPO concentration. The existence of ions in the system does not affect the partition coefficient significantly and the addition of a small amount of chloroform in the solution of reverse micelles was found to improve the extraction significantly.

  2. Optimization and application of homogeneous liquid-liquid extraction in preconcentration of copper (II) in a ternary solvent system

    Energy Technology Data Exchange (ETDEWEB)

    Farajzadeh, Mir Ali [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)], E-mail: farajzade@yahoo.com; Bahram, Morteza [Department of Chemistry, Faculty of Science, Urmia University, Urmia (Iran, Islamic Republic of); Zorita, Saioa [Department of Analytical Chemistry, University of Lund, P.O. Box 124, 221 00 Lund (Sweden); Mehr, Behzad Ghorbani [Department of Chemistry, Faculty of Science, Urmia University, Urmia (Iran, Islamic Republic of)

    2009-01-30

    In this study a homogeneous liquid-liquid extraction based on the Ph-dependent phase-separation process was investigated using a ternary solvent system (water-acetic acid-chloroform) for the preconcentration of Cu{sup 2+} ions. 8-Hydroxy quinoline was used as the chelating agent prior to its extraction. Flame atomic absorption spectrophotometry using acetylene-air flame was used for the quantitation of analyte after preconcentration. The effect of various experimental parameters in extraction step was investigated using two optimization methods, one variable at a time and central composite design. The experimental design was done at five levels of operating parameters. Nearly the same optimized results were obtained using both methods: sample size, 5 mL; volume of NaOH 10 M, 2 mL; chloroform volume, 300 {mu}L; 8-hydroxy quinoline concentration more than 0.01 M and salt amount did not affect the extraction significantly. Under the optimum conditions the calibration graph was linear over the range 10-2000 {mu}g L{sup -1}. The relative standard deviation was 7.6% for six repeated determinations (C = 500 {mu}g L{sup -1}). Furthermore, the limit of detection (S/N = 3) and limit of quantification (S/N = 10) of the method were obtained as 1.74 and 6 {mu}g L{sup -1}, respectively.

  3. Simultaneous determination of dextromethorphan, dextrorphan, and guaifenesin in human plasma using semi-automated liquid/liquid extraction and gradient liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Eichhold, Thomas H; McCauley-Myers, David L; Khambe, Deepa A; Thompson, Gary A; Hoke, Steven H

    2007-01-17

    A method for the simultaneous determination of dextromethorphan (DEX), dextrorphan (DET), and guaifenesin (GG) in human plasma was developed, validated, and applied to determine plasma concentrations of these compounds in samples from six clinical pharmacokinetic (PK) studies. Semi-automated liquid handling systems were used to perform the majority of the sample manipulation including liquid/liquid extraction (LLE) of the analytes from human plasma. Stable-isotope-labeled analogues were utilized as internal standards (ISTDs) for each analyte to facilitate accurate and precise quantification. Extracts were analyzed using gradient liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Use of semi-automated LLE with LC-MS/MS proved to be a very rugged and reliable approach for analysis of more than 6200 clinical study samples. The lower limit of quantification was validated at 0.010, 0.010, and 1.0 ng/mL of plasma for DEX, DET, and GG, respectively. Accuracy and precision of quality control (QC) samples for all three analytes met FDA Guidance criteria of +/-15% for average QC accuracy with coefficients of variation less than 15%. Data from the thorough evaluation of the method during development, validation, and application are presented to characterize selectivity, linearity, over-range sample analysis, accuracy, precision, autosampler carry-over, ruggedness, extraction efficiency, ionization suppression, and stability. Pharmacokinetic data are also provided to illustrate improvements in systemic drug and metabolite concentration-time profiles that were achieved by formulation optimization.

  4. Analysis of biogenic amines in wines by salting-out assisted liquid-liquid extraction and high-performance liquid chromatography with fluorimetric detection.

    Science.gov (United States)

    Ramos, Rui Miguel; Valente, Inês Maria; Rodrigues, José António

    2014-06-01

    Biogenic amines are nitrogenous organic compounds of low molecular weight that are either formed or metabolized in cells of living organisms and can be found in several food products, being produced mainly by amino acid decarboxylation. When ingested in high concentrations they can induce several health problems in humans. In alcoholic beverages, and especially in wine, they are formed during the vinification process as a result of the action of microorganisms. In this work it is proposed a new methodology for the determination of biogenic amines in wines, which includes a sample preparation approach based on salting-out assisted liquid-liquid extraction, the use of dansyl chloride for the derivatization and chromatographic separation by high-performance liquid chromatography with fluorimetric detection. The salting-out effect is used to promote phase separation between water and a water-miscible organic solvent, while improving the extraction of organic or inorganic species. Several extraction parameters were optimized, such as the dansyl chloride concentration, pH and the effects caused by the order in which the extraction and derivatization were performed. Extraction of amines, and consequent detection, depends on the presence of dansyl chloride in solution prior to extraction. The results showed the possibility to simultaneously perform the extraction and the derivatization, making sample preparation easier and less time-consuming. The methodology was successfully applied to the determination of biogenic amines in five wines (white, red and rosé). This method has the potential to be a good alternative to existing methods since it is cheaper, easier and simplifies the sample preparation step.

  5. Removal of acetic acid from simulated hemicellulosic hydrolysates by emulsion liquid membrane with organophosphorus extractants.

    Science.gov (United States)

    Lee, Sang Cheol

    2015-09-01

    Selective removal of acetic acid from simulated hemicellulosic hydrolysates containing xylose and sulfuric acid was attempted in a batch emulsion liquid membrane (ELM) system with organophosphorus extractants. Various experimental variables were used to develop a more energy-efficient ELM process. Total operation time of an ELM run with a very small quantity of trioctylphosphine oxide as the extractant was reduced to about a third of those required to attain almost the same extraction efficiency as obtained in previous ELM works without any extractant. Under specific conditions, acetic acid was selectively separated with a high degree of extraction and insignificant loss of xylose, and its purity and enrichment ratio in the stripping phase were higher than 92% and 6, respectively. Also, reused organic membrane solutions exhibited the extraction efficiency as high as fresh organic solutions did. These results showed that the current ELM process would be quite practical.

  6. Pressurized liquid extraction of phenolic compounds from rice (Oryza sativa) grains.

    Science.gov (United States)

    Setyaningsih, W; Saputro, I E; Palma, M; Barroso, C G

    2016-02-01

    An analytical pressurized liquid extraction (PLE) process has been studied for the extraction of phenolic compounds from rice grains. A fractional factorial design (2(7-2)) with a centre point was used to optimize PLE parameters such as solvent composition (EtOAc in MeOH), extraction temperature, pressure, flushing, static extraction time, solvent-purge and sample weight. Extraction temperature, solvent and static extraction time were found to have a significant effect on the response value. The optimized method was validated for selectivity, linearity, limits of detection and quantification, recovery and precision. The validated method was successfully applied for the analysis of a wide variety of rice grains. Seventeen phenolic compounds were detected in the sample and guaiacol, ellagic acid, vanillic acid and protocatechuic acid were identified as the most abundant compounds. Nonetheless, different species of rice show very varied compound diversity and levels of compounds in their grain compositions.

  7. Extraction of lipids from microalgae using CO2-expanded methanol and liquid CO2.

    Science.gov (United States)

    Paudel, Ashok; Jessop, Michael J; Stubbins, Spencer H; Champagne, Pascale; Jessop, Philip G

    2015-05-01

    The use of CO2-expanded methanol (cxMeOH) and liquid carbon dioxide (lCO2) is proposed to extract lipids from Botryococcus braunii. When compressed CO2 dissolves in methanol, the solvent expands in volume, decreases in polarity and so increases in its selectivity for biodiesel desirable lipids. Solid phase extraction of the algal extract showed that the cxMeOH extracted 21 mg of biodiesel desirable lipids per mL of organic solvent compared to 3mg/mL using either neat methanol or chloroform/methanol mixture. The non-polar lCO2 showed a high affinity for non-polar lipids. Using lCO2, it is possible to extract up to 10% neutral lipids relative to the mass of dry algae. Unlike extractions using conventional solvents, these new methods require little to no volatile, flammable, or chlorinated organic solvents. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. Aromatics extraction from pyrolytic sugars using ionic liquid to enhance sugar fermentability.

    Science.gov (United States)

    Li, Xiaohua; Luque-Moreno, Luis C; Oudenhoven, Stijn R G; Rehmann, Lars; Kersten, Sascha R A; Schuur, Boelo

    2016-09-01

    Fermentative bioethanol production from pyrolytic sugars was improved via aromatics removal by liquid-liquid extraction. As solvents, the ionic liquid (IL) trihexyltetradecylphosphonium dicyanamide (P666,14[N(CN)2]) and ethyl acetate (EA) were compared. Two pyrolytic sugar solutions were created from acid-leached and untreated pinewood, with levoglucosan contents (most abundant sugar) of 29.0% and 8.3% (w/w), respectively. In a single stage extraction, 70% of the aromatics were effectively removed by P666,14[N(CN)2] and 50% by EA, while no levoglucosan was extracted. The IL was regenerated by vacuum evaporation (100mbar) at 220°C, followed by extraction of aromatics from fresh pyrolytic sugar solutions. Regenerated IL extracted aromatics with similar extraction efficiency as the fresh IL, and the purified sugar fraction from pretreated pinewood was hydrolyzed to glucose and fermented to ethanol, yielding 0.46g ethanol/(g glucose), close to the theoretical maximum yield.

  9. Liquid-liquid extraction kinetics of uranyl nitrate and actinides (III)-lanthanides nitrates by extractants with amide function; Cinetique d`extraction liquide-liquide du nitrate d`uranyle et des nitrates d`actinides (III) et de lanthanides (III) par des extractants a fonction amide

    Energy Technology Data Exchange (ETDEWEB)

    Toulemonde, V.

    1995-12-20

    Nowadays, the most important part of electric power is generated by fission energy. But spent fuels have then to be reprocessed. The production of these reprocessed materials separately and with a high purity level is done according to a liquid-liquid extraction process (Purex process) with the use of tributyl phosphate as solvent. Optimization studies concerning the extracting agent have been undertaken. This work gives the results obtained for the uranyl nitrate and the actinides (III)-lanthanides (III) nitrates extraction by extractants with amide function (monoamide for U(VI) and diamide for actinides (III) and lanthanides (III)). The extraction kinetics have been studied in the case of a metallic specie transfer from the aqueous phase towards the organic phase. The experiments show that the nitrates extraction kinetics is limited by the complexation chemical reaction of the species at the interface between the two liquids. An adsorption-desorption interfacial reactional mechanism (Langmuir theory) is proposed for the uranyl nitrate. (O.M.). 89 refs.

  10. Rare earth extraction from wet process phosphoric acid by emulsion liquid membrane

    Institute of Scientific and Technical Information of China (English)

    张利昌; 陈前林; 康超; 马昕; 杨尊良

    2016-01-01

    The recovery of rare earths (RE) during the wet processing of phosphoric acid is very important, the method of emul-sion liquid membrane (ELM) with di(2-ethylhexly) phosphate (D2EHPA) as carrier has the high selectivity while cannot provide a satisfactory extraction rate. Here novel method of emulsion liquid membrane (ELM) using Aniline as carrier to extract RE from the feed solution was proposed. The method could increase the extraction rate of RE in the real sample to 93%. The effects of dif-ferent parameters such as type and concentration of carrier and surfactant, hydrochloric acid concentration, organic to internal phase volume ratio, membrane to external phase volume ratio on extraction of RE3+ were investigated. Quantitative extraction (>93%) of RE3+ was observed with 6 vol.% Aniline and 4 vol.% T154 liquid membrane at external to internal phase volume ratio of 10 for the feed solution. The proposed method of ELM using Aniline as carrier can be expected to provide a practical, efficient, and economical method for extracting RE from phosphate leach solution with high acidity in the industry of wet process phospho-ric acid.

  11. Solvent Extraction of Yttrium by Task-specific Ionic Liquids Bearing Carboxylic Group

    Institute of Scientific and Technical Information of China (English)

    王威; 刘郁; 徐爱梅; 杨华玲; 崔红敏; 陈继

    2012-01-01

    A new kind of hydrophobic ionic liquids [1-alkyl-3-(1-carboxylpropyl)im][PF6] has been synthesized, and their extraction.properties for Y(III) in the nitric acid medium was also investigated. The effects of extractant concentration, equilibrium pH of aqueous phase, salt concentration, temperature etc. were discussed. The results show that this kind of Task-Specific Ionic Liquid (TSIL) needs to be saponified before being used for the Y(III) extraction, and the extraction is-acid dependent,-and the extraction efficiency increases with the aqueous phase acldity decreasing. Furthermore, the loaded organic phase is easy to be stripped; more than 95% Y(III) could be stripped from the loaded organic phase when the stripping acidity is higher than 0.07 mol-L-1. The slope analysis technique is used to investigate the extraction mechanism, and a possible cation-exchange extraction mechanism is proposed in the oresent extraction system.

  12. Isolation of atropine and scopolamine from plant material using liquid-liquid extraction and EXtrelut(®) columns.

    Science.gov (United States)

    Śramska, Paula; Maciejka, Artur; Topolewska, Anna; Stepnowski, Piotr; Haliński, Łukasz P

    2017-02-01

    Tropane alkaloids are toxic secondary metabolites produced by Solanaceae plants. Among them, plants from Datura genus produce significant amounts of scopolamine and hyoscyamine; the latter undergoes racemization to atropine during isolation. Because of their biological importance, toxic properties and commonly reported food and animal feed contamination by different Datura sp. organs, there is a constant need for reliable methods for the analysis of tropane alkaloids in many matrices. In the current study, three extraction and sample-clean up procedures for the determination of scopolamine and atropine in plant material were compared in terms of their effectiveness and repeatability. Standard liquid-liquid extraction (LLE) and EXtrelut(®) NT 3 columns were used for the sample clean-up. Combined ultrasound-assisted extraction and 24h static extraction using ethyl acetate, followed by multiple LLE steps was found the most effective separation method among tested. However, absolute extraction recovery was relatively low and reached 45-67% for atropine and 52-73% for scopolamine, depending on the compound concentration. The same method was also the most effective one for the isolation of target compounds from Datura stramonium leaves. EXtrelut(®) columns, on the other hand, displayed relatively low effectiveness in isolating atropine and scopolamine from such a complex matrix and hence could not be recommended. The most effective method was also applied to the extraction of alkaloids from roots and stems of D. stramonium. Quantitative analyses were performed using validated method based on gas chromatography with flame ionization detector (GC-FID). Based on the results, the importance of the proper selection of internal standards in the analysis of tropane alkaloids was stressed out.

  13. Extraction of S- and N-compounds from the mixture of hydrocarbons by ionic liquids as selective solvents.

    Science.gov (United States)

    Gabrić, Beata; Sander, Aleksandra; Cvjetko Bubalo, Marina; Macut, Dejan

    2013-01-01

    Liquid-liquid extraction is an alternative method that can be used for desulfurization and denitrification of gasoline and diesel fuels. Recent approaches employ different ionic liquids as selective solvents, due to their general immiscibility with gasoline and diesel, negligible vapor pressure, and high selectivity to sulfur- and nitrogen-containing compounds. For that reason, five imidazolium-based ionic liquids and one pyridinium-based ionic liquid were selected for extraction of thiophene, dibenzothiophene, and pyridine from two model solutions. The influences of hydrodynamic conditions, mass ratio, and number of stages were investigated. Increasing the mass ratio of ionic liquid/model fuel and multistage extraction promotes the desulfurization and denitrification abilities of the examined ionic liquids. All selected ionic liquids can be reused and regenerated by means of vacuum evaporation.

  14. Sensitive high-performance liquid chromatographic quantitation of gabapentin in human serum using liquid-liquid extraction and pre-column derivatization with 9-fluorenylmethyl chloroformate.

    Science.gov (United States)

    Bahrami, Gholamreza; Kiani, Amir

    2006-05-01

    Most of the published methods for analysis of gabapentin, an antiepileptic agent, in human serum are based on the same approach, involving o-phthaldialdehyde derivatization of deproteinized serum samples. The present paper however, describes a new, simple and sensitive high-performance liquid chromatographic method for determination of gabapentin in human serum using liquid-liquid extraction and 9-fluorenylmethyl chloroformate (FMOC-Cl) as pre-column labeling agent. The drug and an internal standard (azithromycin) were extracted from serum by salting-out approach using a mixture of dichloromethane-2 propanol (1:1, v/v) as the extracting solvent. The extracted analytes were subjected to derivatization with FMOC-Cl in the presence of phosphate buffer (pH 7). A mobile phase consisting of methanol-0.05 M sodium phosphate buffer (73/27, v/v; pH of 3.9) containing 1 ml/l triethylamine was eluted and chromatographic separation was performed on a Shimpack CLC-C18 (150 mm x 4.6 mm) column. The standard curve was linear over the range of 0.03-20 microg/ml and limit of quantification was 0.03 microg/ml. The performance of analysis was studied and the validated method showed excellent performance in terms of selectivity, specificity, sensitivity, precision and accuracy. No interferences were found from commonly co-administered antiepileptic agents.

  15. Hollow fiber-based liquid-liquid-liquid micro-extraction with osmosis: II. Application to quantification of endogenous gibberellins in rice plant.

    Science.gov (United States)

    Wu, Qian; Wu, Dapeng; Duan, Chunfeng; Shen, Zheng; Guan, Yafeng

    2012-11-23

    The phenomenon and benefits of osmosis in hollow fiber-based liquid-liquid-liquid micro-extraction (HF-LLLME) were theoretically discussed in part I of this study. In this work, HF-LLLME with osmosis was coupled with high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-triple quadrupole MS/MS) to analyze eight gibberellins (gibberellin A(1), gibberellin A(3), gibberellin A(4), gibberellin A(7), gibberellin A(8), gibberellin A(9), gibberellin A(19) and gibberellin A(20)) in rice plant samples. According to the theory of HF-LLLME with osmosis, single factor experiments, orthogonal design experiments and mass transfer simulation of extraction process were carried out to select the optimal conditions. Cyclohexanol - n-octanol (1:3, v/v) was selected as organic membrane. Donor phase of 12 mL was adjusted to pH 2 and 20% NaCl (w/v) was added. Acceptor phase with an initial volume of 20 μL was the solution of 0.12 mol L(-1) Na(2)CO(3)-NaHCO(3) buffer (pH 9). Temperature was chosen to be 30 °C and extraction time was selected to be 90 min. Under optimized conditions, this method provided good linearity (r, 0.99552-0.99991) and low limits of detection (0.0016-0.061 ng mL(-1)). Finally, this method was applied to the analysis of endogenous gibberellins from plant extract which was obtained with traditional solvent extraction of rice plant tissues, and the relative recoveries were from 62% to 166%.

  16. Accelerated solvent extraction combined with dispersive liquid-liquid microextraction before gas chromatography with mass spectrometry for the sensitive determination of phenols in soil samples.

    Science.gov (United States)

    Xing, Han-Zhu; Wang, Xia; Chen, Xiang-Feng; Wang, Ming-Lin; Zhao, Ru-Song

    2015-05-01

    A method combining accelerated solvent extraction with dispersive liquid-liquid microextraction was developed for the first time as a sample pretreatment for the rapid analysis of phenols (including phenol, m-cresol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol) in soil samples. In the accelerated solvent extraction procedure, water was used as an extraction solvent, and phenols were extracted from soil samples into water. The dispersive liquid-liquid microextraction technique was then performed on the obtained aqueous solution. Important accelerated solvent extraction and dispersive liquid-liquid microextraction parameters were investigated and optimized. Under optimized conditions, the new method provided wide linearity (6.1-3080 ng/g), low limits of detection (0.06-1.83 ng/g), and excellent reproducibility (extraction with dispersive liquid-liquid microextraction as a sample pretreatment procedure coupled with gas chromatography and mass spectrometry is an excellent method for the rapid analysis of trace levels of phenols in environmental soil samples.

  17. liquid-liquid extraction of iron (iii) from ouenza iron ore leach liquor ...

    African Journals Online (AJOL)

    A. Nouioua

    2017-09-01

    Sep 1, 2017 ... hexyl phosphonic acid mono 2 - ethyl hexyl ester. ... kerosene from chloride medium Chemical Engineering and Processing: Process ... phosphate and synergistic extraction combined with methyl isobutyl ketone, J. Separation ...

  18. Liquid-liquid extraction of metal ions by the 6-membered N-containing macrocycle hexacyclen.

    Science.gov (United States)

    Arpadjan, S; Mitewa, M; Bontchev, P R

    1987-11-01

    The nitrogen-containing analogue of 18-crown-6, 1,4,7,10,13,16-hexa-azaoctadecane (hexacyclen)] was studied as a reagent for complexation and extraction of some metal ions. It was found that with this reagent and methyl isobutyl ketone, metal ions such as silver(I), mercury(II), copper(II), platinum(II) and palladium(II) can be quantitatively extracted and separated from iron(III) and some other metal ions.

  19. Liquid-liquid extraction and recovery of indium using Cyanex 923

    Energy Technology Data Exchange (ETDEWEB)

    Gupta, Bina; Deep, Akash; Malik, Poonma

    2004-06-25

    The extraction of In(III) from HCl, H{sub 2}SO{sub 4}, and HNO{sub 3} media using a 0.20 mol l{sup -1} Cyanex 923 solution in toluene is investigated. In(III) is quantitatively extracted over a fairly wide range of HCl molarity while from H{sub 2}SO{sub 4} and HNO{sub 3} media the extraction is quantitative at low acid concentration. The extracted metal ion has been recovered by stripping with 1.0 mol l{sup -1} H{sub 2}SO{sub 4}. The stoichiometry of the In(III): Cyanex 923 complex is observed to be 1:2. The extraction of In(III) is insignificantly changed in diluents namely toluene, n-hexane, kerosene (160-200 degree sign C), cyclohexane, and xylene having more or less the same dielectric constants, whereas, it decreases with increasing polarity of diluents such as cyclohexanone and chloroform. The extractant is stable towards prolonged acid contact and there is a negligible loss in its extraction efficiency even after recycling for 20 times. The extraction behavior of some commonly associated metal ions namely V(IV), Ti(IV), Al(III), Cr(III), Fe(III), Ga(III), Sb(III), Tl(III), Mn(II), Fe(II), Cu(II), Zn(II), Cd(II), Pb(II), and Tl(I) has also been investigated. Based on the partition data the conditions have been identified for attaining some binary separations of In(III). These conditions are extended for the recovery of pure indium from zinc blend, zinc plating mud, and galena. The recovery of the metal ions is around 95% with purity approximately 99%.

  20. Liquid-liquid extraction of palladium(II) from nitric acid by bis(2-ethylhexyl) sulphoxide

    Energy Technology Data Exchange (ETDEWEB)

    Shukla, J.P. (Radiochemistry Division, Bhabha Atomic Research Centre, Trombay, Bombay 400085 (India)); Singh, R.K.; Sawant, S.R.; Varadarajan, N. (Power Reactor Fuel Reprocessing Plant, Bhabha Atomic Research Centre, Trombay, Bombay 400085 (India))

    1993-04-15

    The extraction of palladium(II) nitrate by bis(2-ethylhexyl) sulphoxide (BESO) was evaluated over a wide range of acidity, and BESO was shown to have a strong extraction ability toward this thiophilic 'soft' metal. Essentially quantitative extraction of trace and macro amounts of palladium is easily accomplished from about 8 M HNO 8 M HNO[sub 3] down to pH 2 solutions by 0.2 M BESO into toluene. Optimum conditions such as aqueous phase acidity, solvent, period of equilibration, aqueous to organic phase ratios, reagent concentration and strippant were established for the selective and reversible extraction and separation of palladium. Slope analyses applied to Pd(II) distribution experiments from nitrate solutions showed a predominant formation of the solvated organic phase complex Pd(NO[sub 3])[sub 2].2BESO. Recovery of the extractant from loaded palladium is easily accomplished by using sodium thiosulphate or a mixture of 2 M sodium carbonate+0.5 M ammonia solution. The extracted complex was characterized by elemental analysis and IR and UV-visible spectrometry, and its composition was confirmed to be Pd(NO[sub 3])[sub 2].2BESO

  1. Liquid-Liquid Extraction Of Zinc By 3-Methyl-Quinoxaline-2-Thione From Nitrate Medium

    Directory of Open Access Journals (Sweden)

    Sanae Baki Senhaji

    2015-09-01

    Full Text Available The extraction of zinc with 3-methyl-2 (1H-quinoxalinethione LH, is investigated in nitrate solution as a function of pHrange 2-6, and analytical concentrations of NO-3 anions (CNO3 and extractant (CLH. The extraction mechanism with LH,is determined on the basis of the variation of the distribution coefficient D with pH, CNO3 and CLH. As a result, the partition equilibrium involves complexing phenomenon, ion-pair formation, and 1H+ exchange reaction. The overall extraction constants are logK01.5 = 5.1, and logK11.5 = -0.6. The extraction complexes are found to be Zn(LH2∫(NO3∫+2 and Zn(L (LH∫-1 (NO3 with l = 1 or 2. The hydrolysis reaction of Zn(II is evaluated and it is found that it results in the formation of Zn(OH+and Zn(OH2aq species, at pH >5.6. Zinc shows maximum percent extraction (75% with the pH 4.7 at low organic ligand concentration (0.01M.

  2. The effect of electric fields upon liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Carleson, T.E.

    1988-04-13

    A series of mass transfer studies were conducted for the extraction of solute from droplets falling in an electric field. The experiments were planned such that the dispersed phase resistance was controlling. In one series of experiments single drops were formed from a charged nozzle and allowed to fall through a continuous, dielectric phase. The drop size and velocity were correlated by means of a simple force balance. Drop mass transfer coefficients were calculated for the drop free fall period and were compared to predictions based upon literature correlations for an oscillating droplet in-the absence of an electric field. Droplet size and velocity were approximately predicted by a staple force balance whereas the mass transfer coefficient was approximately 25--250% higher than that predicted. Droplet extraction efficiencies Increased about 20--30% in the presence of electric fields up to 2 kv/cm. For the same field, the drop diameter decreased 30--50% and the terminal velocity increased by up to 50%. The enhancements for the toluene-water system can be ascribed to increases in terminal velocity and decreases in drop diameter. The mass transfer model for freely falling drops proposed by Skelland and Wellek roughly predicts the moderate mass transfer efficiency increases (about 18% at 1 kv/cm) for the toluene water system but failed to predict the increases (about 25% at 0.5 kv/cm) for the heptane furfural system. The second series of experiments involved the formation of a swarm of droplets In a three stage sieve tray column. In a separate series of experiments. the effect of the electric field upon mass transfer from drops exhibiting interfacial turbulence was evaluated.

  3. Electromembrane extraction with alkylated phosphites and phosphates as supported liquid membranes

    DEFF Research Database (Denmark)

    Huang, Chuixiu; Gjelstad, Astrid; Pedersen-Bjergaard, Stig

    2017-01-01

    A range of alkylated phosphates and phosphites were for the first time investigated as potential supported liquid membranes (SLMs) for electromembrane extraction (EME) of basic drugs from human plasma samples. Six polar basic drugs were used as model analytes for initial testing of the different ...

  4. Pressurised liquid extraction of flavonoids in onions. Method development and validation

    DEFF Research Database (Denmark)

    Søltoft, Malene; Christensen, J.H.; Nielsen, J.

    2009-01-01

    A rapid and reliable analytical method for quantification of flavonoids in onions was developed and validated. Five extraction methods were tested on freeze-dried onions and subsequently high performance liquid chromatography (HPLC) with UV detection was used for quantification of seven flavonoids...

  5. Automated extraction of DNA and PCR setup using a Tecan Freedom EVO® liquid handler

    DEFF Research Database (Denmark)

    Frøslev, Tobias Guldberg; Hansen, Anders Johannes; Stangegaard, Michael

    We have implemented and validated automated protocols for DNA extraction and PCR setup using a Tecan Freedom EVO® liquid handler mounted with the TeMagS magnetic separation device. The methods were validated for accredited, forensic genetic work according to ISO 17025 using the Qiagen Mag...

  6. Determination of Polychlorinated Biphenyls in Soil and Sediment by Selective Pressurized Liquid Extraction with Immunochemical Detection

    Science.gov (United States)

    A selective liquid pressurized extraction (SPLE) method was developed as a streamlined sample preparation/cleanup procedure for determining Aroclors and coplanar polychlorinated biphenyls (PCBs) in soil and sediment matrices. The SPLE method was coupled with an enzyme-linked imm...

  7. Determination of sedative hypnotics in sewage sludge by pressurized liquid extraction with high-performance liquid chromatography and tandem mass spectrometry.

    Science.gov (United States)

    Arbeláez, Paula; Granados, Judith; Borrull, Francesc; Marcé, Rosa Maria; Pocurull, Eva

    2014-12-01

    This paper describes a method for the determination of eight sedative hypnotics (benzodiazepines and barbiturates) in sewage sludge using pressurized liquid extraction and liquid chromatography with tandem mass spectrometry. Pressurized liquid extraction operating conditions were optimized and maximum recoveries were reached using methanol under the following operational conditions: 100ºC, 1500 psi, extraction time of 5 min, one extraction cycle, flush volume of 60% and purge time of 120 s. Pressurized liquid extraction recoveries were higher than 88% for all the compounds except for carbamazepine (55%). The repeatability and reproducibility between days, expressed as relative standard deviation (n = 5), were lower than 6 and 10%, respectively. The detection limits for all compounds were lower than 12.5 μg/kg of dry weight. The method was applied to determine benzodiazepines and barbiturates in sewage sludge from urban sewage treatment plants, and carbamazepine showed the highest concentration (7.9-18.9 μg/kg dry weight).

  8. Economic appraisal of supercritical fluid extraction of refined cashew nut shell liquid.

    Science.gov (United States)

    Patel, Rajesh N; Bandyopadhyay, Santanu; Ganesh, Anuradda

    2006-08-18

    This manuscript summarises the techno-economic feasibility of refined cashew nut shell liquid (CNSL). A simple mass transfer based mathematical model for the yield prediction is presented. The process parameters and extraction time for maximum profit and purity of the product were optimized. The optimum extraction time for maximum profit and purity was found to be 0.9h at 300 bar and 323 K. The influence of the different costs, such as fixed cost, raw material cost, labor cost, utility cost, etc. on profit and cost of production of the extract is also presented.

  9. Gas-assisted dispersive liquid-phase microextraction using ionic liquid as extracting solvent for spectrophotometric speciation of copper.

    Science.gov (United States)

    Akhond, Morteza; Absalan, Ghodratollah; Pourshamsi, Tayebe; Ramezani, Amir M

    2016-07-01

    Gas-assisted dispersive liquid-phase microextraction (GA-DLPME) has been developed for preconcentration and spectrophotometric determination of copper ion in different water samples. The ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate and argon gas, respectively, were used as the extracting solvent and disperser. The procedure was based on direct reduction of Cu(II) to Cu(I) by hydroxylamine hydrochloride, followed by extracting Cu(I) into ionic liquid phase by using neocuproine as the chelating agent. Several experimental variables that affected the GA-DLPME efficiency were investigated and optimized. Under the optimum experimental conditions (IL volume, 50µL; pH, 6.0; acetate buffer, 1.5molL(-1); reducing agent concentration, 0.2molL(-1); NC concentration, 120µgmL(-1); Ar gas bubbling time, 6min; argon flow rate, 1Lmin(-1); NaCl concentration, 6% w/w; and centrifugation time, 3min), the calibration graph was linear over the concentration range of 0.30-2.00µgmL(-1) copper ion with a limit of detection of 0.07µgmL(-1). Relative standard deviation for five replicate determinations of 1.0µgmL(-1) copper ion was found to be 3.9%. The developed method was successfully applied to determination of both Cu(I) and Cu(II) species in water samples.

  10. Selective pressurized liquid extraction for the analysis of polychlorinated biphenyls, polychlorinated dibenzo-p-dioxins and dibenzofurans in soil.

    Science.gov (United States)

    Klees, Marcel; Bogatzki, Corinna; Hiester, Ernst

    2016-10-14

    During this study a high throughout selective pressurized liquid extraction (SPLE) method was developed and validated for the simultaneous extraction of polychlorinated dibenzo-p-dioxins, dibenzofurans (PCDD/PCDFs) and polychlorinated biphenyls (PCBs) from soil. To that end, extraction rates of PCBs from soil utilizing different extraction solvents and different extraction temperatures were investigated whereas extraction rates were comparable for toluene, n-hexane and dichloromethane (extraction conditions for all utilized solvents: 33mL PLE extraction cell, extraction temperature: 110°C, static extraction time: 5min, flush volume: 60%, purge 90s). Ratios of native PCBs and PCDD/PCDFs congener concentrations after Soxhlet and selective pressurized liquid extraction (SPLE) showed that SPLE is an alternative sample preparation step for the simultaneous determination of PCDD/PCDFs and PCBs in soil. Additional clean-up steps for the separation of PCBs and PCDD/PCDFs utilizing alumina were performed in order to avoid interferences between the component classes.

  11. Effect of pressurized liquids on extraction of antioxidants from Chlorella vulgaris.

    Science.gov (United States)

    Cha, Kwang Hyun; Kang, Suk Woo; Kim, Chul Young; Um, Byung Hun; Na, Ye Rim; Pan, Cheol-Ho

    2010-04-28

    Chlorella vulgaris is a green microalga that contains various antioxidants, such as carotenoids and chlorophylls. In this study, antioxidants from C. vulgaris were extracted using pressurized liquid extraction (PLE), which has been recently used for bioactive compound extraction. The antioxidant capacity of individual compounds in chlorella was determined by online HPLC ABTS(*+) analysis. According to the antioxidant analysis of total extracts, the extraction yield, radical scavenging activity, and phenolic compounds using PLE were relatively high compared to those obtained using maceration or ultrasound-assisted extraction. On the basis of online HPLC ABTS(*+) analysis, the 15 major antioxidants from chlorella extracts were identified as hydrophilic compounds, lutein and its isomers, chlorophylls, and chlorophyll derivatives. Using PLE at high temperature (85-160 degrees C) significantly increased antioxidant extraction from chlorella, improving the formation of hydrophilic compounds and yielding more antioxidative chlorophyll derivatives. Online HPLC ABTS(*+) analysis was a useful tool for the separation of main antioxidants from PLE extracts and allowed the simultaneous measurement of their antioxidant capacity, which clearly showed that PLE is an excellent method for extracting antioxidants from C. vulgaris.

  12. Determination of benzoxazinone derivatives in plants by combining pressurized liquid extraction-solid-phase extraction followed by liquid chromatography-electrospray mass spectrometry.

    Science.gov (United States)

    Villagrasa, Marta; Guillamón, Miriam; Eljarrat, Ethel; Barceló, Damià

    2006-02-22

    A new analytical method based on the use of pressurized liquid extraction (PLE) followed by solid-phase extraction with LiChrolut RP C18 cartridges was evaluated for the sample preparation, extraction, and cleanup of eight naturally occurring benzoxazinone derivatives, 2-beta-D-glucopyranosyloxy-4-hydroxy-1,4-benzoxazin-3-one, 2-beta-D-glucopyranosyloxy-4-hydroxy-7-methoxy-1,4-benzoxazin-3-one, 2,4-dihydroxy-1,4-benzoxazin-3-one (DIBOA), 2,4-dihydroxy-7-methoxy-1,4-benzoxazin-3-one, 2-hydroxy-1,4-benzoxazin-3-one, 2-hydroxy-7-methoxy-1,4-benzoxazin-3-one, benzoxazolin-2-one, and 6-methoxybenzoxazolin-2-one in plant samples. Afterward, liquid chromatography-electrospray mass spectrometry, using the selected ion monitoring mode and internal standard (2-MeO-DIBOA, indoxyl-beta-D-glucoside, and quercetin-3-O-rutinoside) quantification method was performed. This paper demonstrates the effectiveness of the PLE method, in conjunction with sensitive and specific mass spectrometric detection, for the quantitative recovery of compounds of the benzoxazinone class from plants. The recoveries of the analytes ranged from 66 to 110% with coefficients of variation ranging from 1 to 14%. This method gave detection limits between 1 and 27 microg/g. The method was applied to foliage and roots of three different wheat cultivars, and the analytes were detected in the range of 11-3261 microg/g of dry weight.

  13. Comparison of liquid-liquid extraction-thin layer chromatography with solid-phase extraction-high-performance thin layer chromatography in detection of urinary morphine.

    Science.gov (United States)

    Ahadi, Ali; Partoazar, Alireza; Abedi-Khorasgani, Mohammad-Hassan; Shetab-Boushehri, Seyed Vahid

    2011-09-01

    Liquid-liquid extraction-thin layer chromatography (LLE-TLC) has been a common and routine combined method for detection of drugs in biological materials. Solid-phase extraction (SPE) is gradually replacing the traditional LLE method. High performance thin layer chromatography (HPTLC) has several advantages over TLC. The present work studied the higher efficiency of a new SPE-HPTLC method over that of a routine LLE-TLC method, in extraction and detection of urinary morphine. Fifty-eight urine samples, primarily identified as morphine-positive samples by a strip test, were re-screened by LLE-TLC and SPE-HPTLC. The results of LLE-TLC and SPE-HPTLC were then compared with each other. The results showed that the SPE-HPTLC detected 74% of total samples as morphine-positive samples whereas the LLE-TLC detected 48% of the same samples. We further discussed the effect of codeine abuse on TLC analysis of urinary morphine. Regarding the importance of morphine detection in urine, the present combined SPE-HPTLC method is suggested as a replacement method for detection of urinary morphine by many reference laboratories.

  14. Extraction and enrichment of natural pigments from solid samples using ionic liquids and chitosan nanoparticles.

    Science.gov (United States)

    Xu, Jing-Jing; Li, Qin; Cao, Jun; Warner, Elisa; An, Mingrui; Tan, Zhijing; Wang, Shu-Ling; Peng, Li-Qing; Liu, Xun-Gao

    2016-09-09

    A green and economical method for the extraction and preconcentration of natural pigments (curcumin, demethoxycurcumin and bisdemethoxycurcumin) was developed using ultrasound-assisted extraction combined with dispersive micro solid-phase extraction. In this work, Ionic liquids (ILs) were used for the pre-extraction of natural pigments. The pure chitosan nanoparticles (CS NPs) were then used as a sorbent for the microextraction mode. The method involves the use of ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry. Operating parameters influencing the performance of extraction steps such as type and concentration of ILs, concentration of CS NPs, type of elution solvent, agitation time and pH of sample-extracting solution were investigated. Under the optimum conditions, the proposed method exhibited a low detection limit in the range of 0.11-0.36ng/mL at S/N=3, and good linearities with coefficients of determination (R(2)) higher than 0.9990. The recoveries of turmeric samples were ranging from 90.45% to 105.04% for the three studied curcuminoids with SD of 3.27-6.58. The experimental results indicated that the ILs and CS NPs were the promising materials for the extraction and enrichment of target curcuminoids from complex solid samples.

  15. Extraction of Co(II) from aqueous solution using emulsion liquid membrane.

    Science.gov (United States)

    Gasser, M S; El-Hefny, N E; Daoud, J A

    2008-03-01

    The extraction equilibrium of Co(II) from thiocyanate medium by CYANEX 923 (mixture of straight chain alkylated phosphine oxides) in cyclohexane was studied. The stoichiometry of the extraction reaction was postulated based on slope analysis method and the extraction constant Kex was calculated. The stripping percentage of Co(II) with sulphuric acid from the loaded CYANEX 923 was found to increase with the increase in acid concentration. The extraction of Co(II) from aqueous thiocyanate medium into emulsion liquid membrane using CYANEX 923 extractant was also studied. The influence of different parameters such as stirring speed, surfactant concentration, pH of the extractant phase, carrier concentration, internal phase stripping acid concentration, initial Co(II) concentration as well as temperature on the emulsion stability were investigated. The applicability of the emulsion liquid membrane (ELM) process using CYANEX 923 as extractant and SPAN 80 as surfactant for the removal and the concentration of Co(II) from thiocyanate solution was investigated. The results show that it is possible to recover 95% of cobalt in the inner phase after 10 min of contacting time with a concentration factor of 5.

  16. A novel CMPO-functionalized task specific ionic liquid: Synthesis, extraction and spectroscopic investigations of actinide and lanthanide complexes

    NARCIS (Netherlands)

    Mohapatra, P.K.; Kandwal, P.; Iqbal, M.; Huskens, Jurriaan; Murali, M.S.; Verboom, Willem

    2013-01-01

    A novel CMPO (carbamoylmethylphosphine oxide) based task specific ionic liquid (TSIL) with an NTf2− counter anion was synthesized and evaluated for actinide/lanthanide extraction from acidic feed solutions using several room temperature ionic liquids (RTILs). The extraction data were compared with

  17. Determination of aflatoxin B1 in cereals by homogeneous liquid-liquid extraction coupled to high performance liquid chromatography-fluorescence detection.

    Science.gov (United States)

    Sheijooni-Fumani, Neda; Hassan, Jalal; Yousefi, Seyed R

    2011-06-01

    A simple and rapid method based on homogeneous liquid-liquid extraction coupled to HPLC with fluorescence detection was developed for the determination of aflatoxin B1 (AFB1) in the rice and grain samples after post-column derivatization. The proposed method eliminated the use of immunoaffinity columns for clean-up in the determination of AFB1. The parameters affecting recovery and preconcentration such as type and volume of organic solvent, volume ratio of water/methanol, concentration of phase separator reagent and extraction time were optimized. Under the optimized conditions, the calibration graph was linear in the concentration range of 0.01-1.0 ng/g with the detection limit of 0.003 ng/g. This method was successfully applied for the analysis of AFB1 in different cereal samples.

  18. Simplified recovery process of Ralstonia solanacearum-synthesized polyhydroxyalkanoates via chemical extraction complemented by liquid-liquid phase separation

    Directory of Open Access Journals (Sweden)

    Karine L. Macagnan

    Full Text Available Poly (3-hydroxybutyrate (P(3HB is the most studied thermoplastic biopolymer belonging to the polyhydroxyalkanoate (PHA family, the main features of which include rapid biodegradability and biocompatibility. The bioplastic recovery process is an important step during production and can directly influence the characteristics of PHAs. However, more efficient methods for the production of P(3HB are necessary to make it economically viable. The aim of the present study was to improve the standard, chloroform-based, extraction step for the recovery of P(3HB. The polymer was produced using a Ralstonia solanacearum strain. The following parameters were improved in the recovery process: heating time, separation method (filtration or liquid-liquid phase separation, biomass state (fresh or dry cell concentrate and the solvent:biomass ratio. By improving the chemical extraction of P(3HB we recovered 98% of the cumulative polymer and reduced the heating time by 75%. Furthermore, we improved the separation process and developed an extraction solution that was faster and more economical.

  19. Determination of artificial sweeteners in sewage sludge samples using pressurised liquid extraction and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Ordoñez, Edgar Y; Quintana, José Benito; Rodil, Rosario; Cela, Rafael

    2013-12-13

    An analytical method for the determination of six artificial sweeteners in sewage sludge has been developed. The procedure is based on pressurised liquid extraction (PLE) with water followed by solid-phase extraction (SPE) and subsequent liquid chromatography-tandem mass spectrometry analysis. After optimisation of the different PLE parameters, extraction with aqueous 500mM formate buffer (pH 3.5) at 80°C during a single static cycle of 21min proved to be best conditions. After a subsequent SPE, quantification limits, referred to dry weight (dw) of sewage sludge, ranged from 0.3ng/g for acesulfame (ACE) to 16ng/g for saccharin (SAC) and neohespiridine dihydrochalcone. The trueness, expressed as recovery, ranged between 72% and 105% and the precision, expressed as relative standard deviation, was lower than 16%. Moreover, the method proved its linearity up to the 2μg/g range. Finally, the described method was applied to the determination of the artificial sweeteners in primary and secondary sewage sludge from urban wastewater treatment plants. Four of the six studied artificial sweeteners (ACE, cyclamate, SAC and sucralose) were found in the samples at concentrations ranging from 17 to 628ng/g dw.

  20. Enhanced spectrofluorimetric determination of aflatoxin M1 in liquid milk after magnetic solid phase extraction

    Science.gov (United States)

    Hashemi, Mahdi; Taherimaslak, Zohreh; Rashidi, Somayeh

    2014-07-01

    A simple and sensitive method using magnetic solid phase extraction (MSPE) followed by spectrofluorimetric detection has been developed for separation and determination of aflatoxin M1 (AFM1) in liquid milk. The method is based on the extraction of AFM1 on the modified magnetic nanoparticles (MMNPs) and subsequent derivatization of extracted AFM1 to AFM1 hemi-acetal derivative (AFM2a) by reaction with trifluoroacetic acid (TFA) for spectrofluorimetric detection. Magnetic nanoparticles (MNPs) coated by 3-(trimethoxysilyl)-1-propantiol (TMSPT) and modified with 2-amino-5-mercapto-1,3,4-thiadiazole (AMT) were used as adsorbent in MSPE procedure. Influential parameters affecting the extraction efficiency were investigated and optimized. Under the optimum conditions the calibration curve for AFM1 determination showed good linearity in the range 0.030-10.0 μg L-1 (R2 = 0.9991). The repeatability and reproducibility (RSD%) for 0.050 μg L-1 of AFM1 were 4.5% and 5.3%, respectively and limit of detection limit (S/N = 3) was estimated to be 0.010 μg L-1. The developed method was successfully applied for extraction of AFM1 from spiked liquid milk and natural contaminated liquid milk. The good spiked recoveries ranging from 91.6% to 96.1% were obtained. The results demonstrated that the developed method is simple, inexpensive, accurate and remarkably free from interference effects.

  1. A new dispersive liquid-liquid microextraction using ionic liquid based microemulsion coupled with cloud point extraction for determination of copper in serum and water samples.

    Science.gov (United States)

    Arain, Salma Aslam; Kazi, Tasneem Gul; Afridi, Hassan Imran; Arain, Mariam Shahzadi; Panhwar, Abdul Haleem; Khan, Naeemullah; Baig, Jameel Ahmed; Shah, Faheem

    2016-04-01

    A simple and rapid dispersive liquid-liquid microextraction procedure based on ionic liquid assisted microemulsion (IL-µE-DLLME) combined with cloud point extraction has been developed for preconcentration copper (Cu(2+)) in drinking water and serum samples of adolescent female hepatitits C (HCV) patients. In this method a ternary system was developed to form microemulsion (µE) by phase inversion method (PIM), using ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C4mim][PF6]) and nonionic surfactant, TX-100 (as a stabilizer in aqueous media). The Ionic liquid microemulsion (IL-µE) was evaluated through visual assessment, optical light microscope and spectrophotometrically. The Cu(2+) in real water and aqueous acid digested serum samples were complexed with 8-hydroxyquinoline (oxine) and extracted into IL-µE medium. The phase separation of stable IL-µE was carried out by the micellar cloud point extraction approach. The influence of of different parameters such as pH, oxine concentration, centrifugation time and rate were investigated. At optimized experimental conditions, the limit of detection and enhancement factor were found to be 0.132 µg/L and 70 respectively, with relative standard deviation <5%. In order to validate the developed method, certified reference materials (SLRS-4 Riverine water) and human serum (Sero-M10181) were analyzed. The resulting data indicated a non-significant difference in obtained and certified values of Cu(2+). The developed procedure was successfully applied for the preconcentration and determination of trace levels of Cu(2+) in environmental and biological samples.

  2. Selection and design of ionic liquids as solvents in extractive distillation and extraction processes

    NARCIS (Netherlands)

    Schuur, B.

    2015-01-01

    Since the late 1990’s there has been a tremendous growth in literature on ionic liquids (ILs) for a broad range of applications, i.e. catalysis, electrolytes for batteries, in solvolysis of biomass, and also in separation technology. ILs can be applied as solvents for absorption (e.g. of CO2), extra

  3. Analysis of potential migrants from plastic materials in milk by liquid chromatography-mass spectrometry with liquid-liquid extraction and low-temperature purification.

    Science.gov (United States)

    Bodai, Zsolt; Szabó, Bálint Sámuel; Novák, Márton; Hámori, Susanne; Nyiri, Zoltán; Rikker, Tamás; Eke, Zsuzsanna

    2014-10-15

    A simple and fast analytical method was developed for the determination of six UV stabilizers (Cyasorb UV-1164, Tinuvin P, Tinuvin 234, Tinuvin 326, Tinuvin 327, and Tinuvin 1577) and five antioxidants (Irgafos 168, Irganox 1010, Irganox 3114, Irganox 3790, and Irganox 565) in milk. For sample preparation liquid-liquid extraction with low-temperature purification combined with centrifugation was used to remove fats, proteins, and sugars. After the cleanup step, the sample was analyzed with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). External standard and matrix calibrations were tested. External calibration proved to be acceptable for Tinuvin P, Tinuvin 234, Tinuvin 326, Tinuvin 327, Irganox 3114, and Irganox 3790. The method was successfully validated with matrix calibration for all compounds. Method detection limits were between 0.25 and 10 μg/kg. Accuracies ranged from 93 to 109%, and intraday precisions were <13%.

  4. The mechanism of lipids extraction from wet microalgae Scenedesmus sp. by ionic liquid assisted subcritical water

    Science.gov (United States)

    Yu, Zhuanni; Chen, Xiaolin; Xia, Shuwei

    2016-06-01

    In this paper, the total sugar concentration, protein concentration, lipid yield and morphology characteristics of the algae residue were determined to explain the mechanism of lipids extraction from wet microalgae Scenedesmus sp. by ionic liquid assisted subcritical water. The results showed similar variation for the sugar, protein and lipid. However, the total sugar was more similar to lipids yield, so the results showed that the reaction between ionic liquid and cellulose and hemicellulose in cell wall was the most important step which determined the lipids extration directly. And the total sugar variation may be representing the lipids yield. For later lipids extraction, we can determine the total sugar concentration to predict the extraction end product.

  5. Study on Extracting Low Concentration Cadmium from Zinc Hydrometallurgy System by Liquid Membrane Crystallizing Technique

    Institute of Scientific and Technical Information of China (English)

    1999-01-01

    The extraction of low concentration cadmium from a system containing high concentration zinc was studied and got CdS product directly. A new liquid membrane system taking DIPSA, TIBPS as carriers, (NH4)2S as precipitating agent was reported. Precipitating Cd2+ in the internal aq. phase that is used to treat sulfuric acid leaching solution of zinc oxide in zinc hydrometallurgy has gotten satisfied results of extracting cadmium from high concentration zinc. After one-stage of batch process under the optimum liquid membrane conditions, 98.6% transferring rate and 98.1% extracting rate of cadmium was obtained with only less than 1.0% transferring rate of zinc, and the feed solution can be purified very well.

  6. Separation of aromatic precipitates from simulated high level radioactive waste by hydrolysis, evaporation and liquid-liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Young, S.R.; Shah, H.B.; Carter, J.T.

    1991-01-01

    The Defense Waste Processing Facility (DWPF) at the SRS will be the United States' first facility to process High Level radioactive Waste (HLW) into a borosilicate glass matrix. The removal of aromatic precipitates by hydrolysis, evaporation and liquid-liquid extraction will be a key step in the processing of the HLW. This step, titled the Precipitate Hydrolysis Process, has been demonstrated by the Savannah River Laboratory with the Precipitate Hydrolysis Experimental Facility (PHEF). The mission of the PHEF is to demonstrate processing of simulated high level radioactive waste which contains tetraphenylborate precipitates and nitrite. Reduction of nitrite by hydroxylamine nitrate and hydrolysis of the tetraphenylborate by formic acid is discussed. Gaseous production, which is primarily benzene, nitrous oxide and carbon dioxide, has been quantified. Production of high-boiling organic compounds and the accumulation of these organic compounds within the process are addressed.

  7. Separation of aromatic precipitates from simulated high level radioactive waste by hydrolysis, evaporation and liquid-liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Young, S.R.; Shah, H.B.; Carter, J.T.

    1991-12-31

    The Defense Waste Processing Facility (DWPF) at the SRS will be the United States` first facility to process High Level radioactive Waste (HLW) into a borosilicate glass matrix. The removal of aromatic precipitates by hydrolysis, evaporation and liquid-liquid extraction will be a key step in the processing of the HLW. This step, titled the Precipitate Hydrolysis Process, has been demonstrated by the Savannah River Laboratory with the Precipitate Hydrolysis Experimental Facility (PHEF). The mission of the PHEF is to demonstrate processing of simulated high level radioactive waste which contains tetraphenylborate precipitates and nitrite. Reduction of nitrite by hydroxylamine nitrate and hydrolysis of the tetraphenylborate by formic acid is discussed. Gaseous production, which is primarily benzene, nitrous oxide and carbon dioxide, has been quantified. Production of high-boiling organic compounds and the accumulation of these organic compounds within the process are addressed.

  8. Novel method for determination of anthracene by coupling dispersive liquid-liquid extraction to first-derivative synchronous spectrofluorimetry.

    Science.gov (United States)

    Abdel-Aziz, Omar; El Kosasy, A M; El-Sayed Okeil, Sherif Mahmoud

    2014-05-01

    A novel method could be adopted successfully for determination of anthracene in environmental samples, utilizing dispersive liquid-liquid extraction followed by first-derivative synchronous fluorimetry at a constant wavelength difference Δλ = 165 nm, where a linear calibration curve was obtained in a concentration range of 0.5-100 ng mL(-1) at 244 nm. The detection limit was 0.1 ng mL(-1). The method can be easily adopted for determination of anthracene in aqueous media including tap water and river water. The recoveries obtained were 85.40-108.02%. The proposed method was validated according to International Conference of Harmonization (ICH) guide lines and successfully applied to determine anthracene in pure form and in water samples including real life water samples from different sources. All the results obtained were compared with those of published method, where no a significant difference was observed.

  9. Deep Extractive Desulfurization of Gasoline with Ionic Liquids Based on Metal Halide

    Institute of Scientific and Technical Information of China (English)

    Wang Haojie; He Jianxun; Yang Cairong; Zhang Hang

    2014-01-01

    Ionic liquid [Et3NH]Cl-FeCl3/CuCl was synthesized by mixing [Et3NH]Cl, anhydrous FeCl3 and anhydrous CuCl, and the desulfurization activity of this ionic liquid was tested. It exhibited remarkable ability in effective desulfurization of model gasoline (thiophene in n-octane) and lfuid catalytic cracking (FCC) gasoline, and the sulfur removal of thiophene in model oil (V(IL):V(oil)=0.08) could reach 93.9%in 50 min at 50℃. Low-sulfur (﹤10μg/g) FCC gasoline could be obtained after three extraction runs at an ionic liquid/oil volume ratio of 0.1, with the yield of FCC gasoline reaching 94.3%. The ionic liquid could be recycled 5 times with merely a slight decrease in activity.

  10. Determination of carbohydrates in tobacco by pressurized liquid extraction combined with a novel ultrasound-assisted dispersive liquid-liquid microextraction method.

    Science.gov (United States)

    Cai, Kai; Hu, Deyu; Lei, Bo; Zhao, Huina; Pan, Wenjie; Song, Baoan

    2015-07-02

    A novel derivatization-ultrasonic assisted-dispersive liquid-liquid microextraction (UA-DLLME) method for the simultaneous determination of 11 main carbohydrates in tobacco has been developed. The combined method involves pressurized liquid extraction (PLE), derivatization, and UA-DLLME, followed by the analysis of the main carbohydrates with a gas chromatography-flame ionization detector (GC-FID). First, the PLE conditions were optimized using a univariate approach. Then, the derivatization methods were properly compared and optimized. The aldononitrile acetate method combined with the O-methoxyoxime-trimethylsilyl method was used for derivatization. Finally, the critical variables affecting the UA-DLLME extraction efficiency were searched using fractional factorial design (FFD) and further optimized using Doehlert design (DD) of the response surface methodology. The optimum conditions were found to be 44 μL for CHCl3, 2.3 mL for H2O, 11% w/v for NaCl, 5 min for the extraction time and 5 min for the centrifugation time. Under the optimized experimental conditions, the detection limit of the method (LODs) and linear correlation coefficient were found to be in the range of 0.06-0.90 μg mL(-1) and 0.9987-0.9999. The proposed method was successfully employed to analyze three flue-cured tobacco cultivars, among which the main carbohydrate concentrations were found to be very different.

  11. Fast, simple and efficient salting-out assisted liquid-liquid extraction of naringenin from fruit juice samples prior to their enantioselective determination by liquid chromatography.

    Science.gov (United States)

    Magiera, Sylwia; Kwietniowska, Ewelina

    2016-11-15

    In this study, an easy, simple and efficient method for the determination of naringenin enantiomers in fruit juices after salting-out-assisted liquid-liquid extraction (SALLE) and high-performance liquid chromatography (HPLC) with diode-array detection (DAD) was developed. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. After extraction, juice samples were incubated with hydrochloric acid in order to achieve hydrolysis of naringin to naringenin. The hydrolysis parameters were optimized by using a half-fraction factorial central composite design (CCD). After sample preparation, chromatographic separation was obtained on a Chiralcel® OJ-RH column using the mobile phase consisting of 10mM aqueous ammonium acetate:methanol:acetonitrile (50:30:20; v/v/v) with detection at 288nm. The average recovery of the analyzed compounds ranged from 85.6 to 97.1%. The proposed method was satisfactorily used for the determination of naringenin enantiomers in various fruit juices samples.

  12. Fire suppression system of a small-scale LNG loading facility at PT Badak NGL

    Science.gov (United States)

    Yustiarza, Farhan Hilmyawan

    2017-03-01

    LNG progressively become favorable energy to replace oil-based fuel due to lower cost and more environment-friendly. In order to support an emerging LNG demands in Kalimantan, PT Badak NGL, one of the leading LNG Company in the world, develops the land-transported LNG loading facility. This facility performs loading the LNG into a small-scale tank (ISO Tank) with 20 m3 capacities. Safety reviews over this facility were conducted. Based on these reviews, the LNG filling station requires supplemental safeguards, such as LNG spill containment and firefighting foam system besides firewater system and dry chemical system. The spill containment provides holding LNG spill within the limits of plant property, while the high expansion foam system deals to minimize the vaporization rate to prevent a fire incident. This paper mainly discusses designing of such supplemental safeguards. The requirement of the spill containment is 20 m3 (6.3 × 3.3 × 2.0) m and the foam system should be capable generating foam at least 40 m3/min.

  13. Ionic liquids for extraction of metals and metal containing compounds from communal and industrial waste water.

    Science.gov (United States)

    Fischer, Lisa; Falta, Thomas; Koellensperger, Gunda; Stojanovic, Anja; Kogelnig, Daniel; Galanski, Markus; Krachler, Regina; Keppler, Bernhard K; Hann, Stephan

    2011-10-01

    In a fundamental study the potential of ionic liquids based on quaternary ammonium- and phosphonium cations and thiol-, thioether-, hydroxyl-, carboxylate- and thiocyanate-functionalized anions has been assessed for future application in advanced sewage treatment. The elimination of the metal(oid)s Ag, As, Cd, Cr, Cu, Hg, Ni, Pb, Pt, Sn, Zn and the cancerostatic platinum compounds cisplatin and carboplatin was screened using a liquid phase micro-extraction set-up. The analytical tool-set consisted of ICP-SFMS and LC-ICP-MS for quantification of metal(oid)s and cancerostatic platinum compounds, respectively. The purity of the ILs was assessed for the investigated metal(oid)s on the base of present EU environmental quality standards and was found to be sufficient for the intended use. In model solutions at environmental relevant concentrations extraction efficiencies≥95% could be obtained for Ag, Cu, Hg and Pt with both phosphonium- and ammonium-based ILs bearing sulphur functionality in the form of thiosalicylate and 2-(methylthiobenzoate) anions, as well as with tricaprylmethylammonium thiocyanate within an extraction time of 120 min. All other metals were extracted to a lower extent (7-79%). In the case of cancerostatic platinum compounds a phosphonium-based IL bearing thiosalicylate functionality showed high extraction efficiency for monoaquacisplatin. For the first time, liquid phase micro extraction with ionic liquids was applied to industrial and communal waste water samples. The concentration of all investigated metal(oid)s could be significantly reduced. The degree of elimination varied with the initial concentration of metals, pH and the amount of suspended particulate matter.

  14. Novel Gas-assisted Three-liquid-phase Extraction System for Simultaneous Separation and Concentration of Anthraquinones in Herbal Extract

    Institute of Scientific and Technical Information of China (English)

    Xingfu Yang; Xiangfeng Liang; Liangrong Yang; Feng Pan; Fuli Deng; Huizhou Liu

    2014-01-01

    abstract Gas-assisted three-liquid-phase extraction (GATE), which has the advantages of both three-liquid-phase extrac-tion and solvent sublation, is a novel separation technique for separation and concentration of two organic com-pounds into different phases in one step. This highly effective and economically applicable method has been developed for separating emodin and rhein from herbal extract. In a GATE system composed of butyl acetate/PEG4000/ammonium sulfate aqueous solution, influence of various parameters including gas flow rate, flotation time, salt concentration, initial volume of PEG and butyl acetate was investigated. Within 50 min of 30 ml·min-1 nitrogen flow, removal ratio of emodin and rhein from aqueous phase could be over 99%and 97%, respectively. Mass fraction of emodin in the BA phase and rhein in the PEG phase could reach 97%and 95%, respectively. It is demonstrated that gas bubbling is effective for partitioning of emodin and rhein into butyl acetate and PEG phase respectively, and dispersed PEG and butyl acetate could be captured from the aqueous solution. Experi-mental results show that GATE could be an effective and economical technology for concentration and separation of co-existed products in medicinal plants.

  15. Evaluation of molecularly imprinted anion-functionalized poly(ionic liquid)s by multi-phase dispersive extraction of flavonoids from plant.

    Science.gov (United States)

    Bi, Wentao; Tian, Minglei; Row, Kyung Ho

    2013-01-15

    Molecularly imprinted anion-functionalized poly(ionic liquid)s (MAPILs) were prepared by radical polymerization for the multi-phase dispersive extraction (MPDE) of flavonoids from plants. Poly(ionic liquid)s were functionalized with different anions via anion metathesis to enhance their separation efficiency, called anion-functionalized poly(ionic liquid)s (APILs). A molecularly imprinting technique was introduced to produce specific recognition sites by forming complexes between the template molecules and anion-functionalized ionic liquid monomers to reduce the interactions with the interference substances and increase the selectivity. Multi-phase dispersive extraction (MPDE) was applied for separation instead of the traditional solid phase extraction method. The target compounds were first extracted by three-phase (sample-solvent-sorbent) dispersive extraction and cleaned up after removing the sample matrix. This method significantly decrease in the interference and analysis cost. A suitable sorbent for MPDE could be identified based on the adsorption behaviors of flavonoids on different MAPILs. The mean recovery yields of quercitrin, myricetin, and amentoflavone from Chamaecyparis obtusa under the optimized conditions were 88.07, 93.59, and 95.13%. This is a promising method for the extraction, separation and determination of flavonoids or other polyphenolic compounds from natural and other sources. Copyright © 2012 Elsevier B.V. All rights reserved.

  16. Automated and sensitive determination of four anabolic androgenic steroids in urine by online turbulent flow solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry: a novel approach for clinical monitoring and doping control.

    Science.gov (United States)

    Guo, Feng; Shao, Jing; Liu, Qian; Shi, Jian-Bo; Jiang, Gui-Bin

    2014-07-01

    A novel method for automated and sensitive analysis of testosterone, androstenedione, methyltestosterone and methenolone in urine samples by online turbulent flow solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry was developed. The optimization and validation of the method were discussed in detail. The Turboflow C18-P SPE column showed the best extraction efficiency for all the analytes. Nanogram per liter (ng/L) level of AAS could be determined directly and the limits of quantification (LOQs) were 0.01 ng/mL, which were much lower than normally concerned concentrations for these typical anabolic androgenic steroids (AAS) (0.1 ng/mL). The linearity range was from the LOQ to 100 ng/mL for each compound, with the coefficients of determination (r(2)) ranging from 0.9990 to 0.9999. The intraday and interday relative standard deviations (RSDs) ranged from 1.1% to 14.5% (n=5). The proposed method was successfully applied to the analysis of urine samples collected from 24 male athletes and 15 patients of prostate cancer. The proposed method provides an alternative practical way to rapidly determine AAS in urine samples, especially for clinical monitoring and doping control.

  17. Extraction of coal with solvents in liquid and supercritical state under nonhydrogenating and hydrogenating conditions

    Science.gov (United States)

    Wilhelm, A.; Hedden, K.

    1982-10-01

    The basic steps of coal extraction to determine the optimum conditions for obtaining a higher coal conversion yield in a technical process of supercritical coal extraction were examined. A fixed bed of coal was slowly heated up in a current of pressurized solvent by a nonisothermal technique. The solvent changes its physical state during extraction from a liquid to a supercritical fluid. The formation rates of extract and gaseous products and their integral yields were measured under different extraction conditions. Various coals and lignites as well as different solvents including H-donor solvents and the effect of the addition of molecular hydrogen to the supercritical phase with and without catalyst were studied. Results are interpreted with an extraction scheme, comprising chemical reactions, phase equilibria and transport processes as single steps of the complex extraction procedure. Using a simplified mathematical model, the formation rates of extract as a function of temperature were quantitatively described with effective kinetic parameters. New process for the hydrogenating supercritical extraction of coal, which produces high coal conversion yields is proposed.

  18. Determination of tetracycline antibiotics in fatty food samples by selective pressurized liquid extraction coupled with high-performance liquid chromatography and tandem mass spectrometry.

    Science.gov (United States)

    Jiao, Zhe; Zhang, Suling; Chen, Hongwei

    2015-01-01

    For the determination of trace residues of tetracycline antibiotics in fatty food samples, selective pressurized liquid extraction coupled with high-performance liquid chromatography and tandem mass spectrometry was applied in this study. Copper(II) isonicotinate was first used as online cleanup adsorbent in the selective pressurized liquid extraction process. The adsorbent to sample ratio, extraction temperature, extraction time, and recycle times, etc. were optimized. The tetracyclines in food samples of pork, chicken meat, and clam meat were detected by liquid chromatography with tandem mass spectrometry. Tetracycline was found at levels of 0.32 and 0.53 μg/g and oxytetracycline was found at 0.14 and 0.21 μg/g in chicken meat and clam meat, respectively, while chlorotetracycline and deoxytetracycline were below the detection limit. The detection limit (S/N = 3) for these four tetracyclines were from 0.2 to 3.3 ng/g, the recoveries were from 75.8 to 110.5%, and relative standard deviations were from 5.5 to 13.6%. Copper(II) isonicotinate showed a higher purification capacity than other cleanup adsorbents for extraction of antibiotics in fatty food and the recovery showed predominance compared with a pressurized liquid extraction method without adsorbent. The study demonstrated that copper(II) isonicotinate would be a promising cleanup adsorbent in pressurized liquid extraction for the analysis of trace organic pollutants in complicated samples.

  19. 微流控液液萃取-液液波导集成化分析系统%Microfluidic Analysis System Integrated with Liquid-liquid Extraction and Liquid-liquid Waveguide

    Institute of Scientific and Technical Information of China (English)

    姜健; 李盼盼; 马滢雪; 杨春光; 徐章润

    2016-01-01

    A microfluidic analysis system integrated with liquid-liquid extraction and liquid-liquid waveguide detection was explored. Multiphase laminar liquid-liquid extraction was realized using 1-butyl-3-methyl imidazolium bromide ionic liquid/sodium carbonate solution aqueous two-phase system. Liquid-liquid waveguide absorption photometric detection was achieved by the ionic liquid with higher refractive index served as liquid core and the salt aqueous solution with lower refractive index served as liquid cladding. The extraction efficiency for cresol red extraction is more than 93%. The linear range, the relative standard devia-tion and the detection limit for cresol red detection were 0. 01—0. 40 mg/mL, 3. 4%(n=11) and 3. 8μg/mL (3σ) respectively. Extraction separation and liquid-liquid waveguide-based long optical path absorbance detection were integrated in the system, which provided a new strategy for expanding the application of absorbance detection in microfluidic systems.%利用溴化1-丁基-3-甲基咪唑离子液体/碳酸钠溶液双水相体系,实现了多相层流液液萃取.以具有较高折射率的离子液体为液芯,较低折射率的盐溶液为包层,实现了液液波导吸光度检测.据此建立了一种液液萃取与液液波导检测集成化的微流控分析系统.该系统对甲酚红试样的萃取率在93%以上,对甲酚红试样检测的线性范围为0.01~0.40 mg/mL,相对标准偏差为3.4%(n=11),检出限为3.8μg/mL(3σ).该系统将萃取分离与液液波导长光程吸光度检测集成在一起,为拓展吸光度检测在微流控系统中的应用提供了新思路.

  20. Thioglycolate-based task-specific ionic liquids: Metal extraction abilities vs acute algal toxicity.

    Science.gov (United States)

    Platzer, Sonja; Leyma, Raphlin; Wolske, Sara; Kandioller, Wolfgang; Heid, Esther; Schröder, Christian; Schagerl, Michael; Krachler, Regina; Jirsa, Franz; Keppler, Bernhard K

    2017-10-15

    We studied the extraction behavior of two thioglycolate-based ionic liquids (ILs), for heavy metals from aqueous solutions; substances of interest were methyltrioctylammonium S-hexyl thioglycolate [N1888][C6SAc] and methyltrioctylphosphonium S-hexyl thioglycolate [P1888][C6SAc]. Theses ILs previously have shown very good extraction abilities towards cadmium and copper, therefore we investigated time-dependent metal removal experiments with aqueous solutions of cobalt(II), nickel(II) and zinc(II). The highest distribution ratio (RIL/Water) was determined for zinc (RIL/Water=2000). Recovery studies for zinc after extraction were performed with different stripping agents showing a successful recycling. Additionally, the two ILs were immobilized on active charcoal, displaying great potential for solid-liquid extraction. Regarding the extraction mechanism, quantum-mechanical calculations were included, which indicate that the metal extraction depends on the stability of the metal-water cluster. Ligands (water as well as ILs) are planar coordinated in nickel complexes but showed a tetrahedral configuration for zinc. As a first estimate of the ecotoxicity of the ILs, in vivo tests toward three freshwater green algae species Tetradesmus obliquus, Desmodesmus armatus and Raphidocelis subcapitata were carried out. The EC50 values (effective concentration after 72 h) confirm high toxicity of all tested ILs to all species, displaying only small differences between the species and EC50ies. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

  1. Identification of fermentation inhibitors in wood hydrolyzates and removal of inhibitors by ion exchange and liquid-liquid extraction

    Science.gov (United States)

    Luo, Caidian

    1998-12-01

    Common methods employed in the ethanol production from biomass consist of chemical or enzymatic degradation of biomass into sugars and then fermentation of sugars into ethanol or other chemicals. However, some degradation products severely inhibit the fermentation processes and substantially reduce the efficiency of ethanol production. How to remove inhibitors from the reaction product mixture and increase the production efficiency are critical in the commercialization of any processes of energy from biomass. The present study has investigated anion exchange and liquid-liquid extraction as potential methods for inhibitor removal. An analytical method has been developed to identify the fermentation inhibitors in a hydrolyzate. The majority of inhibitors present in hybrid poplar hydrolyzate have positively been identified. Ion exchange with weak basic Dowex-MWA-1 resin has been proved to be an effective mean to remove fermentation inhibitors from hybrid poplar hydrolyzate and significantly increase the fermentation productivity. Extraction with n-butanol might be a preferred way to remove inhibitors from wood hydrolyzates and improve the fermentability of sugars in the hydrolyzates. n-Butanol also removes some glucose, mannose and xylose from the hydrolyzate. Inhibitor identification reveals that lignin and sugar degradation compounds including both aromatic and aliphatic aldehydes and carboxylic acids formed in hydrolysis, plus fatty acids and other components from wood extractives are major fermentation inhibitors in Sacchromyces cerevisiae fermentation. There are 35 components identified as fermentation inhibitors. Among them, 4-hydroxy benzoic acid, 3,4-dihydroxy benzoic acid, syringic acid, syringaldehyde, and ferulic acid are among the most abundant aromatic inhibitors in hybrid poplar hydrolyzate. The conversion of aldehyde groups into carboxylic acid groups in the nitric acid catalyzed hydrolysis reduces the toxicity of the hydrolyzate. A wide spectrum of

  2. Complex Formation in a Liquid-Liquid Extraction System Containing Co(II), 4-(2-Thiazolylazo)resorcinol and Monotetrazolium Salt.

    Science.gov (United States)

    Divarova, Vidka; Stojnova, Kirila; Racheva, Petya; Lekova, Vanya

    2016-01-01

    The ion-associated complex formed between anionic chelate of Co(II)-4-(2-Thiazolylazo)resorcinol (TAR) with the monotetrazolium cation of 2-(4-Iodophenyl)-3-(4-nitrophenyl)-5-phenyl-2H-tetrazolium chloride (INT) in the liquid-liquid extraction system Co(II)-TAR-INT-H(2)O-CHCl(3) was studied by the spectrophotometric method. The optimum extraction conditions of Co(II) were found. The extraction equilibria were studied. The equilibrium constants, the recovery factor and some analytical characteristics were calculated. The validity of Beer's law was checked. The molar ratio of the components in the ternary ion-associated complex Co(II)-TAR-INT was determined. The general formula of the complex was suggested. The effect of various foreign ions and reagents on the process of complex formation in the liquid-liquid extraction system was studied.

  3. OPTIMIZED DETERMINATION OF TRACE JET FUEL VOLATILE ORGANIC COMPOUNDS IN HUMAN BLOOD USING IN-FIELD LIQUID-LIQUID EXTRACTION WITH SUBSEQUENT LABORATORY GAS CHROMATOGRAPHIC-MASS SPECTROMETRIC ANALYSIS AND ON-COLUMN LARGE VOLUME INJECTION

    Science.gov (United States)

    A practical and sensitive method to assess volatile organic compounds (VOCs) from JP-8 jet fuel in human whole blood was developed by modifying previously established liquid-liquid extraction procedures, optimizing extraction times, solvent volume, specific sample processing te...

  4. Effects of pulsed UV-light on peanut allergens in extracts and liquid peanut butter.

    Science.gov (United States)

    Chung, S-Y; Yang, W; Krishnamurthy, K

    2008-06-01

    Pulsed ultraviolet (PUV) light, a nonthermal technology, was used to treat both the peanut extracts and liquid peanut butter. The objective was to determine if such treatment would lead to a reduction in the allergenic properties of the peanut extract and butter. Peanut samples were PUV treated using a Xenon RS-3000C under the following conditions: 3 pulses/s, 14.6 cm from the central axis of the lamp, 4 min (extract) or 3 min (liquid peanut butter). After the treatment, the peanut samples were centrifuged and the supernatants analyzed by SDS-PAGE and competitive inhibition enzyme-linked immunosorbent assay (ciELISA). For comparison, boiling treatments were also performed. SDS-PAGE showed that while boiling treatment had little effect on the peanut allergens, PUV-light-treated samples displayed a reduced solubility or level of peanut allergens (63 kDa). Solubility of another allergen (18 to 20 kDa) was unaffected. Insoluble aggregates formed were responsible for the reduced level of allergens in PUV-light-treated samples. ciELISA showed that untreated samples exhibited an IgE binding 7-fold higher than the PUV-treated samples. It was concluded that PUV light was effective in reducing IgE binding of peanut extracts and liquid peanut butter. The current study provides an approach to the development of a possibly less allergenic peanut product. However, the reduction in actual allergenicity needs to be confirmed by clinical studies.

  5. KINETICS OF YTTERBIUM ION EXTRACTION BY CA-12 AT THE LIQUID-LIQUID INTERFACE

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    IntroductionExtractants of the carboxylic acid type, althoughnot as widely used as their organophosphoruscounterparts, have found some application in thehydrometallursical processing of base metals. Forexample, they have been employed in the separationo f copper from nickel and cobalt, the removal ofimpurities from cobalt electrolytes, the sepndion ofyttrium and the rare-each metals, the co-eXtraction ofcobalt and nickel, and the recovery of gallium andindiumll].CA-12(see-octylphenoxy acetic acid) is a newe...

  6. Separation of heavy metals from landfill leachate by reactive liquid-liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Mickler, W. [Potsdam Univ. (Germany). Inst. fuer Anorganische Chemie und Didaktik der Chemie

    2001-05-01

    The objective of this work was to investigate the decontamination of a model landfill leachate by simultaneous separation of heavy metals from alkaline earth metals and iron in order to obtain a leachate that can be led back to the landfill. Reactive extraction as a separation process offers the possibility of selectively separating cations, that is, of separating toxic components from less problematic ones, and also includes the possibility of electrolysis and further processes to obtain the desired metals. (orig.)

  7. CHEMOMETRICS IN BIOANALYTICAL SAMPLE PREPARATION - A FRACTIONATED COMBINED MIXTURE AND FACTORIAL DESIGN FOR THE MODELING OF THE RECOVERY OF 5 TRICYCLIC AMINES FROM PLASMA AFTER LIQUID-LIQUID-EXTRACTION PRIOR TO HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY

    NARCIS (Netherlands)

    WIELING, J; MENSINK, CK; JONKMAN, JHG; COENEGRACHT, PMJ; DUINEVELD, CAA; DOORNBOS, DA

    1993-01-01

    A general systematic approach is described for the chemometric modelling of liquid-liquid extraction data of drugs from biological fluids. Extraction solvents were selected from Snyder's solvent selectivity triangle: methyl tert.-butyl ether, methylene chloride and chloroform. The composition of a m

  8. CHEMOMETRICS IN BIOANALYTICAL SAMPLE PREPARATION - A FRACTIONATED COMBINED MIXTURE AND FACTORIAL DESIGN FOR THE MODELING OF THE RECOVERY OF 5 TRICYCLIC AMINES FROM PLASMA AFTER LIQUID-LIQUID-EXTRACTION PRIOR TO HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY

    NARCIS (Netherlands)

    WIELING, J; MENSINK, CK; JONKMAN, JHG; COENEGRACHT, PMJ; DUINEVELD, CAA; DOORNBOS, DA

    1993-01-01

    A general systematic approach is described for the chemometric modelling of liquid-liquid extraction data of drugs from biological fluids. Extraction solvents were selected from Snyder's solvent selectivity triangle: methyl tert.-butyl ether, methylene chloride and chloroform. The composition of a

  9. Investigation and development of liquid-liquid extraction systems for the removal of pertechnetate from aqueous nuclear waste stream simulants

    Science.gov (United States)

    Gansle, Kristina Marie Rohal

    1998-11-01

    The solvent extraction behavior of perrhenate (ReO 4-) and pertechnetate (TcO4- ) from aqueous nuclear waste stream simulants was examined using the anion-exchange reagent Aliquat-336 nitrate. The extraction tendencies of ReO 4- followed those of TcO4- from both acidic and basic media, demonstrating that ReO4 - was a suitable nonradioactive surrogate for TcO4 -. For ICP-AES analysis of Re in high salt solutions, a V-groove nebulizer and 1:1 dilution of the sample and standards with 0.1% Triton X-100 surfactant reduced deposition of solids within the sample introduction system, thus minimizing memory effects. A new approach to waste remediation technology, Redox-Recyclable Extraction and Recovery (R2ER), was also studied. The redox-active species 1,1',3,3'-tetrakis(2-methyl-2-hexyl)ferrocene (HEP) was oxidized to its cationic form for extraction of TcO4 - or ReO4- from aqueous waste and reduced to its neutral form for recovery of the anion. The thermodynamics of liquid-liquid interfacial electron transfer for the oxidation/activation of HEP were shown to be controlled by three factors: the reduction potentials of the redox-active species in the aqueous and organic phases and the transfer of an ion across the liquid-liquid interface. The deactivation/reduction rate of HEP+NO3- by iron was affected by organic solvent diluent and improved by treating the iron with hexanes and 1 M HCl. The volume of solid secondary-waste in the R2ER cycle was reduced by a factor of 3000. In complete extraction/recovery cycles, HEP+NO3- in 2-nonanone removed greater than 99% TcO4- from the 101-SY, 103-SY, 1 M HCl and 1 M NaOH/1.5 M NaNO3 Hanford Tank waste simulants. Another redox-active extractant, bis(hydridotris(1-pyrazolyl)borato)iron(III) nitrate (FeTp2+NO3-), was also selective for ReO4- remediation from simulated aqueous waste. Organic solutions of the alkyl substituted ferricenium extractants were not stable in the presence of nucleophilic anions and/or reducing agents. HEP+NO3

  10. Separation of monosaccharides by solid-phase extraction with ionic liquid-modified microporous polymers.

    Science.gov (United States)

    Tian, Minglei; Bi, Wentao; Row, Kyung H

    2011-11-01

    Ionic liquid-modified porous polymers with large surface area and large amount of functional groups were developed and used in SPE to separate four monosaccharides. Adsorption isotherm showed that the sorbent with amino ionic liquid groups had the highest interaction with the target compounds. The mobile phase of acetonitrile/water 85:15 and 73:30 v/v can successfully separate the monosaccharides. The sorbent produced reproducible results and performed stably, demonstrating its potential applicability in the separation of extract from natural plant. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Improved extraction of fluoroquinolones with recyclable ionic-liquid-based aqueous biphasic systems.

    Science.gov (United States)

    Almeida, Hugo F D; Freire, Mara G; Marrucho, Isabel M

    2016-05-07

    In the past few years, the improvement of advanced analytical tools allowed to confirm the presence of trace amounts of metabolized and unchanged active pharmaceutical ingredients (APIs) in wastewater treatment plants (WWTPs) as well as in freshwater surfaces. It is known that the continuous contact with APIs, even at very low concentrations (ng L(-1)-μg L(-1)), leads to serious human health problems. In this context, this work shows the feasibility of using ionic-liquid-based aqueous biphasic systems (IL-based ABS) in the extraction of quinolones present in aqueous media. In particular, ABS composed of imidazolium- and phosphonium-based ILs and aluminium-based salts (already used in water treatment plants) were evaluated in one-step extractions of six fluoroquinolones (FQs), namely ciprofloxacin, enrofloxacin, moxifloxacin, norfloxacin, ofloxacin and sarafloxacin, and extraction efficiencies up to 98% were obtained. Despite the large interest devoted to IL-based ABS as extractive systems of outstanding performance, their recyclability/reusability has seldomly been studied. An efficient extraction/cleaning process of the IL-rich phase is here proposed by FQs induced precipitation. The recycling of the IL and its further reuse without losses in the ABS extractive performance for FQs were established, as confirmed by the four consecutive removal/extraction cycles evaluated. This novel recycling strategy supports IL-based ABS as sustainable and cost-efficient extraction platforms.

  12. Liquid-liquid extraction procedure exploiting multicommutation in flow system for the determination of molybdenum in plants

    Energy Technology Data Exchange (ETDEWEB)

    Comitre, Ana Lucia D.; Reis, Boaventura F

    2003-03-10

    A liquid-liquid extraction flow analysis procedure for the spectrophotometric determination of molybdenum in plants at {mu}g l{sup -1} level is described. The flow network comprised a set of solenoid valves assembled to implement the multicommutation approach under microcomputer control. Radiation source (LED, 475 nm), detector (photodiode) and separation chamber were nested together with the flow cell comprising a compact unit. The consumption of reagents (potassium thiocyanate and stannous chloride) and also extracting solvent (isoamyl alcohol) were optimized to 32 mg and 200 {mu}l per determination, respectively. Accuracy was assessed by comparing results with those obtained with ICP-OES and no significant difference at 95% confidence level was observed. Other favorable characteristics such as a linear response ranging from 25 to 150 {mu}g l{sup -1} molybdenum (r=0.999); detection limit of 4.6 {mu}g l{sup -1} sample throughput of 25 determinations per hour and relative standard deviation of 2.5% (n=10) were also achieved.

  13. Radiometric Determination of Uranium in Natural Waters after Enrichment and Separation by Cation-Exchange and Liquid-Liquid Extraction

    CERN Document Server

    Pashalidis, I

    2003-01-01

    The alpha-radiometric determination of uranium after its pre-concentration from natural water samples using the cation-exchange resin Chelex-100, its selective extraction by tributylphosphate and electrodeposition on stainless steel discs is reported. The validity of the separation procedure and the chemical recoveries were checked by addition of uranium standard solution as well as by tracing with U-232. The average uranium yield was determined to be (97 +- 2) % for the cation-exchange, (95 +- 2) % for the liquid-liquid extraction, and more than 99% for the electrodeposition. Employing high-resolution alpha-spectroscopy, the measured activity of the U-238 and U-234 radioisotopes was found to be of similar magnitude; i.e. ~7 mBq/L and ~35 mBq/L for ground- and seawater samples, respectively. The energy resolution (FWHM) of the alpha-peaks was 22 keV, while the Minimum Detectable Activity (MDA) was estimated to be 1 mBq/L (at the 95% confidence limit).

  14. Analysis of amphetamines in urine with liquid-liquid extraction by capillary electrophoresis with simultaneous electrochemical and electrochemiluminescence detection.

    Science.gov (United States)

    Sun, Jinying; Xu, Xiaoyu; Wang, Chunyan; You, Tianyan

    2008-10-01

    Amphetamines including methamphetamine, 3,4-methylenedioxyamphetamine and 3,4-methylenedioxymethamphetamine were separated and detected by CE using simultaneous electrochemical (EC) and electrochemiluminescence (ECL) detection (CE-EC/ECL). Factors that influenced the separation and detection performance, such as the detection potential, the pH value and concentration of the running buffer, the separation voltage and the pH of the detection buffer, were investigated. LODs of 3.3x10(-8) mol/L (0.16 fmol), 1.6x10(-7) mol/L (0.78 fmol) and 3.3x10(-8) mol/L (0.16 fmol) were obtained for methamphetamine, 3,4-methylenedioxyamphetamine and 3,4-methylenedioxymethamphetamine, respectively. For practical application, a liquid-liquid extraction with ethyl acetate procedure was developed for urine sample pretreatment and extraction efficiencies higher than 90% were obtained. The established simultaneous CE-EC/ECL was successfully applied for urine sample analysis.

  15. Detection of sulfonamide drug in urine using liquid-liquid extraction and surface-enhanced Raman spectroscopy

    Science.gov (United States)

    Markina, Natalia E.; Shalabay, Victoria V.; Zakharevich, Andrey M.; Markin, Alexey V.

    2016-04-01

    In this article we have applied liquid-liquid extraction (LLE) as a sample preparation technique for detection of sulfadimethoxine (one of sulfonamide drugs) in urine using surface-enhanced Raman spectroscopy (SERS). SERS substrate based on silver nanoparticles has been prepared by citrate reduction of silver nitrate. Obtained calibration curve (SERS intensity vs. sulfadimethoxine concentration) has been used for detection of sulfadimethoxine in human urine samples artificially contaminated by sulfadimethoxine. Three different solvents (ethyl acetate, diethyl ether, chloroform) have been used for LLE performance tests. Chloroform being found as the most effective one based on calculation of recoveries after SERS measurements. Thus we would like to propose fast (less than 20 minutes), simple and sensitive (detection limit up to 1 μg/ml) test for detecting sulfa drugs in urine using a combination of SERS with LLE with sample volume as low as 100 μL. Such test can be applied for evaluation of the degree of drug extraction from human body and half-life of such drug applied in the course of therapeutic treatments of certain diseases.

  16. Conceptual process design and economic analysis of a process based on liquid-liquid extraction for the recovery of glycols from aqueous streams

    NARCIS (Netherlands)

    Garcia Chavez, L.Y.; Schuur, Boelo; de Haan, A.B.

    2013-01-01

    The recovery of monoethylene glycol (MEG) and 1,2-propylene glycol (PG) from aqueous streams via liquid–liquid extraction (LLE) using a tailor-made ionic liquid [TOA MNaph] is evaluated as an alternative technology to conventional triple effect evaporation of water. In this paper, the conceptual

  17. Extraction of cashew (Anacardium occidentale) nut shell liquid using supercritical carbon dioxide.

    Science.gov (United States)

    Patel, Rajesh N; Bandyopadhyay, Santanu; Ganesh, Anuradda

    2006-04-01

    This work investigated the extraction of cashew nut shell liquid (CNSL) using supercritical carbon dioxide (SC-CO(2)). Effects of process parameters such as extraction pressure, temperature and flow rate of SC-CO(2) were investigated. The yield of CNSL increased with increase in pressure, temperature and mass flow rate of SC-CO(2). However, under different operating conditions, the composition of CNSL varied. The study of physical properties and chemical composition of the oil obtained through super critical fluid extraction (SCFE) showed better quality as compared to the CNSL obtained through thermal route. Experimental results were compared with diffusion based mass transfer model. Based on this simple model, extraction time was optimized.

  18. Extraction of Amino-J Acid from Waste-water by Emulsion Liquid Membrane

    Institute of Scientific and Technical Information of China (English)

    潘碌亭

    2006-01-01

    The emulsion liquid membrane technique was used to extract amino-J acid from industrial dye waste-water. The effects of stirring speed, ratio of the emulsion to water (Rew), ratio of the oil to internal phase (Roi) and membrane phase components on the extraction rate were investigated and optimized. The results showed that the extraction rate of amino-J acid approached 97% when the stirring speed was 300 r/min, Rew 1:6, Roi 1:1, trioctylamine (TOA) 3 mL/100 mL kerosene, and methyl-didecyle-alcohol-acrylate (LMA-2) 3 g/100 mL kerosene, respectively. The extraction rate had not changed with the oil phase reused for times.

  19. Characterization of paprika (Capsicum annuum) extract in orange juices by liquid chromatography of carotenoid profiles.

    Science.gov (United States)

    Mouly, P P; Gaydou, E M; Corsetti, J

    1999-03-01

    The carotenoid pigment profiles of authentic pure orange juices from Spain and Florida and an industrial paprika (Capsicum annuum) extract used for food coloring were obtained using reversed-phase liquid chromatography with a C18 packed column and an acetone/methanol/water eluent system. The procedure involving the carotenoid extraction is described. Both retention times and spectral properties using photodiode array detection for characterization of the major carotenoids at 430 and 519 nm are given. The influence of external addition of tangerine juice and/or paprika extract on orange juice color is described using the U.S. Department of Agriculture scale and adulterated orange juice. The procedure for quantitation of externally added paprika extract to orange juice is investigated, and the limit of quantitation, coefficient of variation, and recoveries are determined.

  20. Determination of capsaicinoids and eugenol in waste-edible-oil by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry%液-液萃取-液相色谱-串联质谱法测定"地沟油"中辣椒碱类化合物及丁香酚

    Institute of Scientific and Technical Information of China (English)

    张忠; 任飞; 张盼

    2012-01-01

    建立了"地沟油"中辣椒碱类化合物(包括辣椒素、二氢辣椒素、合成辣椒素)及丁香酚的液-液萃取及液相色谱-串联质谱(LC-MS/MS)检测方法."地沟油"中辣椒碱类化合物及丁香酚用甲醇萃取,采用SUPEL COSIL ABZ + Plus dC18色谱柱(150 mm ×4.6 mm,5 μm)分离,电喷雾离子源在正、负离子模式下电离,多反应监测(MRM)模式扫描.对辣椒素、二氢辣椒素、合成辣椒素及丁香酚的检出限分别为0.02、0.03、0.03和0.6μg/L,且在一定的质量浓度范围内线性良好.同一操作人员与不同操作人员间测定的精密度低于5%.该方法专属性强、灵敏、准确,可以作为"地沟油"的判定标准之一.%A method was developed for the determination of capsaicinoids ( capsaicin, dihydrocapsaicin and synthetic capsaicin) and eugenol in waste-edible-oil extracted by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry ( LC-MS/MS). The capsaicinoids and eugenol in waste-edible-oil were extracted by methanol, and then separated by a SUPEL COSIL ABZ +Plus dC18 column (150 mm x4. 6 mm, 5 ^m). The analysis was performed by MS/MS with electrospray ionization in positive and negative ion modes with multiple reaction monitoring (MRM). The limits of detection for capsaicin, dihydrocapsaicin, synthetic capsaicin and eugenol were 0.02, 0.03, 0.03 and 0. 6 n.g/L, respectively. The good linear relationships were obtained in certain concentration ranges of capsaicinoids and eugenol. The relative standard deviations (RSDs, n - 5) of same-worker and different-worker were less than 5%. The method is exclusive, sensitive and accurate, and can be used in waste-edible-oil determination.

  1. Micro-electromembrane extraction across free liquid membranes. Instrumentation and basic principles.

    Science.gov (United States)

    Kubáň, Pavel; Boček, Petr

    2014-06-13

    A micro-electromembrane extraction (μ-EME) technique using electrically induced transfer of charged analytes across free liquid membranes (FLMs) was presented. A disposable extraction unit was proposed and it was made of a short segment of transparent perfluoroalkoxy tubing, which was successively filled with three liquid plugs serving as acceptor solution, FLM and donor solution. These plugs formed a three-phase extraction system, which was precisely defined, that was stable and required μL to sub-μL volumes of all respective solutions. Basic instrumental set-up and extraction principles of μ-EME were examined using an anionic and a cationic dye, 4,5-dihydroxy-3-(p-sulfophenylazo)-2,7-naphthalene disulfonic acid trisodium salt (SPADNS) and crystal violet, respectively. Transfers of the charged dyes from donor into acceptor solutions across FLMs consisting of 1-pentanol were visualized by a microscope camera and quantitative measurements were performed by UV-vis spectrophotometry. The effects of operational parameters of μ-EME system were comprehensively investigated and experimental measurements were accompanied with theoretical calculations. Extraction recoveries above 60% were achieved for 5min μ-EME of 1mM SPADNS at 100V with repeatability values below 5%. Selectivity of FLMs was additionally examined by capillary electrophoretic analyses of acceptor solutions and the potential of FLMs for μ-EME pretreatment of samples with artificial complex matrices was demonstrated. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Intravascular Residence Time Determination for the Cyanide Antidote Dimethyl Trisulfide in Rat by Using Liquid-Liquid Extraction Coupled with High Performance Liquid Chromatography

    Science.gov (United States)

    De Silva, Deepthika; Lee, Steven; Duke, Anna; Angalakurthi, Siva; Chou, Ching-En; Ebrahimpour, Afshin; Thompson, David E.

    2016-01-01

    These studies represent the first report on the intravascular residence time determinations for the cyanide antidote dimethyl trisulfide (DMTS) in a rat model by using high performance liquid chromatography coupled with ultraviolet absorption spectroscopy (HPLC-UV). The newly developed sample preparation included liquid-liquid extraction by cyclohexanone. The calibration curves showed a linear response for DMTS concentrations between 0.010 and 0.30 mg/mL with R2 = 0.9994. The limit of detection for DMTS via this extraction method was 0.010 mg/mL, and the limit of quantitation was 0.034 mg/mL. Thus this calibration curve provided a tool for determining DMTS in the range between 0.04 and 0.30 mg/mL. Rats were given 20 mg/kg DMTS dose (in 15% Polysorbate 80) intravenously, and blood samples were taken 15, 60, 90, 120, and 240 min after DMTS injections. The data points were plotted as DMTS concentration in RBCs versus time, and the intravascular residence time was determined graphically. The results indicated a half-life of 36 min in a rat model, suggesting that the circulation time is long enough to provide a reasonable time interval for cyanide antagonism. PMID:28053802

  3. Intravascular Residence Time Determination for the Cyanide Antidote Dimethyl Trisulfide in Rat by Using Liquid-Liquid Extraction Coupled with High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Deepthika De Silva

    2016-01-01

    Full Text Available These studies represent the first report on the intravascular residence time determinations for the cyanide antidote dimethyl trisulfide (DMTS in a rat model by using high performance liquid chromatography coupled with ultraviolet absorption spectroscopy (HPLC-UV. The newly developed sample preparation included liquid-liquid extraction by cyclohexanone. The calibration curves showed a linear response for DMTS concentrations between 0.010 and 0.30 mg/mL with R2 = 0.9994. The limit of detection for DMTS via this extraction method was 0.010 mg/mL, and the limit of quantitation was 0.034 mg/mL. Thus this calibration curve provided a tool for determining DMTS in the range between 0.04 and 0.30 mg/mL. Rats were given 20 mg/kg DMTS dose (in 15% Polysorbate 80 intravenously, and blood samples were taken 15, 60, 90, 120, and 240 min after DMTS injections. The data points were plotted as DMTS concentration in RBCs versus time, and the intravascular residence time was determined graphically. The results indicated a half-life of 36 min in a rat model, suggesting that the circulation time is long enough to provide a reasonable time interval for cyanide antagonism.

  4. Estrogens determination in wastewater samples by automatic in-syringe dispersive liquid-liquid microextraction prior silylation and gas chromatography.

    Science.gov (United States)

    González, Alba; Avivar, Jessica; Cerdà, Víctor

    2015-09-25

    A new procedure for the extraction, preconcentration and simultaneous determination of the estrogens most used in contraception pharmaceuticals (estrone, 17β-estradiol, estriol, and 17α-ethynylestradiol), cataloged as Contaminants of Emergent Concern by the Environmental Protection Agency of the United States (US-EPA), is proposed. The developed system performs an in-syringe magnetic stirring-assisted dispersive liquid-liquid microextraction (in-syringe-MSA-DLLME) prior derivatization and gas chromatography (GC-MS). Different extraction (carbon tetrachloride, ethyl acetate, chloroform and trichloroethylene) and disperser solvents (acetone, acetonitrile and methanol) were tested. Chloroform and acetone were chosen as extraction and disperser solvent, respectively, as they provided the best extraction efficiency. Then, a multivariate optimization of the extraction conditions was carried out. Derivatization conditions were also studied to ensure the conversion of the estrogens to their respective trimethylsilyl derivatives. Low LODs and LOQs were achieved, i.e. between 11 and 82ngL(-1), and 37 and 272ngL(-1), respectively. Good values for intra and inter-day precision were obtained (RSDs≤7.06% and RSD≤7.11%, respectively). The method was successfully applied to wastewater samples.

  5. Parallel artificial liquid membrane extraction as an efficient tool for removal of phospholipids from human plasma

    DEFF Research Database (Denmark)

    Ask, Kristine Skoglund; Bardakci, Turgay; Parmer, Marthe Petrine

    2016-01-01

    Generic Parallel Artificial Liquid Membrane Extraction (PALME) methods for non-polar basic and non-polar acidic drugs from human plasma were investigated with respect to phospholipid removal. In both cases, extractions in 96-well format were performed from plasma (125μL), through 4μL organic solv...... matrix effects were investigated with fluoxetine, fluvoxamine, and quetiapine as model analytes. No signs of matrix effects were observed. Finally, PALME was evaluated for the aforementioned drug substances, and data were in accordance with European Medicines Agency (EMA) guidelines....

  6. Foaming and rheological properties of the liquid phase extracted from wheat flour dough

    OpenAIRE

    2015-01-01

    Dough liquor (DL) is considered as a good model of bread dough liquid phase which plays an important role in alveolar structure creation. In this work, DL was extracted from dough pieces of various contents (g for 100 g flour) of water (55-70), sugar (0-15), rapeseed oil (0-10) and bran (0-20). The extraction yield of DL was 5.0 +/- 2.4% and its dry matter content varied between 10.8 and 27.2% of total DL mass. Its composition has been determined in terms of lipids content (

  7. Molecular dynamics simulations of hydrophobous ions at the liquid-liquid interfaces: case of dicarbollide anions as synergy agents and of ionic liquids as extracting medium; Simulations par dynamique moleculaire d'ions hydrophobes aux interfaces liquide - liquide: le cas des anions dicarbollides comme agents de synergie et celui des liquides ioniques comme milieu extractant

    Energy Technology Data Exchange (ETDEWEB)

    Chevrot, G

    2008-01-15

    Based on molecular dynamics simulations, we first describe the distribution of dicarbollide salts (CCD{sup -}, Mn{sup +}) in concentrated monophasic solutions (water, chloroform, octanol, nitrobenzene) and in the corresponding biphasic 'oil' - water solutions. We point to the importance of surface activity of the CCD{sup -}s and of their self-aggregation in water, with marked counterions effects, and we explain the synergistic effect of CCD{sup -}s in the Eu{sup 3+} extraction by BTP ligands. In the second part of the thesis we report exploratory simulations on the extraction of Sr{sup 2+} by 18-crown-6 to an hydrophobic ionic liquid ([BMI][PF6]), focusing on the liquid - liquid interface. Analogies and differences with a classical aqueous interface are outlined. (author)

  8. Identical extraction behavior and coordination of trivalent or hexavalent f-element cations using ionic liquid and molecular solvents.

    Science.gov (United States)

    Cocalia, Violina A; Jensen, Mark P; Holbrey, John D; Spear, Scott K; Stepinski, Dominique C; Rogers, Robin D

    2005-06-07

    The extraction of both UO2(2+) and trivalent lanthanide and actinide ions (Am3+, Nd3+, Eu3+) by dialkylphosphoric or dialkylphosphinic acids from aqueous solutions into the ionic liquid, 1-decyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide has been studied and compared to extractions into dodecane. Radiotracer partitioning measurements show comparable patterns of distribution ratios for both the ionic liquid/aqueous and dodecane/aqueous systems, and the limiting slopes at low acidity indicate the partitioning of neutral complexes in both solvent systems. The metal ion coordination environment, elucidated from EXAFS and UV-visible spectroscopy measurements, is equivalent in the ionic liquid and dodecane solutions with coordination of the uranyl cation by two hydrogen-bonded extractant dimers, and of the trivalent cations by three extractant dimers. This is the first definitive report of a system where both the biphasic extraction equilibria and metal coordination environment are the same in an ionic liquid and a molecular organic solvent.

  9. Neodymium(III) Complexes of Dialkylphosphoric and Dialkylphosphonic Acids Relevant to Liquid-Liquid Extraction Systems

    Energy Technology Data Exchange (ETDEWEB)

    Lumetta, Gregg J.; Sinkov, Sergey I.; Krause, Jeanette A.; Sweet, Lucas E.

    2016-01-27

    The complexes formed during the extraction of neodymium(III) into hydrophobic solvents containing acidic organophosphorus extractants were probed by single-crystal X-ray diffractometry, visible spectrophotometry, and Fourier-transform infrared spectroscopy. The crystal structure of the compound Nd(DMP)3 (1, DMP = dimethyl phosphate) revealed a polymeric arrangement in which each Nd(III) center is surrounded by six DMP oxygen atoms in a pseudo-octahedral environment. Adjacent Nd(III) ions are bridged by (MeO)2POO– anions, forming the polymeric network. The diffuse reflectance visible spectrum of 1 is nearly identical to that of the solid that is formed when an n-dodecane solution of di-(2-ethylhexyl)phosphoric acid (HA) is saturated with Nd(III), indicating a similar coordination environment around the Nd center in the NdA3 solid. The visible spectrum of the HA solution fully loaded with Nd(III) is very similar to that of the NdA3 material, both displaying hypersensitive bands characteristic of an pseudo-octahedral coordination environment around Nd. These spectral characteristics persisted across a wide range of organic Nd concentrations, suggesting that the pseudo-octahedral coordination environment is maintained from dilute to saturated conditions.

  10. Fractionation of Gibberellins in plant extracts by reverse phase high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Jones, M.G.; Metzger, J.D.; Zeevaart, J.A.D.

    1980-02-01

    In studies on endogenous plant gibberellins (GAs), reverse phase (Bondapak C/sub 18/) high performance liquid chromatography (HPLC) has proved to be a useful method for the fractionation of plant extracts. The behavior of 18 authentic GAs in such a chromatographic system is described. The main factors determining chromatographic behavior are the degree and the position of hydroxylation of the GA. As an illustration of the use of reverse phase HPLC, the endogeneous GAs of immature seeds of Pharbitis nil L., strain Violet, were reinvestigated. The presence of gibberellins A/sub 3/, A/sub 5/, A/sub 17/, A/sub 20/, and A/sub 29/ was confirmed by gas-liquid chromatography-mass spectrometry. In addition, two other GAs, A/sub 19/ and A/sub 44/, were also identified in extracts of this material.

  11. Liquid phase micro-extraction: Towards the green methodology for ultratrace metals determination in aquatic ecosystems

    Directory of Open Access Journals (Sweden)

    López-López J. A.

    2013-04-01

    Full Text Available Heavy metals are normally found, in natural waters, in very low concentrations. Some of them are essential for life in low level; however, in higher level they are toxic. Therefore, analyzing their bio-available fraction is of main interest. Standard methodology is based in the collection of a number of samples from a water body. Collected samples must be stored, pre-treated and then analyzed. Pre-treatment usually involves pre-concentrating the metal, with the corresponding risk of contamination or loss of analyte. This way, punctual information is obtained from every sampling campaign. As an alternative, passive sampling techniques allow the continuous and coupled sampling-pre-treatment for heavy metals analysis, giving a better approach in the characterization of the studied water body. Liquid phase micro-extraction (LPME is a green analytical alternative for liquid-liquid extraction that promotes a reduction of sample volume, solvent needed and waste generation. Using these systems, polypropylene hollow fibers (HF with pores in their walls can be used. A few micro-liters of organic solvent are supported in the pores. The sample is placed in the outer part of the fiber and a receiving phase is placed in its inner part, allowing continuous liquid extraction of the metal from the sample. Several fibers with different physical features have been employed to analyzed total concentration and bio-availability of some heavy metals (Ag, Ni, Cu in natural water samples. Thanks to fibers configuration, devices for passive sampling based in HF-LPME could be designed. Advantages of this methodology over existing ones are supported because the receiving phase is liquid. As a consequence, retained metals do not need to be eluted from the acceptor prior to instrumental analysis.

  12. Combined liquid and solid-phase extraction improves quantification of brain estrogen content

    Directory of Open Access Journals (Sweden)

    Andrew eChao

    2011-09-01

    Full Text Available Accuracy in quantifying brain-derived steroid hormones (‘neurosteroids’ has become increasingly important for understanding the modulation of neuronal activity, development, and physiology. Relative to other neuroactive compounds and classical neurotransmitters, steroids pose particular challenges with regard to isolation and analysis, owing to their lipid solubility. Consequently, anatomical studies of the distribution of neurosteroids have relied primarily on the expression of neurosteroid synthesis enzymes. To evaluate the distribution of synthesis enzymes vis-à-vis the actual steroids themselves, traditional steroid quantification assays, including radioimmunoassays (RIA, have successfully employed liquid extraction methods (e.g., ether, dichloromethane or methanol to isolate steroids from microdissected brain tissue. Due to their sensitivity, safety and reliability, the use of commercial enzyme immunoassays (EIA for laboratory quantification of steroids in plasma and brain has become increasingly widespread. However, EIAs rely on enzymatic reactions in vitro, making them sensitive to interfering substances in brain tissue and thus producing unreliable results. Here, we evaluate the effectiveness of a protocol for combined, two-stage liquid/solid phase extraction as compared to conventional liquid extraction alone for the isolation of estradiol (E2 from brain tissue. We employ the songbird model system, in which brain steroid production is pronounced and linked to neural mechanisms of learning and plasticity. This study outlines a combined liquid-solid phase extraction protocol that improves the performance of a commercial EIA for the quantification of brain E2 content. We demonstrate the effectiveness of our optimized method for evaluating the region specificity of brain E2 content, compare these results to established anatomy of the estrogen synthesis enzyme and estrogen receptor, and discuss the nature of potential EIA interfering

  13. Multi-phase extraction of glycoraphanin from broccoli using aminium ionic liquid-based silica.

    Science.gov (United States)

    Tian, Minglei; Bi, Wentao; Row, Kyung Ho

    2013-01-01

    Glucosinolates, a class of phytochemicals found in broccoli, have attracted recent interest due to the potential health benefits associated with their dietary intake. Glucoraphanin, the most common glucosinolate in broccoli can be converted to a known cancer chemopreventive agent. Multi-phase extraction in solid-phase extraction cartridges was developed to simultaneously extract and separate this compound. Multi-phase extraction with functionalised ionic liquid-based silica as a sorbent was used to simultaneously extract and separate glucoraphanin from broccoli. The sorbent and broccoli sample were packed into a single cartridge, and a fixed volume of water was then used to extract and remove the target compound from the sample to the sorbent over 15 repetitions. The sorbent was then washed with n-hexane to remove any interference and the target compound was eluted with water-1% acetic acid (vol.). Under the optimised condition, 0.038 mg/g of glucoraphanin was obtained by multi-phase extraction with 0.2 g of sorbent. The adsorption isotherm allowed investigation of the interactions between the sorbent and target compound and provided evidence for the accuracy of this method. The low deviation error, small amount of solvents required, highly selective separation and stability of the method justify further research. Copyright © 2012 John Wiley & Sons, Ltd.

  14. Pressurized liquid extraction of Aglaonema sp. iminosugars: Chemical composition, bioactivity, cell viability and thermal stability.

    Science.gov (United States)

    Rodríguez-Sánchez, S; Martín-Ortiz, A; Carrero-Carralero, C; Ramos, S; Sanz, M L; Soria, A C

    2016-08-01

    Pressurized liquid extraction of Aglaonema sp. iminosugars has been optimized. A single cycle under optimal conditions (80mg, 100°C, 2min) was enough to extract ⩾96% of most iminosugars. Further incubation with Saccharomyces cerevisiae for 5h removed coextracted interfering low molecular weight carbohydrates from extracts of different Aglaonema cultivars. A complete characterization of these extracts was carried out by gas chromatography-mass spectrometry: three iminosugars were tentatively identified for the first time; α-homonojirimycin and 2,5-dideoxy-2,5-imino-d-mannitol were the major iminosugars determined. α-Glucosidase inhibition activity, cell viability and thermal stability of Aglaonema extracts were also evaluated. Extracts with IC50 for α-glucosidase activity in the 0.010-0.079mgmL(-1) range showed no decrease of Caco-2 cell viability at concentrations lower than 125μgmL(-1) and were stable at 50°C for 30days. These results highlight the potential of Aglaonema extracts as a source of bioactives to be used as functional ingredients.

  15. Hard cap espresso extraction and liquid chromatography determination of bioactive compounds in vegetables and spices.

    Science.gov (United States)

    Martinez-Sena, María Teresa; de la Guardia, Miguel; Esteve-Turrillas, Francesc A; Armenta, Sergio

    2017-12-15

    A new analytical procedure, based on liquid chromatography with diode array and fluorescence detection, has been proposed for the determination of bioactive compounds in vegetables and spices after hard cap espresso extraction. This novel extraction system has been tested for the determination of capsaicin and dihydrocapsaicin from fresh chilli and sweet pepper, piperine from ground pepper, curcumin from turmeric and curry, and myristicin from nutmeg. Extraction efficiency was evaluated by using acetonitrile:water and ethanol:water mixtures. The proposed method allows the extraction of samples with 100mL of 60% (v/v) ethanol in water. The obtained limits of quantification for the proposed procedure ranged from 0.07 to 0.30mgg(-1) and results were statistically comparable with those obtained by ultrasound assisted extraction. Hard cap espresso machines offer a fast, effective and quantitative tool for the extraction of bioactive compounds from food samples with an extraction time lower than 30s, using a global available and low cost equipment. Copyright © 2017 Elsevier Ltd. All rights reserved.

  16. Chemical constituents and antioxidant activities of waste liquid extract from Apostichopus japonicus Selenka processing

    Institute of Scientific and Technical Information of China (English)

    LI Chaofeng; LI Xiancui; LI Hong; GUO Shuju; ZHU Xiaobin

    2013-01-01

    Apostichopus japonicus Selenka is an ideal tonic food that is used traditionally in many Asian countries,and it contains many bioactive substances,such as antioxidant,antimicrobial,and anticancer materials.To convert waste liquid generated during production into a useful resource,extract from waste liquid was isolated by column chromatography and studied by the pyrogallol autoxidation and 1,10-phenanthroline-Fe2+ oxidation methods.Results show that the extract scavenged about 91% of the superoxide anion radical at a concentration of 1.4 mg/mL and 24% of the hydroxyl radical at 3.3 mg/mL.Four compounds were isolated and identified from the extract:2,4-dihydroxy-5-methyl-1,3-azine; 2,4-dihydroxy-1,3-diazine; 3-O-[β-D-quinovopranosyl-(1→2)-4-O-sodium sulfate-β-D-xylopranosyl]-holosta-9(11)-ene-3β,12t,17α-triol; and 24-ethyl-5t-cholesta-7-ene-3β-O-β-D-xylopyranoside.All of these compounds are known in A.japonicus,and were found in the waste liquid for the first time.

  17. Ionic liquid based dispersive liquid-liquid microextraction coupled with micro-solid phase extraction of antidepressant drugs from environmental water samples.

    Science.gov (United States)

    Ge, Dandan; Lee, Hian Kee

    2013-11-22

    Ionic liquid-dispersive liquid-liquid microextraction combined with micro-solid phase extraction (IL-DLLME-μ-SPE), and high-performance liquid chromatography (HPLC) was developed for the determination of tricyclic antidepressants (TCAs) in water samples. Two hundred microliters of an organic solvent (as disperser solvent) and 20 μl of 1-hexyl-3-methylimidazolium tris(pentafluoroethyl)trifluorophosphate were injected into a 5.0 ml sample for sonication-assisted DLLME. After this, a μ-SPE device, containing a novel material zeolite imidazolate framework 4 (ZIF-4), was added into the sample solution and 1 min of vortex-assisted extraction was performed. After 5 min of sonication-assisted desorption, 10 μl of desorption solvent was injected into a HPLC system for analysis. A characteristic property of DLLME-VA-μ-SPE is that any organic solvent and solid sorbent immiscible with water can be used. Special apparatus, or conical-bottom test tubes, and tedious procedures conventionally associated with DLLME such as centrifugation, or refrigeration of solvent are not necessary in the present approach. A novel material, ZIF-4 was employed as μ-SPE sorbent. Under the optimized conditions, the calibration curves were linear in the range of 1-1000 μg/L. The relative standard deviations and the limits of detection were in the range of 1.5% and 7.8% and 0.3 and 1 μg/L, respectively. The relative recoveries of canal water samples, spiked with drugs, were in the range of 94.3% and 114.7%. The results showed that IL-DLLME-μ-SPE was suitable for the determination of TCAs in water samples.

  18. Electrochemical assessment of water|ionic liquid biphasic systems towards cesium extraction from nuclear waste.

    Science.gov (United States)

    Stockmann, T Jane; Zhang, Jing; Montgomery, Anne-Marie; Ding, Zhifeng

    2014-04-22

    A room temperature ionic liquid (IL) composed of a quaternary alkylphosphonium (trihexyltetradecylphosphonium, P66614(+)) and tetrakis(pentafluorophenyl)borate anion (TB(-)) was employed within a water|P66614TB (w|P66614TB or w|IL) biphasic system to evaluate cesium ion extraction in comparison to that with a traditional water|organic solvent (w|o) combination. (137)Cs is a major contributor to the radioactivity of spent nuclear fuel as it leaves the reactor, and its extraction efficiency is therefore of considerable importance. The extraction was facilitated by the ligand octyl(phenyl)-N,N'-diisobutylcarbamoylphosphine oxide (CMPO) used in TRans-Uranium EXtraction processes and investigated through well established liquid|liquid electrochemistry. This study gave access to the metal ion to ligand (1:n) stoichiometry and overall complexation constant, β, of the interfacial complexation reaction which were determined to be 1:3 and 1.6×10(11) at the w|P66614TB interface while the study at w|o elicited an n equal to 1 with β equal to 86.5. Through a straightforward relationship, these complexation constant values were converted to distribution coefficients, δ(α), with the ligand concentrations studied for comparison to other studies present in the literature; the w|o and w|IL systems gave δ(α) of 2 and 8.2×10(7), respectively, indicating a higher overall extraction efficiency for the latter. For the w|o system, the metal ion-ligand stoichiometries were confirmed through isotopic distribution analysis of mass spectra obtained by the direct injection of an emulsified water-organic solvent mixture into an electron spray ionization mass spectrometer.

  19. Extraction of copper(II) ions from aqueous solutions with a methimazole-based ionic liquid.

    Science.gov (United States)

    Reyna-González, Juan M; Torriero, Angel A J; Siriwardana, Amal I; Burgar, Iko M; Bond, Alan M

    2010-09-15

    The recently synthesized ionic liquid (IL) 2-butylthiolonium bis(trifluoromethanesulfonyl)amide, [mimSBu][NTf(2)], has been used for the extraction of copper(II) from aqueous solution. The pH of the aqueous phase decreases upon addition of [mimSBu](+), which is attributed to partial release of the hydrogen attached to the N(3) nitrogen atom of the imidazolium ring. The presence of sparingly soluble water in [mimSBu][NTf(2)] also is required in solvent extraction studies to promote the incorporation of Cu(II) into the [mimSBu][NTf(2)] ionic liquid phase. The labile copper(II) system formed by interacting with both the water and the IL cation component has been characterized by cyclic voltammetry as well as UV-vis, Raman, and (1)H, (13)C, and (15)N NMR spectroscopies. The extraction process does not require the addition of a complexing agent or pH control of the aqueous phase. [mimSBu][NTf(2)] can be recovered from the labile copper-water-IL interacting system by washing with a strong acid. High selectivity of copper(II) extraction is achieved relative to that of other divalent cobalt(II), iron(II), and nickel(II) transition-metal cations. The course of microextraction of Cu(2+) from aqueous media into the [mimSBu][NTf(2)] IL phase was monitored in situ by cyclic voltammetry using a well-defined process in which specific interaction with copper is believed to switch from the ionic liquid cation component, [mimSBu], to the [NTf(2)] anion during the course of electrochemical reduction from Cu(II) to Cu(I). The microextraction-voltammetry technique provides a fast and convenient method to determine whether an IL is able to extract electroactive metal ions from an aqueous solution.

  20. Screen-printed electrode based electrochemical detector coupled with ionic liquid dispersive liquid-liquid microextraction and microvolume back-extraction for determination of mercury in water samples.

    Science.gov (United States)

    Fernández, Elena; Vidal, Lorena; Martín-Yerga, Daniel; Blanco, María del Carmen; Canals, Antonio; Costa-García, Agustín

    2015-04-01

    A novel approach is presented, whereby gold nanostructured screen-printed carbon electrodes (SPCnAuEs) are combined with in-situ ionic liquid formation dispersive liquid-liquid microextraction (in-situ IL-DLLME) and microvolume back-extraction for the determination of mercury in water samples. In-situ IL-DLLME is based on a simple metathesis reaction between a water-miscible IL and a salt to form a water-immiscible IL into sample solution. Mercury complex with ammonium pyrrolidinedithiocarbamate is extracted from sample solution into the water-immiscible IL formed in-situ. Then, an ultrasound-assisted procedure is employed to back-extract the mercury into 10 µL of a 4 M HCl aqueous solution, which is finally analyzed using SPCnAuEs. Sample preparation methodology was optimized using a multivariate optimization strategy. Under optimized conditions, a linear range between 0.5 and 10 µg L(-1) was obtained with a correlation coefficient of 0.997 for six calibration points. The limit of detection obtained was 0.2 µg L(-1), which is lower than the threshold value established by the Environmental Protection Agency and European Union (i.e., 2 µg L(-1) and 1 µg L(-1), respectively). The repeatability of the proposed method was evaluated at two different spiking levels (3 and 10 µg L(-1)) and a coefficient of variation of 13% was obtained in both cases. The performance of the proposed methodology was evaluated in real-world water samples including tap water, bottled water, river water and industrial wastewater. Relative recoveries between 95% and 108% were obtained. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Development of sample preparation method for eleutheroside B and E analysis in Acanthopanax senticosus by ionic liquids-ultrasound based extraction and high-performance liquid chromatography detection.

    Science.gov (United States)

    Yang, Lei; Ge, Hongshuang; Wang, Wenjie; Zu, Yuangang; Yang, Fengjian; Zhao, Chunjian; Zhang, Lin; Zhang, Ying

    2013-12-01

    An ionic liquids-based ultrasonic-assisted extraction (ILUAE) method was successfully developed for extracting eleutheroside B and E from Radix Acanthopanax senticosus. Thirteen 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were investigated and 1-butyl-3-methylimidazolium bromide ([C4mim]Br) solution was selected as the solvent. The conditions for ILUAE, including the ionic liquid concentration, soaking time, ultrasonic power, ultrasonic time, solid-liquid ratio and number of extraction cycles, were optimized. With the proposed method, the energy consumption time was reduced to 30 min, whereas conventional method requires about 4h. The proposed method had good recovery (97.96-103.39%) and reproducibility (RSD, n=5; 3.3% for eleutheroside B, 4.6% for eleutheroside E). ILUAE was an efficient, rapid and simple sample preparation technique that showed high reproducibility and was environmental friendly.

  2. Liquid-liquid extraction of cadmium(II) by TIOACl (tri-iso-octyl ammonium chloride) ionic liquid and its application to a TIOACl impregnated carbon nanotubes system

    Energy Technology Data Exchange (ETDEWEB)

    Alguacil, F. J.; Garcia-Diaz, I.; Lopez, F. A.; Rodriguez, O.

    2015-07-01

    The extraction of cadmium(II) by the ionic liquid (R{sub 3}NH{sup +}Cl{sup -}) (R: tri-iso-octyl) in Exxsol D100 from hydrochloric acid solution has been investigated. The extraction reaction is exothermic. The numerical analysis of metal distribution data suggests the formation of R{sub 3}NH{sup +}CdCl{sup -}{sub 3} - and (R{sub 3}NH{sup +}){sub 2}CdCl{sub 4}{sup 2}- species in the organic phase. The results obtained for cadmium(II) distribution have been implemented in an impregnated multi-walled carbon nanotubes system. The influence of aqueous solution stirring speed (250-2000 min{sup -}1), adsorbent dosage (0.05-0.2 g) and temperature (20 degree centigrade-60 degree centigrade) on cadmium adsorption have been investigated. (Author)

  3. Liquid Phase Micro-Extraction of Linear Alkylbenzene Sulfonate Anionic Surfactants in Aqueous Samples

    Directory of Open Access Journals (Sweden)

    Jan Åke Jönsson

    2011-10-01

    Full Text Available Hollow fiber liquid phase micro-extraction (LPME of linear alkylbenzene sulfonates (LAS from aqueous samples was studied. Ion pair extraction of C10, C11, C12 and C13 homologues was facilitated with trihexylamine as ion-pairing agent, using di-n-hexylether as solvent for the supported liquid membrane (SLM. Effects of extraction time, acceptor buffer concentration, stirring speed, sample volume, NaCl and humic acids were studied. At 10–50 µg L−1 linear R2-coefficients were 0.99 for C10 and C11 and 0.96 for C12. RSD was typically ~15%. Three observations were especially made. Firstly, LPME for these analytes was unusually slow with maximum enrichment observed after 15–24 h (depending on sample volume. Secondly, the enrichment depended on LAS sample concentration with 35–150 times enrichment below ~150 µg L−1 and 1850–4400 times enrichment at 1 mg L−1. Thirdly, lower homologues were enriched more than higher homologues at low sample concentrations, with reversed conditions at higher concentrations. These observations may be due to the fact that LAS and the amine counter ion themselves influence the mass transfer at the water-SLM interface. The observations on LPME of LAS may aid in LPME application to other compounds with surfactant properties or in surfactant enhanced membrane extraction of other compounds.

  4. Liquid phase micro-extraction of linear alkylbenzene sulfonate anionic surfactants in aqueous samples.

    Science.gov (United States)

    Larsson, Niklas; Otrembska, Paulina; Villar, Mercedes; Jönsson, Jan Åke

    2011-10-13

    Hollow fiber liquid phase micro-extraction (LPME) of linear alkylbenzene sulfonates (LAS) from aqueous samples was studied. Ion pair extraction of C10, C11, C12 and C13 homologues was facilitated with trihexylamine as ion-pairing agent, using di-n-hexylether as solvent for the supported liquid membrane (SLM). Effects of extraction time, acceptor buffer concentration, stirring speed, sample volume, NaCl and humic acids were studied. At 10-50 µg L-1 linear R2-coefficients were 0.99 for C10 and C11 and 0.96 for C12. RSD was typically ~15%. Three observations were especially made. Firstly, LPME for these analytes was unusually slow with maximum enrichment observed after 15-24 h (depending on sample volume). Secondly, the enrichment depended on LAS sample concentration with 35-150 times enrichment below ~150 µg L-1 and 1850-4400 times enrichment at 1 mg L-1. Thirdly, lower homologues were enriched more than higher homologues at low sample concentrations, with reversed conditions at higher concentrations. These observations may be due to the fact that LAS and the amine counter ion themselves influence the mass transfer at the water-SLM interface. The observations on LPME of LAS may aid in LPME application to other compounds with surfactant properties or in surfactant enhanced membrane extraction of other compounds.

  5. Liquid-liquid extraction of biomolecules in downstream processing - A review paper

    Directory of Open Access Journals (Sweden)

    M. E. Silva

    2000-03-01

    Full Text Available Economic analysis shows that protein separation and purification are a very important aspect of biomolecules production and processing. This is particularly true for protein processing which, because of the complexity of the starting material, often requires many steps to reach the levels of purity required for medical and food applications. The separation specialists' task is to develop safe and simple processes to achieve products with a high level of purity. On a large scale, chromatography of proteins is not an easily applied method, although on a laboratory scale it is very effective and relatively simple. When it is scaled up, shortcomings such as discontinuity in the process, slow protein diffusion and large pressure drops in the system are seen. For these reasons a substantial research effort has been directed toward the use of aqueous two-phase systems (ATPSs to replace the initial steps in protein purification and chromatography. This article reviews the chronology and main ATPS fundamentals and discuss the broader applications of this type of system in the extraction and separation of biomolecules.

  6. Extraction of DNA by magnetic ionic liquids: tunable solvents for rapid and selective DNA analysis.

    Science.gov (United States)

    Clark, Kevin D; Nacham, Omprakash; Yu, Honglian; Li, Tianhao; Yamsek, Melissa M; Ronning, Donald R; Anderson, Jared L

    2015-02-03

    DNA extraction represents a significant bottleneck in nucleic acid analysis. In this study, hydrophobic magnetic ionic liquids (MILs) were synthesized and employed as solvents for the rapid and efficient extraction of DNA from aqueous solution. The DNA-enriched microdroplets were manipulated by application of a magnetic field. The three MILs examined in this study exhibited unique DNA extraction capabilities when applied toward a variety of DNA samples and matrices. High extraction efficiencies were obtained for smaller single-stranded and double-stranded DNA using the benzyltrioctylammonium bromotrichloroferrate(III) ([(C8)3BnN(+)][FeCl3Br(-)]) MIL, while the dicationic 1,12-di(3-hexadecylbenzimidazolium)dodecane bis[(trifluoromethyl)sulfonyl]imide bromotrichloroferrate(III) ([(C16BnIM)2C12(2+)][NTf2(-), FeCl3Br(-)]) MIL produced higher extraction efficiencies for larger DNA molecules. The MIL-based method was also employed for the extraction of DNA from a complex matrix containing albumin, revealing a competitive extraction behavior for the trihexyl(tetradecyl)phosphonium tetrachloroferrate(III) ([P6,6,6,14(+)][FeCl4(-)]) MIL in contrast to the [(C8)3BnN(+)][FeCl3Br(-)] MIL, which resulted in significantly less coextraction of albumin. The MIL-DNA method was employed for the extraction of plasmid DNA from bacterial cell lysate. DNA of sufficient quality and quantity for polymerase chain reaction (PCR) amplification was recovered from the MIL extraction phase, demonstrating the feasibility of MIL-based DNA sample preparation prior to downstream analysis.

  7. Antioxidant White Grape Seed Phenolics: Pressurized Liquid Extracts from Different Varieties

    Directory of Open Access Journals (Sweden)

    Carmen Garcia-Jares

    2015-11-01

    Full Text Available Grape seeds represent a high percentage (20% to 26% of the grape marc obtained as a byproduct from white winemaking and keep a vast proportion of grape polyphenols. In this study, seeds obtained from 11 monovarietal white grape marcs cultivated in Northwestern Spain have been analyzed in order to characterize their polyphenolic content and antioxidant activity. Seeds of native (Albariño, Caiño, Godello, Loureiro, Torrontés, and Treixadura and non-native (Chardonnay, Gewurtzträminer, Pinot blanc, Pinot gris, and Riesling grape varieties have been considered. Low weight phenolics have been extracted by means of pressurized liquid extraction (PLE and further analyzed by LC-MS/MS. The results showed that PLE extracts, whatever the grape variety of origin, contained large amounts of polyphenols and high antioxidant activity. Differences in the varietal polyphenolic profiles were found, so a selective exploitation of seeds might be possible.

  8. Antioxidant White Grape Seed Phenolics: Pressurized Liquid Extracts from Different Varieties.

    Science.gov (United States)

    Garcia-Jares, Carmen; Vazquez, Alberto; Lamas, Juan P; Pajaro, Marta; Alvarez-Casas, Marta; Lores, Marta

    2015-11-19

    Grape seeds represent a high percentage (20% to 26%) of the grape marc obtained as a byproduct from white winemaking and keep a vast proportion of grape polyphenols. In this study, seeds obtained from 11 monovarietal white grape marcs cultivated in Northwestern Spain have been analyzed in order to characterize their polyphenolic content and antioxidant activity. Seeds of native (Albariño, Caiño, Godello, Loureiro, Torrontés, and Treixadura) and non-native (Chardonnay, Gewurtzträminer, Pinot blanc, Pinot gris, and Riesling) grape varieties have been considered. Low weight phenolics have been extracted by means of pressurized liquid extraction (PLE) and further analyzed by LC-MS/MS. The results showed that PLE extracts, whatever the grape variety of origin, contained large amounts of polyphenols and high antioxidant activity. Differences in the varietal polyphenolic profiles were found, so a selective exploitation of seeds might be possible.

  9. Quantitative spatial analysis of the mouse brain lipidome by pressurized liquid extraction surface analysis

    DEFF Research Database (Denmark)

    Almeida, Reinaldo; Berzina, Zane; Christensen, Eva Arnspang

    2015-01-01

    of internal lipid standards in the extraction solvent. The analysis of lipid microextracts by nanoelectrospray ionization provides long-lasting ion spray which in conjunction with a hybrid ion trap-orbitrap mass spectrometer enables identification and quantification of molecular lipid species using a method......Here we describe a novel surface sampling technique termed pressurized liquid extraction surface analysis (PLESA), which in combination with a dedicated high-resolution shotgun lipidomics routine enables both quantification and in-depth structural characterization of molecular lipid species...... with successive polarity shifting, high-resolution Fourier transform mass spectrometry (FTMS), and fragmentation analysis. We benchmarked the performance of the PLESA approach for in-depth lipidome analysis by comparing it to conventional lipid extraction of excised tissue homogenates and by mapping the spatial...

  10. Butanol fermentation from microalgae-derived carbohydrates after ionic liquid extraction.

    Science.gov (United States)

    Gao, Kai; Orr, Valerie; Rehmann, Lars

    2016-04-01

    Lipid extracted algae (LEA) is an attractive feedstock for alcohol fuel production as it is a non-food crop which is largely composed of readily fermented carbohydrates like starch rather than the more recalcitrant lignocellulosic materials currently under intense development. This study compares the suitability of ionic liquid extracted algae (ILEA) and hexane extracted algae (HEA) for acetone, butanol, and ethanol (ABE) fermentation. The highest butanol titers (8.05 g L(-1)) were achieved with the fermentation of the acid hydrolysates of HEA, however, they required detoxification to support product formation after acid hydrolysis while ILEA did not. Direct ABE fermentation of ILEA and HEA (without detoxification) starches resulted in a butanol titer of 4.99 and 6.63 g L(-1), respectively, which significantly simplified the LEA to butanol process. The study demonstrated the compatibility of producing biodiesel and butanol from a single feedstock which may help reduce the feedstock costs of each individual process.

  11. Focused ultrasound solid-liquid extraction for the determination of organic biomarkers in beachrocks.

    Science.gov (United States)

    Blanco-Zubiaguirre, L; Arrieta, N; Iturregui, A; Martinez-Arkarazo, I; Olivares, M; Castro, K; Olazabal, M A; Madariaga, J M

    2015-11-01

    Beachrocks are consolidated coastal sedimentary formations resulting mainly from the relative rapid cementation of beach sediments by different calcium carbonate polymorphs. Although previous works have already studied the elemental composition and the mineral phases composing these cements, few of them have focused their attention on the organic matter present therein. This work describes an extraction methodology based on focused ultrasound solid-liquid extraction (FUSLE), followed by analysis using large volume injection (LVI) in a programmable temperature vaporizer (PTV) combined with gas chromatography-mass spectrometry (GC-MS) in order to determine organics such as polycyclic aromatic hydrocarbons (PAHs) and biomarkers (hopanes), which can increase and confirm the information obtained so far. This goal has been achieved after the optimization of the main parameters affecting the extraction procedure, such as, extraction solvent, FUSLE variables (amplitude, extraction time and pulse time) and also variables affecting the LVI-PTV (vent time, injection speed and cryo-focusing temperature). The developed method rendered results comparable to traditional extraction methods in terms of accuracy (77-109%) and repeatability (RSD<23%). Finally, the analyses performed over real beachrock samples from the Bay of Biscay (Northern Spain) revealed the presence of the 16 EPA priority PAHs, as well as some organic biomarkers which could increase the knowledge about such beachrock formation.

  12. Improvement of the cloud point extraction of uranyl ions by the addition of ionic liquids.

    Science.gov (United States)

    Gao, Song; Sun, Taoxiang; Chen, Qingde; Shen, Xinghai

    2013-12-15

    The cloud point extraction (CPE) of uranyl ions by different kinds of extractants in Triton X-114 (TX-114) micellar solution was investigated upon the addition of ionic liquids (ILs) with various anions, i.e., bromide (Br(-)), tetrafluoroborate (BF4(-)), hexafluorophosphate (PF6(-)) and bis[(trifluoromethyl)sulfonyl]imide (NTf2(-)). A significant increase of the extraction efficiency was found on the addition of NTf2(-) based ILs when using neutral extractant tri-octylphosphine oxide (TOPO), and the extraction efficiency kept high at both nearly neutral and high acidity. However, the CPE with acidic extractants, e.g., bis(2-ethylhexyl) phosphoric acid (HDEHP) and 8-hydroxyquinoline (8-HQ) which are only effective at nearly neutral condition, was not improved by ILs. The results of zeta potential and (19)F NMR measurements indicated that the anion NTf2(-) penetrated into the TX-114 micelles and was enriched in the surfactant-rich phase during the CPE process. Meanwhile, NTf2(-) may act as a counterion in the CPE of UO2(2+) by TOPO. Furthermore, the addition of IL increased the separation factor of UO2(2+) and La(3+), which implied that in the micelle TOPO, NTf2(-) and NO3(-) established a soft template for UO2(2+). Therefore, the combination of CPE and IL provided a supramolecular recognition to concentrate UO2(2+) efficiently and selectively.

  13. Extraction of arsenic from a soil in the blackfoot disease endemic area with ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    Liao, Chang-Yu [Department of Environmental Engineering, National Cheng Kung University, Tainan 70101, Taiwan (China); Peng, Ching-Yu [Department of Civil and Environmental Engineering, University of Washington, Seattle, WA 98105 (United States); Wang, Hong-Chung [Division of Chest Medicine, Department of Medicine, Veterans General Hospital-Kaohsiung, Kaohsiung 81362, Taiwan (China); Kang, Hsu-Ya [Department of Environmental Engineering, National Cheng Kung University, Tainan 70101, Taiwan (China); Paul Wang, H., E-mail: wanghp@mail.ncku.edu.tw [Department of Environmental Engineering, National Cheng Kung University, Tainan 70101, Taiwan (China)

    2011-10-01

    Speciation of arsenic extracted with room temperature ionic liquids (RTILs) ([bmim][BF{sub 4}] (1-butyl-3-methylimidazolium tetrafluoroborate) and [bmim][PF{sub 6}] (1-butyl-3-methylimidazolium hexafluorophosphate)) from an As-humic acid (As-HA) complex contaminated soil (As-HA/soil) in a blackfoot disease endemic area has been studied by X-ray absorption (near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS)) spectroscopy. About 45% of arsenic in the As-HA/soil can be extracted with [bmim][BF{sub 4}] while the relatively less hydrophilic [bmim][PF{sub 6}] extracts 25% of arsenic. The extracted arsenic in the [bmim][BF{sub 4}] and [bmim][PF{sub 6}] from the As-HA/soil possesses mainly As(III) species, suggesting that at least two reaction paths may be involved in the extraction process: (1) splitting of As-HA and (2) reduction of As(V) to As(III). The refined EXAFS spectra also indicate that the As(III) extracted in the RTILs possesses the AsO{sub 2}{sup -} structure, which has the As-O bond distances of 1.77-1.79 A and coordination numbers of 4.0-4.2.

  14. Solvent extraction of Th(IV) from aqueous solution with methylimidazole in ionic liquid

    Energy Technology Data Exchange (ETDEWEB)

    Li, Wenkui; Lv, Hui; Liu, Ziyi; Wu, Jianrong; Li, Shun; Shen, Yinglin [Lanzhou Univ. (China). Radiochemistry Lab.; Yang, Shenghua [State Key Laboratory of Applied Organic Chemistry, Lanzhou (China)

    2016-07-01

    An extraction of Th(IV) was performed using 1-methylimidazole (1-MIM) or 2-methylimidazole (2-MIM) as the extractant in imidazolium type ionic liquids (ILs) or n-pentanol. The extractability for Th{sup 4+} in ILs was by far higher than that obtained in n-pentanol. The extraction mechanism was determined by slope analysis and ESI-MS. The transfer of Th{sup 4+} with MIM into ILs proceeded through both a cationic exchange and a neutral solvation mechanism, whereas the partitioning of Th{sup 4+} with MIM into n-pentanol only underwent a neutral solvation mechanism. The thermodynamic parameters values (ΔH, ΔS and ΔG) for extraction of Th{sup 4+} with 1-MIM in IL were calculated and the results indicated the extraction reaction was spontaneous and went through endothermic process. Separation of Th{sup 4+} from the solution of lanthanides (III) and uranium was also carried out by 1-MIM in ILs and n-pentanol.

  15. Electrochemical assessment of water|ionic liquid biphasic systems towards cesium extraction from nuclear waste

    Energy Technology Data Exchange (ETDEWEB)

    Stockmann, T. Jane [Laboratoire d’Electrochimie Physique et Analytique, Ecole Polytechnique Fédérale de Lausanne (EPFL), Station 6, Lausanne CH-1015 (Switzerland); Department of Chemistry, The University of Western Ontario, 1151 Richmond Street, London, Ontario N6A 5B7 (Canada); Zhang, Jing; Montgomery, Anne-Marie [Department of Chemistry, The University of Western Ontario, 1151 Richmond Street, London, Ontario N6A 5B7 (Canada); Ding, Zhifeng, E-mail: zfding@uwo.ca [Department of Chemistry, The University of Western Ontario, 1151 Richmond Street, London, Ontario N6A 5B7 (Canada)

    2014-04-01

    Highlights: • Electroanalytical chemistry was employed to assess cesium ion extraction in biphasic systems. • Water|ionic liquid systems are much more efficient than traditional water|organic ones. • The metal ion to ligand stoichiometry and overall complexation constant were determined. • The stoichiometry was confirmed by mass spectrometry. • The ligand CMPO used in TRUEX processes was found to be effective for the FIT. Abstract: A room temperature ionic liquid (IL) composed of a quaternary alkylphosphonium (trihexyltetradecylphosphonium, P66614⁺) and tetrakis(pentafluorophenyl)borate anion (TB⁻) was employed within a water|P66614TB (w|P66614TB or w|IL) biphasic system to evaluate cesium ion extraction in comparison to that with a traditional water|organic solvent (w|o) combination. ¹³⁷Cs is a major contributor to the radioactivity of spent nuclear fuel as it leaves the reactor, and its extraction efficiency is therefore of considerable importance. The extraction was facilitated by the ligand octyl(phenyl)-N,N'-diisobutylcarbamoylphosphine oxide (CMPO) used in TRans-Uranium EXtraction processes and investigated through well established liquid|liquid electrochemistry. This study gave access to the metal ion to ligand (1:n) stoichiometry and overall complexation constant, β, of the interfacial complexation reaction which were determined to be 1:3 and 1.6 × 10¹¹ at the w|P66614TB interface while the study at w|o elicited an n equal to 1 with β equal to 86.5. Through a straightforward relationship, these complexation constant values were converted to distribution coefficients, δα, with the ligand concentrations studied for comparison to other studies present in the literature; the w|o and w|IL systems gave δα of 2 and 8.2 × 10⁷, respectively, indicating a higher overall extraction efficiency for the latter. For the w|o system, the metal ion-ligand stoichiometries were

  16. Separation of americium by liquid-liquid extraction using diglycol-amides water-soluble complexing agents

    Energy Technology Data Exchange (ETDEWEB)

    Chapron, S.; Marie, C.; Pacary, V.; Duchesne, M.T.; Miguirditchian, M. [CEA, Centre de Marcoule, Nuclear Energy Division, RadioChemistry and Processses Departement, 30207 Bagnols-sur-Ceze (France); Arrachart, G.; Pellet-Rostaing, S. [Institut de Chimie Separative de Marcoule, LTSM, Bat 426, F-30207 Bagnols-sur- Ceze (France)

    2016-07-01

    Recycling americium (Am) alone from spent nuclear fuels is an important option studied for the future nuclear cycle (Generation IV systems) since Am belongs to the main contributors of the long-term radiotoxicity and heat power of final waste. Since 2008, a liquid-liquid extraction process called EXAm has been developed by the CEA to allow the recovery of Am alone from a PUREX raffinate (a dissolution solution already cleared from U, Np and Pu). A mixture of DMDOHEMA (N,N'-dimethyl-N,N'-dioctyl-2-(2-(hexyloxy)ethyl)-malonamide) and HDEHP (di-2-ethylhexylphosphoric acid) in TPH is used as the solvent and the Am/Cm selectivity is improved using TEDGA (N,N,N',N'-tetraethyl-diglycolamide) as a selective complexing agent to maintain Cm and heavier lanthanides in the acidic aqueous phase (5 M HNO{sub 3}). Americium is then stripped selectively from light lanthanides at low acidity (pH=3) with a poly-aminocarboxylic acid. The feasibility of sole Am recovery was already demonstrated during hot tests in ATALANTE facility and the EXAm process was adapted to a concentrated raffinate to optimize the process compactness. The speciation of TEDGA complexes formed in the aqueous phase with Am, Cm and lanthanides was studied to better understand and model the behavior of TEDGA in the process. Some Ln-TEDGA species are extracted into the organic phase and this specific chemistry might play a role in the Am/Cm selectivity improvement. Hence the hydrophilicity-lipophilicity balance of the complexing agent is an important parameter. In this comprehensive study, new analogues of TEDGA were synthesized and tested in the EXAm process conditions to understand the relationship between their structure and selectivity. New derivatives of TEDGA with different N-alkyl chain lengths and ramifications were synthesized. The impact of lipophilicity on ligand partitioning and Am/Cm selectivity was investigated. (authors)

  17. Turbulence in microfluidics: Cleanroom-free, fast, solventless, and bondless fabrication and application in high throughput liquid-liquid extraction.

    Science.gov (United States)

    de Camargo, Camila L; Shiroma, Letícia S; Giordano, Gabriela F; Gobbi, Angelo L; Vieira, Luis C S; Lima, Renato S

    2016-10-12

    This paper addresses an important breakthrough in the deployment of ultra-high adhesion strength microfluidic technologies to provide turbulence at harsh flow rate conditions. This paper is only, to our knowledge, the second reporting on the generation of high flow rate-assisted turbulence in microchannels. This flow solves a crucial bottleneck in microfluidics: the generation of high throughput homogeneous mixings. We focused on the fabrication of bulky polydimethylsiloxane (PDMS) microchips (without any interfaces) rather than the laborious surface modifications that were employed in the first reporting about turbulence-assisted microfluidics. The fabrication is cleanroom-free, simple, low-cost, fast, solventless, and bondless requiring only a laboratory oven. More specifically, our method relies on the shaping of a nylon scaffold, cure of PDMS with embedded nylon, and removal of this scaffold. The scaffold was obtained by manually wrapping nylon threads. The withdrawing out of the scaffold was completed in few seconds using only a plier. Such microchannels endured flow rates of up to 60.0 mL min(-1) with a strikingly low elastic deformation. The importance in producing turbulence into microscale channels was successfully shown in liquid-liquid extractions. The great energy dissipation rate relative to the turbulence created high throughput and efficient extractions in microfluidics for the first time. The residence time was only 0.01 s at 25.0 mL min(-1) (total flow rate of the immiscible phases). In addition, the partition coefficient determined in a single run was similar to that obtained by the conventional batch shake-flask method that was realized in triplicate.

  18. The effect of Yucca schidigera liquid extract on water quality and survival of Pacific Red Snapper Lutjanus peru during acclimatization

    National Research Council Canada - National Science Library

    Castillo-Vargasmachuca, S; Ponce-Palafox, JT; Arredondo-Figueroa, JL; García-Ulloa, M; Benítez-Valle, A; Martínez-Cárdenas, L; Puga-López, D; Seidavi, A

    2015-01-01

    The goal of this study was to determine the effect of the liquid extract of Yucca schidigera on water quality and survival of Pacific red snapper Lutjanus peru during its transfer from wild to laboratory conditions...

  19. Determination of fluoroquinolones in chicken feces - a new liquid-liquid extraction method combined with LC-MS/MS.

    Science.gov (United States)

    Janusch, Franziska; Scherz, Gesine; Mohring, Siegrun A I; Hamscher, Gerd

    2014-11-01

    The application of antibiotics including fluoroquinolones to farming animals is widespread and may lead to the development of antibiotic resistance and other environmental effects. To calculate environmental loads and for a proper risk assessment it is necessary to determine the antibiotic concentration in feces. Therefore, a new liquid-liquid extraction method combined with HPLC-MS/MS for the detection of marbofloxacin, ciprofloxacin, enrofloxacin and difloxacin in chicken feces was developed. Recoveries ranged from 51.0% to 83.5%. LOQs were between 0.10 and 1.09μg/kg. Feces of chickens treated with an enrofloxacin dosage of 10mg/kg bodyweight revealed maximum enrofloxacin and ciprofloxacin concentrations of 61.3 and 18.8mg/kg. Both antibiotics could be detected in feces up to two days after the last application in notable amounts (∼1mg/kg). Thus, feces of recently medicated chickens should not be used as a fertilizer without any further processing. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. A microfluidic platform for the rapid determination of distribution coefficients by gravity assisted droplet-based liquid-liquid extraction

    DEFF Research Database (Denmark)

    Poulsen, Carl Esben; Wootton, Robert C. R.; Wolff, Anders

    2015-01-01

    for the testing of valuable and scarce drug candidates. Herein we present a simple micro fluidic platform for the determination of distribution coefficients using droplet-based liquid-liquid extraction. For simplicity, this platform makes use of gravity to enable phase separation for analysis and is 48 times...... faster and uses 99 % less reagents than performing an equivalent measurement using the shake-flask method. Furthermore, the D measurements achieved in our platform are in good agreement with literature values measured using traditional shake-flask techniques. Since D is affected by volume ratios, we use...... the apparent acid dissociation constant, pK', as a proxy for inter-system comparison. Our platform determines a pK' value of 7.24 ± 0.15, compared to 7.25 ± 0.58 for the shake-flask method in our hands and 7.21 for the shake-flask method in literature. Devices are fabricated using injection moulding, the batch...

  1. Determination of suvorexant in human plasma using 96-well liquid-liquid extraction and HPLC with tandem mass spectrometric detection.

    Science.gov (United States)

    Breidinger, S A; Simpson, R C; Mangin, E; Woolf, E J

    2015-10-01

    A method, using liquid chromatography with tandem mass spectrometric detection (LC-MS/MS), was developed for the determination of suvorexant (MK-4305, Belsomra(®)), a selective dual orexin receptor antagonist for the treatment insomnia, in human plasma over the concentration range of 1-1000ng/mL. Stable isotope labeled (13)C(2)H3-suvorexant was used as an internal standard. The sample preparation procedure utilized liquid-liquid extraction, in the 96-well format, of a 100μL plasma sample with methyl t-butyl ether. The compounds were chromatographed under isocratic conditions on a Waters dC18 (50×2.1mm, 3μm) column with a mobile phase consisting of 30/70 (v/v %) 10mM ammonium formate, pH3/acetonitrile at a flow rate of 0.3mL/min. Multiple reaction monitoring of the precursor-to-product ion pairs for suvorexant (m/z 451→186) and (13)C(2)H3-suvorexant (m/z 455→190) on an Applied Biosystems API 4000 tandem mass spectrometer was used for quantitation. Intraday assay precision, assessed in six different lots of control plasma, was within 10% CV at all concentrations, while assay accuracy ranged from 95.6 to 105.0% of nominal. Quality control (QC) samples in plasma were stored at -20°C. Initial within day analysis of QCs after one freeze-thaw cycle showed accuracy within 9.5% of nominal with precision (CV) of 6.7% or less. The plasma QC samples were demonstrated to be stable for up to 25 months at -20°C. The method described has been used to support clinical studies during Phase I through III of clinical development.

  2. Trace analysis of trimethoprim and sulfonamide, macrolide, quinolone, and tetracycline antibiotics in chlorinated drinking water using liquid chromatography electrospray tandem mass spectrometry

    Science.gov (United States)

    Ye, Z.; Weinberg, H.S.; Meyer, M.T.

    2007-01-01

    A multirun analytical method has been developed and validated for trace determination of 24 antibiotics including 7 sulfonamides, 3 macrolides, 7 quinolones, 6 tetracyclines, and trimethoprim in chlorine-disinfected drinking water using a single solid-phase extraction method coupled to liquid chromatography with positive electrospray tandem mass spectrometry detection. The analytes were extracted by a hydrophilic-lipophilic balanced resin and eluted with acidified methanol (0.1% formic acid), resulting in analyte recoveries generally above 90%. The limits of quantitation were mostly below 10 ng/L in drinking water. Since the concentrated sample matrix typically caused ion suppression during electrospray ionization, the method of standard addition was used for quantitation. Chlorine residuals in drinking water can react with some antibiotics, but ascorbic acid was found to be an effective chlorine quenching agent without affecting the analysis and stability of the antibiotics in water. A preliminary occurrence study using this method revealed the presence of some antibiotics in drinking waters, including sulfamethoxazole (3.0-3.4 ng/L), macrolides (1.4-4.9 ng/L), and quinolones (1.2-4.0 ng/L). ?? 2007 American Chemical Society.

  3. "Bligh and Dyer" and Folch Methods for Solid-Liquid-Liquid Extraction of Lipids from Microorganisms. Comprehension of Solvatation Mechanisms and towards Substitution with Alternative Solvents.

    Science.gov (United States)

    Breil, Cassandra; Abert Vian, Maryline; Zemb, Thomas; Kunz, Werner; Chemat, Farid

    2017-03-27

    Bligh and Dyer (B & D) or Folch procedures for the extraction and separation of lipids from microorganisms and biological tissues using chloroform/methanol/water have been used tens of thousands of times and are "gold standards" for the analysis of extracted lipids. Based on the Conductor-like Screening MOdel for realistic Solvatation (COSMO-RS), we select ethanol and ethyl acetate as being potentially suitable for the substitution of methanol and chloroform. We confirm this by performing solid-liquid extraction of yeast (Yarrowia lipolytica IFP29) and subsequent liquid-liquid partition-the two steps of routine extraction. For this purpose, we consider similar points in the ternary phase diagrams of water/methanol/chloroform and water/ethanol/ethyl acetate, both in the monophasic mixtures and in the liquid-liquid miscibility gap. Based on high performance thin-layer chromatography (HPTLC) to obtain the distribution of lipids classes, and gas chromatography coupled with a flame ionisation detector (GC/FID) to obtain fatty acid profiles, this greener solvents pair is found to be almost as effective as the classic methanol-chloroform couple in terms of efficiency and selectivity of lipids and non-lipid material. Moreover, using these bio-sourced solvents as an alternative system is shown to be as effective as the classical system in terms of the yield of lipids extracted from microorganism tissues, independently of their apparent hydrophilicity.

  4. Extraction of acetic acid, glycolaldehyde and acetol from aqueous solutions mimicking pyrolysis oil cuts using ionic liquids

    NARCIS (Netherlands)

    Li, X.; Kersten, Sascha R.A.; Schuur, Boelo

    2017-01-01

    Value-added oxygenates, such as acetic acid (HAc), glycolaldehyde and acetol, are present in pyrolysis oil and its cuts in substantial amounts. This work describes the separation of these value-added oxygenates from artificial aqueous fractions of pyrolysis oil via liquid-liquid extraction. Three

  5. Extraction of acetic acid, glycolaldehyde and acetol from aqueous solutions mimicking pyrolysis oil cuts using ionic liquids

    NARCIS (Netherlands)

    Li, X.; Kersten, Sascha R.A.; Schuur, Boelo

    2017-01-01

    Value-added oxygenates, such as acetic acid (HAc), glycolaldehyde and acetol, are present in pyrolysis oil and its cuts in substantial amounts. This work describes the separation of these value-added oxygenates from artificial aqueous fractions of pyrolysis oil via liquid-liquid extraction. Three ph

  6. The effect of Yucca schidigera liquid extract on water quality and survival of Pacific Red Snapper Lutjanus peru during acclimatization

    Directory of Open Access Journals (Sweden)

    S Castillo-Vargasmachuca

    2015-01-01

    Full Text Available The goal of this study was to determine the effect of the liquid extract of Yucca schidigera on water quality and survival of Pacific red snapper Lutjanus peru during its transfer from wild to laboratory conditions. Three experimental groups (0.00; 0.25 and 0.75 mg of Y. schidigera liquid extract per liter of culture were tested with four replicates using water recirculating systems. The liquid extract was dispensed every 72 h during 28 days. It was proved that Y. schidigera extract could be effective to reduce ammonia nitrogen caused by biogenic source (excretion of fish juveniles diminishing mortality of Pacific red snapper during acclimatization process. It is recommended the use of yucca extract concentration at a dose of 0.75 mg L-1 to reduce ammonia concentration in marine water for holding red snapper juveniles.

  7. Drop size in a liquid pulsed sieve-plate extraction column

    Directory of Open Access Journals (Sweden)

    M. R. Usman

    2009-12-01

    Full Text Available The (Benzoic acid + kerosene + water system was studied in a 5.0 cm diameter liquid pulsed liquid-liquid extraction column with a total number of 80 sieve plates. The effect of pulsation intensity, dispersed phase superficial velocity, and continuous phase superficial velocity on volume-surface mean diameter was studied. Generally, the mean drop diameter decreased more rapidly with the increase of pulsation intensities and superficial velocities at low pulsation intensities and superficial velocities. However, the effect was not found to be significant at higher pulsation intensities and higher superficial velocities. In the interpretation of the experimental results, the drop size was observed to be a function of the operating regimes (mixer-settler, dispersion, and emulsion of the pulsed sieve-plate extraction column. The experimental mean drop diameters were compared to the most acceptable analytical drop size correlation developed by Kumar and Hartland (1986. The correlation proved to be in good agreement for the column operating in the dispersion regime.

  8. Efficient tandem solid-phase extraction and liquid chromatography-triple quadrupole mass spectrometry method to determine polar benzotriazole, benzothiazole and benzenesulfonamide contaminants in environmental water samples.

    Science.gov (United States)

    Herrero, P; Borrull, F; Pocurull, E; Marcé, R M

    2013-09-27

    An analytical method has been developed that allows the simultaneous determination of five benzotriazole (BTRs), four benzothiazole (BTs) and five benzenesulfonamide (BSAs) derivates. The method is based on tandem solid-phase extraction (SPE) with Oasis HLB followed by a clean-up step with Florisil. The chromatographic analysis was performed in less than 15min and detection was carried out with a triple quadrupole mass analyser operating in multiple reaction monitoring (MRM) mode. A comparison was performed between Oasis HLB and Oasis MAX sorbents for the solid-phase extraction, with Oasis HLB being the sorbent that gave the highest recoveries, ranging between 75% and 106%, depending on the compound and the matrix analysed. The proposed clean-up with Florisil sorbent reduced the matrix effect to below 20%. The repeatability (%RSD, 50-3000ng/L, n=3) of the method was less than 15% for all of the compounds in all of the matrices. The limits of detection (LODs) achieved ranged from 1ng/L for BTR in river water up to 100ng/L for BT in influent sewage. All of the compounds were determined in environmental waters such as river water and sewage. The highest concentrations determined corresponded to influent sewage samples in which the sum of concentrations for all compounds were between 4.6μg/L and 8.0μg/L. These concentrations were slightly reduced in secondary effluent and tertiary effluent sewage. Moreover, samples from tertiary effluent sewage based on ultra-filtration membrane treatments were also analysed and preliminary results seem to indicate that these treatments may be most effective for removing BTR, BT and BSA derivates.

  9. Mixed-mode solid-phase extraction coupled with liquid chromatography tandem mass spectrometry to determine phenoxy acid, sulfonylurea, triazine and other selected herbicides at nanogram per litre levels in environmental waters.

    Science.gov (United States)

    Zhang, Pei; Bui, Anhduyen; Rose, Gavin; Allinson, Graeme

    2014-01-17

    The method presented uses a mixed-mode anion exchange SPE and liquid chromatography tandem mass spectrometry to analyze 5 sulfonylurea, 8 phenoxy acid, 12 triazine and 6 other herbicides in environmental waters. The mixed-mode SPE cartridge is able to retain a wide range of herbicides with acidic-neutral-basic characteristics, particularly the highly polar and acidic compounds clopyralid, dicamba and picloram. The neutral and basic herbicides can be effectively eluted with methanol, after which the acidic herbicides can be eluted using acidified methanol. The method has achieved an LOD of 0.7-3ng/L for the sulfonylureas, 4-12ng/L for the phenoxy acids and 0.4-30ng/L for the triazine and additional herbicides, with recoveries in the range 76-107%, 73-126%, and 65-104%, respectively. The precision of the method, calculated as relative standard deviation (RSD), was below 10% for both sulfonylurea and phenoxy acid herbicides, and less than 20% for the remaining herbicides. The developed method was used to determine the concentration of target herbicides in a range of environmental waters, and many of the target herbicides were detected at ng/L level.

  10. Fast and comprehensive analysis of secondary metabolites in cocoa products using ultra high-performance liquid chromatography directly after pressurized liquid extraction.

    Science.gov (United States)

    Damm, Irina; Enger, Eileen; Chrubasik-Hausmann, Sigrun; Schieber, Andreas; Zimmermann, Benno F

    2016-08-01

    Fast methods for the extraction and analysis of various secondary metabolites from cocoa products were developed and optimized regarding speed and separation efficiency. Extraction by pressurized liquid extraction is automated and the extracts are analyzed by rapid reversed-phase ultra high-performance liquid chromatography and normal-phase high-performance liquid chromatography methods. After extraction, no further sample treatment is required before chromatographic analysis. The analytes comprise monomeric and oligomeric flavanols, flavonols, methylxanthins, N-phenylpropenoyl amino acids, and phenolic acids. Polyphenols and N-phenylpropenoyl amino acids are separated in a single run of 33 min, procyanidins are analyzed by normal-phase high-performance liquid chromatography within 16 min, and methylxanthins require only 6 min total run time. A fourth method is suitable for phenolic acids, but only protocatechuic acid was found in relevant quantities. The optimized methods were validated and applied to 27 dark chocolates, one milk chocolate, two cocoa powders and two food supplements based on cocoa extract.

  11. Determination of hormones in milk by hollow fiber-based stirring extraction bar liquid-liquid microextraction gas chromatography mass spectrometry.

    Science.gov (United States)

    Xu, Xu; Liang, Fanghui; Shi, Jiayuan; Zhao, Xin; Liu, Zhuang; Wu, Lijie; Song, Ying; Zhang, Hanqi; Wang, Ziming

    2013-08-06

    The hollow fiber-based stirring extraction bar liquid-liquid microextraction was applied to the extraction of hormones, including 17-α-ethinylestradiol, 17-α-estradiol, estriol, 17-β-estradiol, estrone, 17-α-hydroxyprogesterone, medroxyprogesterone, progesterone and norethisterone acetate, in milk. The present method has the advantages of both hollow fiber-liquid phase microextraction and stirring bar sorptive extraction. The stirring extraction bar was used as both the stirring bar of microextraction, and extractor of the analytes, which can make extraction, clean-up and concentration be carried out in one step. When the extraction was completed, the stirring extraction bar was easy isolated from the extraction system with the magnet. Several experimental parameters, including the type of extraction solvent, the number of hollow stirring extraction bar, extraction time, stirring speed, ionic strength, and desorption conditions were investigated and optimized. The analytes in the extract were derived and determined by gas chromatography mass spectrometry. Under optimal experimental conditions, good linearity was observed in the range of 0.20-20.00ng mL(-1). The limits of detection and quantification were in the range of 0.02-0.06ng mL(-1) and 0.07-0.19ng mL(-1), respectively. The present method was applied to the analysis of milk samples, and the recoveries of analytes were in the range of 93.6-104.6% with the relative standard deviations ranging from 1.6% to 6.2% (n=5). The results showed that the present method was a rapid and feasible method for the determination of hormones in milk samples.

  12. Pretreatment of corn stover by combining ionic liquid dissolution with alkali extraction.

    Science.gov (United States)

    Geng, Xinglian; Henderson, Wesley A

    2012-01-01

    Pretreatment plays an important role in the efficient enzymatic hydrolysis of biomass into fermentable sugars for biofuels. A highly effective pretreatment method is reported for corn stover which combines mild alkali-extraction followed by ionic liquid (IL) dissolution of the polysaccharides and regeneration (recovery of the polysaccharides as solids). Air-dried, knife-milled corn stover was soaked in 1% NaOH at a moderate condition (90°C, 1 h) and then thoroughly washed with hot deionized (DI) water. The alkali extraction solublized 75% of the lignin and 37% of the hemicellulose. The corn stover fibers became softer and smoother after the alkali extraction. Unextracted and extracted corn stover samples were separately dissolved in an IL, 1-butyl-3-methylimidazolium chloride (C(4) mimCl), at 130°C for 2 h and then regenerated with DI water. The IL dissolution process did not significantly change the chemical composition of the materials, but did alter their structural features. Untreated and treated corn stover samples were hydrolyzed with commercial enzyme preparations including cellulases and hemicellulases at 50°C. The glucose yield from the corn stover sample that was both alkali-extracted and IL-dissolved was 96% in 5 h of hydrolysis. This is a highly effective methodology for minimizing the enzymatic loading for biomass hydrolysis and/or maximizing the conversion of biomass polysaccharides into sugars.

  13. Selective extraction and determination of neonicotinoid insecticides in wine by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Rodríguez-Cabo, T; Casado, J; Rodríguez, I; Ramil, M; Cela, R

    2016-08-19

    A simplified, high throughput procedure for the determination of five neonicotinoid insecticides in red and white wines, using liquid chromatography (LC)-tandem mass spectrometry (MS/MS), is presented. The effects of different experimental parameters (extraction sorbent, solvent elution and clean-up conditions) in the efficiency and the selectivity of the sample preparation process were assessed through calculation of the extraction yields and the matrix effects (MEs). Wines (10mL) were concentrated using OASIS HLB cartridges, on-line connected to Florisil clean-up cartridges, with acetonitrile serving as the elution solvent. The extract (5mLvol) was concentrated to 1mL and injected in the LC-ESI-MS/MS system. The optimized procedure provided quantitative extraction yields at the same time that the efficiency of ESI ionization remained unchanged between standards and sample extracts. Overall recoveries, calculated against authentic standards in ACN, varied between 77 and 119% and the attained limits of quantification remained below 0.2ngmL(-1). Analysis of commercial wines revealed imidacloprid residues in more than 50% of processed samples, with a maximum level of 14ngmL(-1). Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Determination of triazine herbicides in fresh vegetables by dynamic microwave-assisted extraction coupled with homogeneous ionic liquid microextraction high performance liquid chromatography.

    Science.gov (United States)

    Wu, Lijie; Hu, Mingzhu; Li, Zhanchao; Song, Ying; Yu, Cui; Zhang, Yupu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

    2015-02-01

    A novel extraction method, dynamic microwave-assisted extraction coupled with homogeneous ionic liquid microextraction, was developed for the determination of triazine herbicides, including desmetryn, terbumeton, propazine, terbuthylazine, dimethametryn, and dipropetryn in fresh vegetable samples by high performance liquid chromatography (HPLC). In the developed method, 120 μL of 1-butyl-3-methylimidazolium tetrafluoroborate ([C4MIM][BF4]) was added to 10 mL of aqueous solution containing 0.3 g of NaCl to obtained the extraction solvent. Six triazines could be extracted completely within 4 min by the present method. Then, [NH4][PF6] was added into the extract to form a water-insoluble ionic liquid [C4MIM][PF6] via a simple metathesis reaction, and the analytes were enriched into the ionic liquid phase. After centrifugation and dilution with acetonitrile, the resulting solution was analyzed directly by HPLC. The effects of some experimental parameters, including type and volume of ionic liquid, volume of extraction solvent, amount of ion-pairing agent [NH4][PF6], salt concentration, microwave power, and flow rate of extraction solvent on the extraction efficiency were investigated and optimized. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 2.50-250.00 μg kg(-1), with the correlation coefficients ranging from 0.9989 to 0.9999. When the present method was applied to the analysis of vegetable samples, satisfactory recoveries were obtained in the range of 76.8%-106.9%, and relative standard deviations were lower than 9.8%.

  15. Development of Hydrothermal Liquefaction and Upgrading Technologies for Lipid-Extracted Algae Conversion to Liquid Fuels

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Yunhua; Albrecht, Karl O.; Elliott, Douglas C.; Hallen, Richard T.; Jones, Susanne B.

    2013-10-01

    Bench-scale tests were performed for lipid-extracted microalgae (LEA) conversion to liquid fuels via hydrotreating liquefaction (HTL) and upgrading processes. Process simulation and economic analysis for a large-scale LEA HTL and upgrading system were developed based on the best available test results. The system assumes an LEA feed rate of 608 dry metric ton/day and that the feedstock is converted to a crude HTL bio-oil and further upgraded via hydrotreating and hydrocracking to produce liquid hydrocarbon fuels, mainly alkanes. Performance and cost results demonstrate that HTL would be an effective option to convert LEA to liquid fuel. The liquid fuels annual yield was estimated to be 26.9 million gallon gasoline-equivalent and the overall energy efficiency at higher heating value basis was estimated to be 69.5%. The minimum fuel selling price (MFSP) was estimated to be $0.75/L with LEA feedstock price at $33.1 metric ton at dry basis and 10% internal rate of return. A sensitivity analysis indicated that the largest effects to production cost would come from the final products yields and the upgrading equipments cost. The impact of plant scale on MFSP was also investigated.

  16. Extraction of lignins from aqueous-ionic liquid mixtures by organic solvents.

    Science.gov (United States)

    Xin, Qin; Pfeiffer, Katie; Prausnitz, John M; Clark, Douglas S; Blanch, Harvey W

    2012-02-01

    The commercial development of ionic liquids (ILs) to pretreat lignocellulose by dissolution of whole biomass and cellulose precipitation by addition of water is hindered by the absence of an effective technique to recover the lignin content of the biomass from the IL. Three organic solvents [ethyl acetate, 1,4-dioxane, and tetrahydrofuran (THF)] were studied for their ability to form a two-liquid-phase system with water and 1-ethyl-3-methylimidazolium acetate ([C(2)mim][OAc]), and for partitioning model lignins and lignin monomers between the two liquid phases. Ternary diagrams were obtained for three [C(2)mim][OAc]/organic solvent/water systems at 22°C. Partition coefficients were measured for several types of lignin in these three systems. Partition coefficients increase with rising water content in the IL phase, and depend strongly on the type of lignin and on the organic solvent. Partition coefficients rise as the pH of the ionic-liquid-rich phase falls. Small molecule model lignin monomer compounds (guaiacol, syringaldehyde) are also readily extracted from the IL/water system by THF. Copyright © 2011 Wiley Periodicals, Inc.

  17. Maghemite nanoparticle-decorated hollow fiber electromembrane extraction combined with dispersive liquid-liquid microextraction for the determination of thymol from Carum copticum

    DEFF Research Database (Denmark)

    Khajeh, Mostafa; Pedersen-Bjergaard, Stig; Bohlooli, Mousa

    2017-01-01

    BACKGROUND A novel technique using maghemite nanoparticle-decorated hollow fibers to assist electromembrane extraction is proposed. Electromembrane extraction combined with dispersive liquid–liquid microextraction (EME-DLLME) was applied for the extraction of thymol from Carum copticum, followed.......2% respectively. The intra- and inter-day accuracy was higher than 93.6%. CONCLUSION The results indicated that EME-DLLME/GC-FID is a useful technique for the extraction and determination of thymol in C copticum. © 2016 Society of Chemical Industry...

  18. Determination of Polysaccharide in Radix pseudostellariae Extract by Size-Exclusion High-Performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A simple size-exclusion high-performance liquid chromatographic method was developed for rapid molecular mass screening to determine the average molecular mass, polydispersity, and quantity of Taizishen polysaccharides extract. The screening used a TOSOH TSK-GEL G3000SW high-performance liquid chromatographic column with 0.1 mol/L NaNO3 buffer as the mobile phase and refractive index detector. The molecular mass calibration curve was linear for polysaccharide standards from 10 to 100 kDa with a correlation coefficient of 0.9991. The method can be used to analyze the quantity, average molecular mass,and polydispersity of polysaccharides. In addition, the screening method is suitable for quality control of polysaccharide preparations in Chinese medicines and pharmaceutical products.

  19. Determination of Sudan I-IV in candy using ionic liquid/anionic surfactant aqueous two-phase extraction coupled with high-performance liquid chromatography.

    Science.gov (United States)

    Yu, Wei; Liu, Zhongling; Li, Qiang; Zhang, Hanqi; Yu, Yong

    2015-04-15

    Ionic liquid/anionic surfactant aqueous two-phase system was developed and applied for the extraction of Sudan I-IV. High-performance liquid chromatography was applied to the determination of the analytes. The aqueous two-phase system (ATPS) was formed in the present of C4[MIM]BF4, sodium dodecyl benzene sulphonate and (NH4)2SO4. The parameters affecting the extraction efficiency, such as volume of ionic liquid, amount of sodium dodecyl benzene sulphonate, ionic strength, pH value of system, extraction time and temperature were investigated. The limits of detection for Sudan I, II, III and IV were 5.45, 4.66, 3.68, 4.20 μg kg(-1), respectively. When the present method was applied to the analysis of candy samples, the recoveries of the analytes ranged from 82.3% to 112.1% and relative standard deviations were lower than 7.41%.

  20. Extraction of catechol violet, chrome azurol S and eriochrome cyanine R with chloroform solutions of liquid anion-exchangers.

    Science.gov (United States)

    Przeszlakowski, S; Wydra, H

    1984-06-01

    The extraction of Catechol Violet, Chrome Azurol S and Eriochrome Cyanine R with chloroform solutions of tri-n-octylamine (TOA), TOA hydrochloride and Aliquat 336 has been investigated. From the extraction isotherms, absorption spectra of the organic phases and dependence of the extraction coefficients on extractant concentration, it was found that the singly-charged anions HL(-) are extracted preferentially, but acidic groups other than sulphonate can also form ion-pairs with alkylammonium cations at higher pH values of the aqueous phase, and at high acidity these dyes can be extracted other than by an anion-exchange reaction. The three dyes (especially Eriochrome Cyanine R and Chrome Azurol S) were strongly extracted with the liquid anion-exchanger used and Aliquat 336 was a better extractant than TOA or TOA hydrochloride. The absorption spectra for the organic phases containing Chrome Azurol S and Eriochrome Cyanine R depended on the extractant used.

  1. Rapid determination of pesticide residues in herbs using selective pressurized liquid extraction and fast gas chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Du, Gang; Xiao, Yao; Yang, Hua-Rong; Wang, Li; Song, Yue-Lin; Wang, Yi-Tao

    2012-08-01

    A selective pressurized liquid extraction and gas chromatography coupled with triple quadrupole mass spectrometer method was developed for simultaneous determination of 52 pesticide residues in medicine and food dual-purpose herbs. The developed extraction method integrated extraction and cleanup processes for sample preparation. The sorbents, 5 g Florisil and 100 mg graphitized carbon black, were placed inside the extraction cell to remove matrix interferences. Optimized conditions of selective pressurized liquid extraction were ethyl acetate as extraction solvent, 120°C of extraction temperature, 6 min of static extraction time, 50% of flush volume extracted for two cycles. An ultra inert capillary GC-MS HP-5 UI column (20 m × 0.18 mm id, 0.18 μm) and column backflush system were used for the analysis. Multiple-reaction monitoring was employed for the quantitative analysis with electron ionization mode. All calibration curves showed good linearity (r(2) > 0.995) within the test ranges. The average recoveries of most pesticides were from 81 to 118%. The validated method was successfully applied for the determination of pesticide residues in four herbs. The results indicate that selective pressurized liquid extraction and GC-MS/MS is a sensitive and reliable analytical method for the simultaneous determination of multiple pesticide residues in herbs.

  2. Potential of liquid extracts of Sargassum wightii on growth, biochemical and yield parameters of cluster bean plant

    Directory of Open Access Journals (Sweden)

    N. Vijayanand

    2014-06-01

    Conclusion: The presence of micro and macro nutrients, vitamins, growth hormones and other constituents in the seaweed extract might be very much useful to the crops but their level should be appropriate to enhance growth and productivity. It may be concluded that liquid seaweed extracts could serve as cost effective eco-friendly product for sustainable agriculture.

  3. Unique selectivity reversal in Am(3+)-Eu(3+) extraction in a tripodal TREN-based diglycolamide in ionic liquid: extraction, luminescence, complexation and structural studies.

    Science.gov (United States)

    Leoncini, Andrea; Mohapatra, Prasanta K; Bhattacharyya, Arunasis; Raut, Dhaval R; Sengupta, Arijit; Verma, Parveen K; Tiwari, Nidhi; Bhattacharyya, Dibyendu; Jha, Sambhunath; Wouda, Anna M; Huskens, Jurriaan; Verboom, Willem

    2016-02-14

    An N-pivot diglycolamide extractant (DGA-TREN) was synthesized for the first time and its complexation behaviour was studied towards trivalent lanthanide/actinide ions. The solvent extraction studies suggested a unique selectivity reversal in the extraction of trivalent actinides versus trivalent lanthanides which was observed performing extraction studies in an ionic liquid vis-à-vis a molecular diluent for a tripodal TREN-based diglycolamide ligand (DGA-TREN) vs. a tripodal diglycolamide ligand (T-DGA) which may have great significance in radioactive waste remediation. The nature of the bonding to Eu(3+) ion was investigated by EXAFS as well as by DFT calculations.

  4. Quantitative high-performance liquid chromatographic determination of delta 4-3-ketosteroids in adrenocortical extracts.

    Science.gov (United States)

    Ballerini, R; Chinol, M; Ghelardoni, M

    1980-05-30

    A high-performance liquid chromatographic method is described for the determination of seven steroids in adrenocortical extracts showing a delta 4-3-ketonic conjugated system. The seven steroids (cortisol, cortisone, 11-dehydrocorticosterone, corticosterone, 11-deoxycortisol, aldosterone and 11-deoxycorticosterone) were separated with a chloroform-methanol gradient on a 5-micron silica column and with a water-acetonitrile gradient on a 10-micron RP-8 column. Effluents were monitored by UV absorption at 242 nm. Quantitative analysis was performed by comparing peak areas, which are proportional to the amounts of the individual substances (external standard method). The method is rapid, sensitive, easy to perform and reproducible.

  5. A modified technique for extracting a dislocated lens with perfluorocarbon liquids and viscoelastics.

    Science.gov (United States)

    Dalma-Weiszhausz, José; Franco-Cardenas, Valentina; Dalma, Alejandro

    2010-01-01

    The authors describe a modified technique for extraction of a dislocated crystalline lens or large and hard lens fragments displaced into the vitreous cavity. An ophthalmic viscosurgical device was used around and on top of the heavy liquid bubble to keep the lens centered and less mobile for easier phacofragmentation or removal by the cutting-suction probe. This technique was used in 10 eyes, including cases of traumatic dislocation and Marfan syndrome, with excellent anatomical results and no complications that could be attributed to the surgical technique. The technique has also been used to retrieve and reposition dislocated intraocular lenses.

  6. The application of supported liquid extraction in the analysis of benzodiazepines using surface enhanced Raman spectroscopy.

    Science.gov (United States)

    Doctor, Erika L; McCord, Bruce

    2015-11-01

    Benzodiazepines are among the most frequently prescribed medicines for anxiety disorders and are present in many toxicological screens. These drugs are often administered in the commission of drug facilitated sexual assaults due their effects on the central nervous system. Due to the potency of the drugs, only small amounts are usually given to victims; therefore, the target detection limit for these compounds in biological samples has been set at 50 ng/mL. Currently the standard screening method for detection of this class of drug is the immunoassay; however, screening methods that are more sensitive and selective than immunoassays are needed to encompass the wide range of structural variants of this class of compounds. Surface enhanced Raman spectroscopy (SERS) can be highly sensitive and has been shown to permit analysis of various benzodiazepines with limits of detection as low as 6 ng/mL. This technique permits analytical results in less than 2 min when used on pure drug samples. For biological samples, a key issue for analysis by SERS is removal of exogenous salts and matrix components. In this paper we examine supported liquid extraction as a useful preparation technique for SERS detection. Supported liquid extraction has many of the benefits of liquid-liquid extraction along with the ability to be automated. This technique provides a fast and clean extraction for benzodiazepines from urine at a pH of 5.0, and does not produce large quantities of solvent waste. To validate this procedure we have determined figures of merit and examined simulated urine samples prepared with commonly appearing interferences. It was shown that at a pH 5.0 many drugs that are prevalent in urine samples can be removed, permitting a selective detection of the benzodiazepine of interest. This technique has been shown to provide rapid (less than 20 min), sensitive, and specific detection of benzodiazepines with limits of detection between 32 and 600 ng/mL and dynamic range of 32

  7. Determination of Earthy-musty Odorous Compounds in Drinking Water by Vortex Assisted Dispersive Liquid-Liquid Microextraction Combined with Gas Chromatography Tandem Mass Spectrometry.

    Science.gov (United States)

    Lu, Jian; Wu, Zhong-Ping; Che, Wen-Jun; Xian, Yan-Ping; Guo, Xin-Dong; Lv, Jia-Xin; Li, He

    2016-01-01

    A new method was developed for the determination of eight earthy-musty compounds in drinking water by gas chromatography tandem mass spectrometry (GC-MS/MS) combined with dispersive liquid-liquid microextraction (DLLME). In this work, the type and volume of extraction solvent and dispersion agent, and the amount of NaCl were optimized; the linearity, detection limit, recovery and precision of method were investigated. The results indicated that the target analytes were in the range of 0.2 - 100 μg/L with correlation coefficient (r) ranging from 0.9991 to 0.9999, the limit of detection (LOD, S/N = 3) of the analytes ranged from 0.2 to 1.0 ng/L with the enrichment factor of 320. The mean recoveries for drinking water at three spiked concentrations levels of 0.6 - 32 ng/L were in the range of 91.3 to 103%, the precision ranged from 3.1 to 7.5% (n = 6), and the inter-day precision was from 6.1 to 11.1% (n = 5). Only one of 15 selected real samples tested positive for GSM, and the concentration was 3 ng/L. This method was confirmed to be simple, fast, efficient, and accurate for the determination of earthy-musty compounds in aqueous samples.

  8. Indacaterol determination in human urine: validation of a liquid-liquid extraction and liquid chromatography-tandem mass spectrometry analytical method.

    Science.gov (United States)

    Ammari, Wesam G; Al-Qadhi, Zainab; Khalil, Mohammad; Tayyem, Rabab; Qammaz, Samir; Oriquat, Ghaleb; Basheti, Iman A; Chrystyn, Henry

    2015-06-01

    Indacaterol is a novel once-a-day inhaled ultra-long-acting β2-agonist. Quantitative bioanalysis supports pharmacokinetic and clinical research. The aim of the current work was to validate an in-house developed high performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) analytical method for indacaterol determination in human urine samples. A liquid-liquid extraction method has been developed to extract indacaterol from human urine samples using ethyl acetate. Indacaterol dry extract was reconstituted with 200 μL of the mobile phase (acidified water:methanol (30:70, v/v)) of which 5 μL was needed for the HPLC-MS/MS analysis. Indacaterol was eluted on a reversed C18 stationary phase with an isocratic mobile phase at a flow of 1 mL/min. Formoterol was the internal standard (IS). The MS/MS detection was employed with a turbo-ion spray ionization in the positive ion mode. A consensus of the international Guidelines for Bioanalytical Method Validation was followed. Indacaterol was detected at a mass to charge ratio (m/z) of 393.3 and its MS/MS daughter at 173.2. The retention times of indacaterol and IS were 1.60 and 1.20 min, respectively. Validated calibration curves were linear over a range of 0.075-100 ng/mL with correlation coefficients (r)≥0.990. The curves' regression weighting factor was 1/x. Method specificity was established in six different human urine batches. No matrix interference was observed. The intra- and inter-batch precision and accuracy within±20% (at lower limit) and±15% (other quality control (QC) levels) were confirmed. The indacaterol mean recovery (precision) percentages at Low, Mid, and High QC levels were 93.5 (3.84), 89.8 (2.15), and 92.2 (2.17), respectively. Short-term, long-term, freeze-thaw, and auto-sampler stability results were accepted. A specific, accurate and precise HPLC-MS/MS method has been validated for indacaterol quantification in human urine. This simple method is reproducible and robust

  9. Optimization of an accelerated solvent extraction dispersive liquid-liquid microextraction method for the separation and determination of essential oil from Ligusticum chuanxiong Hort by gas chromatography with mass spectrometry.

    Science.gov (United States)

    Yang, Guang; Sun, Qiushi; Hu, Zhiyan; Liu, Hua; Zhou, Tingting; Fan, Guorong

    2015-10-01

    In this study, an accelerated solvent extraction dispersive liquid-liquid microextraction coupled with gas chromatography and mass spectrometry was established and employed for the extraction, concentration and analysis of essential oil constituents from Ligusticum chuanxiong Hort. Response surface methodology was performed to optimize the key parameters in accelerated solvent extraction on the extraction efficiency, and key parameters in dispersive liquid-liquid microextraction were discussed as well. Two representative constituents in Ligusticum chuanxiong Hort, (Z)-ligustilide and n-butylphthalide, were quantitatively analyzed. It was shown that the qualitative result of the accelerated solvent extraction dispersive liquid-liquid microextraction approach was in good agreement with that of hydro-distillation, whereas the proposed approach took far less extraction time (30 min), consumed less plant material (usually extraction and analysis of essential oil.

  10. Investigation on the extraction of strontium ions from aqueous phase using crown ether-ionic liquid systems

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    The extraction of strontium ions using DCH18C6 as the extractant and various ionic liquids(ILs) as solvents has been investigated.The distribution ratio of Sr2+ can reach as high as 103 under certain conditions,much larger than that in DCH18C6/n-octanol system.The extraction capacity depends greatly on the structure of ionic liquids.In Ils-based extraction systems,the extraction efficiency of strontium ions is reduced by increasing the concentration of nitric acid and can also be influenced directly by the presence of Na+ and K+ in the aqueous phase.It is confirmed that the extraction proceeds mainly via a cation-exchange mechanism.

  11. Investigation on the extraction of strontium ions from aqueous phase using crown ether-ionic liquid systems

    Institute of Scientific and Technical Information of China (English)

    XU Chao; SHEN XingHai; CHEN QingDe; GAO HongCheng

    2009-01-01

    The extraction of strontium ions using DCH18C6 as the extractant and various ionic liquids (Ils) as solvents has been investigated.The distribution ratio of Sr~(2+) can reach as high as 10~3 under certain conditions,much larger than that in DCH18C6/n-octanol system.The extraction capacity depends greatly on the structure of ionic liquids.In Ils-based extraction systems,the extraction efficiency of strontium ions is reduced by increasing the concentration of nitric acid and can also be influenced directly by the presence of Na~+ and K~+ in the aqueous phase.It is confirmed that the extraction proceeds mainly via a cation-exchange mechanism.

  12. Determination of sulfonamide antibiotics and metabolites in liver, muscle and kidney samples by pressurized liquid extraction or ultrasound-assisted extraction followed by liquid chromatography-quadrupole linear ion trap-tandem mass spectrometry (HPLC-QqLIT-MS/MS).

    Science.gov (United States)

    Hoff, Rodrigo Barcellos; Pizzolato, Tânia Mara; Peralba, Maria do Carmo Ruaro; Díaz-Cruz, M Silvia; Barceló, Damià

    2015-03-01

    Sulfonamides are widely used in human and veterinary medicine. The presence of sulfonamides residues in food is an issue of great concern. Throughout the present work, a method for the targeted analysis of 16 sulfonamides and metabolites residue in liver of several species has been developed and validated. Extraction and clean-up has been statistically optimized using central composite design experiments. Two extraction methods have been developed, validated and compared: i) pressurized liquid extraction, in which samples were defatted with hexane and subsequently extracted with acetonitrile and ii) ultrasound-assisted extraction with acetonitrile and further liquid-liquid extraction with hexane. Extracts have been analyzed by liquid chromatography-quadrupole linear ion trap-tandem mass spectrometry. Validation procedure has been based on the Commission Decision 2002/657/EC and included the assessment of parameters such as decision limit (CCα), detection capability (CCβ), sensitivity, selectivity, accuracy and precision. Method׳s performance has been satisfactory, with CCα values within the range of 111.2-161.4 µg kg(-1), limits of detection of 10 µg kg(-1) and accuracy values around 100% for all compounds.

  13. Characterization and in vitro permeation study of microemulsions and liquid crystalline systems containing the anticholinesterase alkaloidal extract from Tabernaemontana divaricata

    DEFF Research Database (Denmark)

    Chaiyana, Wantida; Rades, Thomas; Okonogi, Siriporn

    2013-01-01

    and water with the oil:surfactant ratios of 1:5 and 2:5. The formulations were characterized by photon correlation spectroscopy, polarizing light microscopy, differential scanning calorimetry, and viscosity measurement. A reverse micellar phase, w/o microemulsions, liquid crystalline systems, liquid crystal...... in microemulsion systems and coarse emulsions were formed along the aqueous dilution line of both oil:surfactant ratios. Formulations with the ratio of 1:5 containing 0.1μg/ml extract showed a significantly higher acetylcholinesterase inhibition than those with the ratio of 2:5. The skin of stillborn piglet...... was used in the permeation study. The liquid crystalline and microemulsion systems significantly increased the transdermal delivery of the extract within 24h. It was concluded that the alkaloidal extract from T. divaricata stem loaded in liquid crystalline or microemulsion systems comprising Z. cassumunar...

  14. Determination of chlorobenzenes in textiles by pressurized hot water extraction followed by vortex-assisted liquid-liquid microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lu, Yang; Zhu, Yan

    2013-12-06

    A method for quantitative determination of chlorobenzenes in textiles is developed, using pressurized hot water extraction (PHWE), vortex-assisted liquid-liquid microextraction (VALLME) and gas chromatography-mass spectrometry (GC-MS). VALLME serves as a trapping step after PHWE. The extraction conditions are investigated, as well as the quantitative features such as linearity, limits of detection (LODs), limits of quantification (LOQs), repeatabilities and reproducibilities between days. LOQs of 0.018-0.032mg/kg were achieved. The present method provides good repeatabilities (RSDGC-MS is a simple, rapid and environmentally friendly method for determination of chlorobenzenes in textiles.

  15. 3-phenyl-4-acyl-5-isoxazolones as reagents for liquid-liquid extraction of tetravalent zirconium and hafnium from acidic chloride solutions

    OpenAIRE

    Reddy,B. Ramachandra; Kumar,J. Rajesh; Reddy,A. Varada

    2006-01-01

    Liquid liquid extraction of tetravalent zirconium and hafnium from acidic chloride solutions has been investigated using 3-phenyl-4-acyl-5-isoxazolones in xylene such as 3-phenyl-4-benzoyl-5-isoxazolones (HPBI), 3-phenyl-4-(4-fluorobenzoyl)-5-isoxazolone (HFBPI) and 3-phenyl-4-(4-toluoyl)-5-isoxazolone (HTPI). The extraction of zirconium(IV) / hafnium(IV) shows a ion exchange mechanism: MO2+ (aq) + 2 HA (org) « MOA2 (org) + 2 H+(aq), where M = Zr(IV) / Hf(IV) and HA = HPBI or HFBPI or H...

  16. Extraction liquide-solide de Dysprosium(III) par le charbon actif ferromagnétique

    OpenAIRE

    khiri, khaira

    2014-01-01

    L’extraction liquide-solide de Dy(III) a été faite par le charbon actif ferromagnétique, dans un milieu nitré. L’effet de pH initial, concentration initial en ion Dy(III), le temps de contact, la force ionique, la température, la masse et l’élution ont été étudiés. La capacité de sorption augmente avec l’augmentation de la concentration initiale en Dy(III), le pH et la température. L’isotherme de Freundlich décrit mieux le processus d’extraction, ainsi que le modèle cinétique de p...

  17. Determination of triazine herbicides in milk by cloud point extraction and high-performance liquid chromatography.

    Science.gov (United States)

    Liu, Tiantian; Cao, Peng; Geng, Jinpei; Li, Jinqiang; Wang, Mingzhen; Wang, Minglin; Li, Xiaoyu; Yin, Dalu

    2014-01-01

    High-performance liquid chromatography with UV detection was used to detect four triazines in milk. An efficient pretreatment method known as cloud point extraction (CPE) was proposed for extracting and preconcentrating analytes. The parameters of CPE including surfactant type and concentration, electrolyte, sample pH, incubation temperature and duration were investigated. Under optimal conditions, satisfying recoveries in the range of 70.5-96.9% were achieved for four triazines. The limits of detection ranged from 6.79 to 11.19μg L(-1). The linear range of quantitation for the four triazines was 50-2000μg L(-1), and the correlation coefficients of the calibration curves were all 0.9999. The results demonstrated that the proposed method was efficient and reliable for the determination of triazine herbicides in milk samples.

  18. Development of an extraction process for removal of heteroatoms from coal liquids. Final report

    Energy Technology Data Exchange (ETDEWEB)

    1994-04-01

    The main goal of this contract was to develop an extraction process for upgrading coal liquids; and in doing so, to reduce the hydrogen requirement in downstream upgrading processes and to yield valuable byproducts. This goal was to be achieved by developing a novel carbon dioxide extraction process for heteroatom removal from coal-derived naphtha, diesel, and jet fuel. The research plan called for the optimization of three critical process variables using a statistically-designed experimental matrix. The commercial potential of the new process was to be evaluated by demonstrating quantitatively the effectiveness of heteroatom removal from three different feedstocks and by conducting a comparative economic analysis of alternate heteroatom removal technologies. Accomplishments are described for the following tasks: food procurement and analysis process variable screening studies; and process assessment.

  19. Determination of Lead in Water Samples Using a New Vortex-Assisted, Surfactant-Enhanced Emulsification Liquid-Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry.

    Science.gov (United States)

    Peng, Guilong; He, Qiang; Lu, Ying; Mmereki, Daniel; Pan, Weiliang; Tang, Xiaohui; Zhou, Guangming; Mao, Yufeng; Su, Xaioxuan

    2016-04-01

    A low toxic solvent-based vortex-assisted surfactant-enhanced emulsification liquid-liquid microextraction (LT-VSLLME) combined with graphite furnace atomic absorption spectrometry was developed for the extraction and determination of lead (Pb) in water samples. In the LT-VSLLME method, the extraction solvent was dispersed into the aqueous samples by the assistance of vortex agitator. Meanwhile, the addition of a surfactant, which acted as an emulsifier, could enhance the speed of the mass-transfer from aqueous samples to the extraction solvent. The influences of analytical parameters, including extraction solvent type and its volume, surfactant type and its volume, pH, concentration of chelating agent, salt effect and extraction time were investigated. Under the optimized conditions, a good relative standard deviation of 3.69% at 10 ng L(-1) was obtained. The calibration graph showed a linear pattern in the ranges of 5-30 ngL(-1), with a limit of detection of 0.76 ng L(-1). The linearity was obtained by five points in the concentration range of 5-30 ngL(-1). The enrichment factor was 320. The procedure was applied to wastewater and river water, and the accuracy was assessed through the analysis of the recovery experiments.

  20. On-line micro-volume introduction system developed for lower density than water extraction solvent and dispersive liquid-liquid microextraction coupled with flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Anthemidis, Aristidis N., E-mail: anthemid@chem.auth.gr [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, Thessaloniki 54124 (Greece); Mitani, Constantina; Balkatzopoulou, Paschalia; Tzanavaras, Paraskevas D. [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, Thessaloniki 54124 (Greece)

    2012-07-06

    Highlights: Black-Right-Pointing-Pointer A dispersive liquid-liquid micro extraction method for lead and copper determination. Black-Right-Pointing-Pointer A micro-volume transportation system for extractant solvent lighter than water. Black-Right-Pointing-Pointer Analysis of natural water samples. - Abstract: A simple and fast preconcentration/separation dispersive liquid-liquid micro extraction (DLLME) method for metal determination based on the use of extraction solvent with lower density than water has been developed. For this purpose a novel micro-volume introduction system was developed enabling the on-line injection of the organic solvent into flame atomic absorption spectrometry (FAAS). The effectiveness and efficiency of the proposed system were demonstrated for lead and copper preconcentration in environmental water samples using di-isobutyl ketone (DBIK) as extraction solvent. Under the optimum conditions the enhancement factor for lead and copper was 187 and 310 respectively. For a sample volume of 10 mL, the detection limit (3 s) and the relative standard deviation were 1.2 {mu}g L{sup -1} and 3.3% for lead and 0.12 {mu}g L{sup -1} and 2.9% for copper respectively. The developed method was evaluated by analyzing certified reference material and it was applied successfully to the analysis of environmental water samples.

  1. Selective extraction and recovery of rare earth metals from phosphor powders in waste fluorescent lamps using an ionic liquid system.

    Science.gov (United States)

    Yang, Fan; Kubota, Fukiko; Baba, Yuzo; Kamiya, Noriho; Goto, Masahiro

    2013-06-15

    The recycling of rare earth metals from phosphor powders in waste fluorescent lamps by solvent extraction using ionic liquids was studied. Acid leaching of rare earth metals from the waste phosphor powder was examined first. Yttrium (Y) and europium (Eu) dissolved readily in the acid solution; however, the leaching of other rare earth metals required substantial energy input. Ionization of target rare earth metals from the waste phosphor powders into the leach solution was critical for their successful recovery. As a high temperature was required for the complete leaching of all rare earth metals, ionic liquids, for which vapor pressure is negligible, were used as an alternative extracting phase to the conventional organic diluent. An extractant, N, N-dioctyldiglycol amic acid (DODGAA), which was recently developed, showed a high affinity for rare earth metal ions in liquid-liquid extraction although a conventional commercial phosphonic extractant did not. An effective recovery of the rare earth metals, Y, Eu, La and Ce, from the metal impurities, Fe, Al and Zn, was achieved from the acidic leach solution of phosphor powders using an ionic liquid containing DODGAA as novel extractant system.

  2. Enzyme-assisted extraction and ionic liquid-based dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for determination of patulin in apple juice and method optimization using central composite design.

    Science.gov (United States)

    Mohammadi, Abdorreza; Tavakoli, Rouya; Kamankesh, Marzieh; Rashedi, Hamid; Attaran, Abdolmohammad; Delavar, Mostafa

    2013-12-01

    A simple and highly sensitive analytical methodology for isolation and determination of patulin in apple-juice samples, based on enzyme-assisted extraction (EAE) and ionic liquid-based dispersive liquid-liquid microextraction (IL-DLLME) was developed and optimized. Enzymes play essential roles in eliminating interference and increasing the extraction efficiency of patulin. Apple-juice samples were treated with pectinase and amylase. A mixture of 80 μL ionic liquid and 600 μL methanol (disperser solvent) was used for the IL-DLLME process. The sedimented phase was analyzed by high-performance liquid chromatography (HPLC). Experimental parameters controlling the performance of DLLME, were optimized using response surface methodology (RSM) based on central composite design (CCD). Under optimum conditions, the calibration curves showed high levels of linearity (R(2)>0.99) for patulin in the range of 1-200 ng g(-1). The relative standard deviation (RSD) for the seven analyses was 7.5%. The limits of detection (LOD) and limits of quantification (LOQ) were 0.15 ng g(-1) and 0.5 ng g(-1), respectively. The merit figures, compared with other methods, showed that new proposed method is an accurate, precise and reliable sample-pretreatment method that substantially reduces sample matrix interference and gives very good enrichment factors and detection limits for investigation trace amount of patulin in apple-juice samples.

  3. Determination of flumequine and oxolinic acid in sediments and soils by microwave-assisted extraction and liquid chromatography-fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Prat, M.D. [Departament de Quimica Analitica, Universitat de Barcelona, Avda. Diagonal 647, E-08028 Barcelona (Spain)]. E-mail: mdprat@ub.edu; Ramil, D. [Departament de Quimica Analitica, Universitat de Barcelona, Avda. Diagonal 647, E-08028 Barcelona (Spain); Compano, R. [Departament de Quimica Analitica, Universitat de Barcelona, Avda. Diagonal 647, E-08028 Barcelona (Spain); Hernandez-Arteseros, J.A. [Departament de Quimica Analitica, Universitat de Barcelona, Avda. Diagonal 647, E-08028 Barcelona (Spain); Granados, M. [Departament de Quimica Analitica, Universitat de Barcelona, Avda. Diagonal 647, E-08028 Barcelona (Spain)

    2006-05-17

    A method is reported for the determination of the quinolones oxolinic acid and flumequine in aquatic sediments and agricultural soils. The analytes are extracted by liquid-liquid partitioning between a sample homogenated in an aqueous buffer solution and dichloromethane. Microwave-assisted extraction (MAE) was tested to improve the speed and efficiency of the extraction process. The parameters affecting the efficiency of MAE, such as irradiation time and temperature, were studied. The clean-up consists of back-extraction in 1 M sodium hydroxide. The determination is carried out by reversed phase liquid chromatography on an octyl silica-based column and fluorimetric detection. The optimised method was applied to the analysis of two sediments and one agricultural soil spiked with the analytes. The absolute recovery rates for the whole process range from 79% to 94% (RSD 3-7%), and detection limits are in the low {mu}g kg{sup -1} level.

  4. Insight into the extraction mechanism of polymeric ionic liquid sorbent coatings in solid-phase microextraction.

    Science.gov (United States)

    Ho, Tien D; Cole, William T S; Augusto, Fabio; Anderson, Jared L

    2013-07-12

    An investigation into the mechanism of extraction for polymeric ionic liquid (PIL)-based solid phase microextraction sorbent coatings is described. Four PIL-based coatings, namely, a poly(1-4-vinylbenzyl)-3-hexadecylimidazolium bis[(trifluoromethyl)sulfonyl] imide (poly([VBHDIM][NTf2])) PIL produced through 2,2'-azo-bis(isobutyronitrile) (AIBN) initiated free-radical polymerization, a UV-initiated poly(1-vinyl-3-hexylimidazolium) chloride (poly([VHIM][Cl])) PIL, and two crosslinked PILs containing the same IL monomers copolymerized with dicationic IL crosslinkers, were investigated. Calibration curves of 1-octanol were plotted in the presence of naphthalene, a model interfering compound, to observe changes in the linear range, sensitivity, and amount of analytes extracted. Results were compared with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) coating and a polyacrylate (PA) coating which are known to extract analytes primarily through adsorption and partitioning mechanisms, respectively. All PIL-based coatings extracted analytes via a non-competitive partitioning mechanism regardless of the extent of crosslinking.

  5. Determination of xanthohumol in beer based on cloud point extraction coupled with high performance liquid chromatography.

    Science.gov (United States)

    Chen, Ligang; Zhao, Qi; Jin, Haiyan; Zhang, Xiaopan; Xu, Yang; Yu, Aimin; Zhang, Hanqi; Ding, Lan

    2010-04-15

    A method based on coupling of cloud point extraction (CPE) with high performance liquid chromatography separation and ultraviolet detection was developed for determination of xanthohumol in beer. The nonionic surfactant Triton X-114 was chosen as the extraction medium. The parameters affecting the CPE were evaluated and optimized. The highest extraction yield of xanthohumol was obtained with 2.5% of Triton X-114 (v/v) at pH 5.0, 15% of sodium chloride (w/v), 70 degrees C of equilibrium temperature and 10 min of equilibrium time. Under these conditions, the limit of detection of xanthohumol is 0.003 mg L(-1). The intra- and inter-day precisions expressed as relative standard deviations are 4.6% and 6.3%, respectively. The proposed method was successfully applied for determination of xanthohumol in various beer samples. The contents of xanthohumol in these samples are in the range of 0.052-0.628 mg L(-1), and the recoveries ranging from 90.7% to 101.9% were obtained. The developed method was demonstrated to be efficient, green, rapid and inexpensive for extraction and determination of xanthohumol in beer.

  6. Enhanced mass transfer during solid-liquid extraction of gamma-irradiated red beetroot

    Energy Technology Data Exchange (ETDEWEB)

    Nayak, Chetan A. [Department of Food Engineering, Central Food Technological Research Institute, Mysore 570 020 (India); Chethana, S. [Department of Food Engineering, Central Food Technological Research Institute, Mysore 570 020 (India); Rastogi, N.K. [Department of Food Engineering, Central Food Technological Research Institute, Mysore 570 020 (India)]. E-mail: nkrastogi@cftri.com; Raghavarao, K.S.M.S. [Department of Food Engineering, Central Food Technological Research Institute, Mysore 570 020 (India)

    2006-01-15

    The exposure to gamma-irradiation pretreatment increases cell wall permeabilization, resulting in loss of turgor pressure, which led to the increase of extractability of betanin from red beetroot. The degree of extraction of betanin was investigated using gamma irradiation as a pretreatment prior to the solid-liquid extraction process and compared with control beetroot samples. The beetroot subjected to different doses of gamma irradiation (2.5, 5.0, 7.5, 10.0 kGy) and control was dipped in an acetic acid medium (1% v/v) to extract the betanin. The diffusion coefficients for betanin as well as ionic component were estimated considering Fickian diffusion. The results indicated an increase in the diffusion coefficient of betanin (0.302x10{sup -9}-0.463x10{sup -9} m{sup 2}/s) and ionic component (0.248x10{sup -9}-0.453x10{sup -9} m{sup 2}/s) as the dose rate increased (from 2.5 to 10.0 kGy). The degradation constant was found to increase (0.050-0.079 min{sup -1}) with an increase gamma-irradiation doses (2.5-10.0 kGy), indicating lower stability of the betanin as compared to control sample at 65 deg. C.

  7. [Determination of six pesticides in milk using cloud point extraction-high performance liquid chromatography].

    Science.gov (United States)

    Wang, Jian; Cui, Yanmei; Liu, Wei; Yang, Mingmin; Chen, Jianbo

    2007-11-01

    The feasibility of employing cloud point extraction (CPE) as extraction and preconcentration method for the recovery of herbicides from milk samples followed by high performance liquid chromatography (HPLC) analysis is demonstrated. An aqueous surfactant solution containing 60 g/L Tween 20 or Triton X-100 was heated with an appropriate concentration of (NH4)2SO4 or NaCl for the extraction of herbicides. The extract was analyzed by HPLC subsequently. Six herbicides in milk were analyzed simultaneously. The results showed that the linear dynamic ranges of detection were 20 - 10 000 microg/L for tralkoxydim, metribuzin and bromoxynil, 30 - 10 000 microg/L for mefenacet, and 50 - 10 000 microg/L for bensulfuron-methyl and nicosulfuron. The correlation coefficients were 0.998 1 - 0.999 7. The average recoveries of the six herbicides ranged from 85.09% to 96.74%. The relative standard deviations for the six herbicides were in the range of 1.90% - 3.98%. The limits of detection for the six pesticides were lower than the maximum residue limits (MRL) of China. The results indicate that the method is easier, faster, sensitive and produces less pollutants.

  8. The isolation of soyasaponins by fractional precipitation, solid phase extraction, and low pressure liquid chromatography.

    Science.gov (United States)

    Gurfinkel, D M; Reynolds, W F; Rao, A V

    2005-11-01

    Bioactive soyasaponins are present in soybean (Glycine max). In this study, the isolation of soyasaponins in relatively pure form (>80%) using precipitation, solid phase extraction and reverse phase low pressure liquid chromatography (RP-LPLC) is described. Soy flour soyasaponins were separated from non-saponins by methanol extraction and precipitation with ammonium sulphate. Acetylated group A soyasaponins were isolated first by solid phase extraction followed by RP-LPLC (solvent: ethanol-water). Soyasaponins, from a commercial preparation, were saponified and fractionated into deacetylated group A and group B soyasaponins by solid phase extraction (methanol-water). Partial hydrolysis of group B soyasaponins produced a mixture of soyasaponin III and soyasapogenol B monoglucuronide. RP-LPLC of deacetylated group A soyasaponins separated soyasaponin A1 and A2 (38% methanol); of group B soyasaponins isolated soyasaponin I (50% ethanol); and of the partial hydrolysate separated soyasaponin III from soyasapogenol B monoglucuronide (50% ethanol). This methodology provides soyasaponin fractions that are suitable for biological evaluation.

  9. Chromatographic analysis of Polygalae Radix by online hyphenating pressurized liquid extraction

    Science.gov (United States)

    Song, Yuelin; Song, Qingqing; Li, Jun; Shi, Shepo; Guo, Liping; Zhao, Yunfang; Jiang, Yong; Tu, Pengfei

    2016-06-01

    Practicing “green analytical chemistry” is of great importance when profiling the chemical composition of complex matrices. Herein, a novel hybrid analytical platform was developed for direct chemical analysis of complex matrices by online hyphenating pressurized warm water extraction followed by turbulent flow chromatography coupled with high performance liquid chromatography-tandem mass spectrometry (PWWE-TFC-LC-MS/MS). Two parallel hollow guard columns acted as extraction vessels connected to a long narrow polyether ether ketone tube, while warm water served as extraction solvent and was delivered at a flow rate of 2.5 mL/min to generate considerable back pressure at either vessel. A column oven heated both the solvent and crude materials. A TFC column, which is advantageous for the comprehensive trapping of small molecular substances from fluids under turbulent flow conditions, was employed to transfer analytes from the PWWE module to LC-MS/MS. Two electronic valves alternated each vessel between extraction and elution phases. As a proof-of-concept, a famous herbal medicine for the treatment of neurodegenerative disorders, namely Polygalae Radix, was selected for the qualitative and quantitative analyses. The results suggest that the hybrid platform is advantageous in terms of decreasing time, material, and solvent consumption and in its automation, versatility, and environmental friendliness.

  10. Ultrasonic Removal of Mucilage for Pressurized Liquid Extraction of Omega-3 Rich Oil from Chia Seeds (Salvia hispanica L.).

    Science.gov (United States)

    Castejón, Natalia; Luna, Pilar; Señoráns, Francisco J

    2017-03-29

    Chia (Salvia hispanica L.) seeds contain an important amount of edible oil rich in omega-3 fatty acids. Fast and alternative extraction techniques based on polar solvents, such as ethanol or water, have become relevant for oil extraction in recent years. However, chia seeds also contain a large amount of soluble fiber or mucilage, which makes difficult an oil extraction process with polar solvents. For that reason, the aim of this study was to develop a gentle extraction method for mucilage in order to extract chia oil with polar solvents using pressurized liquids and compare with organic solvent extraction. The proposed mucilage extraction method, using an ultrasonic probe and only water, was optimized at mild conditions (50 °C and sonication 3 min) to guarantee the omega-3 oil quality. Chia oil extraction was performed using pressurized liquid extraction (PLE) with different solvents and their mixtures at five different extraction temperatures (60, 90, 120, 150, and 200 °C). Optimal PLE conditions were achieved with ethyl acetate or hexane at 90 °C in only 10 min of static extraction time (chia oil yield up to 30.93%). In addition, chia oils extracted with nonpolar and polar solvents by PLE were analyzed by gas chromatography-mass spectrometry (GC-MS) to evaluate fatty acid composition at different extraction conditions. Chia oil contained ∼65% of α-linolenic acid regardless of mucilage extraction method, solvent, or temperature used. Furthermore, tocopherols and tocotrienols were also analyzed by HPLC in the extracted chia oils. The mucilage removal allowed the subsequent extraction of the chia oil with polar or nonpolar solvents by PLE producing chia oil with the same fatty acid and tocopherol composition as traditional extraction.

  11. Miniaturized selective pressurized liquid extraction of polychlorinated biphenyls and polybrominated diphenyl ethers from feedstuffs.

    Science.gov (United States)

    Pena-Abaurrea, M; Ramos, J J; Gonzalez, M J; Ramos, L

    2013-01-18

    A new miniaturized pressurized liquid extraction (PLE) with in-cell purification method has been developed for the simultaneous extraction of endogenous prioritary and toxic polychlorinated biphenyls (PCBs) and environmentally relevant tri- to deca-brominated diphenyl ether (PBDE) congeners from different feed matrices. Parameters affecting the efficiency of the selective PLE process, such as sorbent:matrix ratio, volume and nature of the extraction solvent, PLE working mode, extraction time and temperature, and amount of co-sorbents, were optimized. n-Hexane and n-hexane:dichloromethane (1:1, v/v) were used as extraction solvents. 8-mL of organic solvents and 3.5 g of sorbents sufficed for complete sample treatment. Only 0.25 g of feed sample were required for accurate determination of the endogenous PCBs studied using gas chromatography with a micro-electron capture detector (GC-μECD) during method development, and for PBDE analysis using either GC-μECD or gas chromatography with negative chemical ionization-quadrupole mass spectrometry (GC-NCI-qMS). Gas chromatography coupled to ion trap detection working in tandem mode, GC-ITD (MS/MS), was used for final PCB confirmation. Additional purification of the sample extracts was not required. The performance of the complete PLE-based method was evaluated at two spiking levels, 0.4 and 4 ng/g wet weight. Recoveries in the range 60-120% were obtained for PCBs, while those of PBDEs ranged from 86% to 114% for most of the target analytes. The relative standard deviations were in general lower than 20%. The optimized procedure was applied to the determination of the investigated PCBs and PBDEs in a variety of feed samples.

  12. Comparison of air-agitated liquid-liquid microextraction technique and conventional dispersive liquid-liquid micro-extraction for determination of triazole pesticides in aqueous samples by gas chromatography with flame ionization detection.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Mogaddam, Mohammad Reza Afshar; Aghdam, Abdollah Abdollahi

    2013-07-26

    Two micro-extraction methods, air-agitated liquid-liquid microextraction (AALLME) and dispersive liquid-liquid microextraction (DLLME), have been compared with each other by applying them for the analysis of five triazole pesticides (penconazole, hexaconazole, diniconazole, tebuconazole and triticonazole) in aqueous samples by gas chromatography with flame ionization detection (GC-FID). In the AALLME method, which excludes any disperser solvent, much less volume of organic solvent is used. In order to form fine and dispersed organic droplets in the aqueous phase, the mixture of aqueous sample solution and extraction solvent is repeatedly aspirated and dispensed with a syringe. In the DLLME method, an appropriate mixture of extraction solvent and disperser solvent is rapidly injected by a syringe into the aqueous sample. Effect of the pertinent experimental factors on DLLME (i.e. identity and volume of the extraction and disperser solvents and ionic strength) and on AALLME (identity and volume of the extraction solvent, number of agitations, and ionic strength) were investigated. Under optimal conditions, limits of detection for the five target pesticides obtained by AALLME-GC-FID and DLLME-GC-FID ranged from 0.20 to 1.1ngmL(-1) and 1.9 to 5.9ngmL(-1), respectively. The relative standard deviations (RSDs, n=5) were in the range of 1-4% and 3-5% with the enrichment factors of 449-504 and 79-143 for AALLME-GC-FID and DLLME-GC-FID, respectively. Both of the compared methods are simple, fast, efficient, inexpensive and can be applied to the analysis of the five pesticides in different aqueous samples in which penconazole and hexaconazole were found. For spiked samples, the recoveries were in the ranges of 92-105%, and 92-104% for AALLME and DLLME, respectively.

  13. Ionic liquid-based microwave-assisted extraction of essential oil and biphenyl cyclooctene lignans from Schisandra chinensis Baill fruits.

    Science.gov (United States)

    Ma, Chun-hui; Liu, Ting-ting; Yang, Lei; Zu, Yuan-gang; Chen, Xiaoqiang; Zhang, Lin; Zhang, Ying; Zhao, Chunjian

    2011-12-02

    Ionic liquid-based microwave-assisted extraction (ILMAE) has been successfully applied in extracting essential oil and four kinds of biphenyl cyclooctene lignans from Schisandra chinensis Baill. 0.25 M 1-lauryl-3-methylimidazolium bromide ionic liquid is selected as solvent. The optimum parameters of dealing with 25.0 g sample are 385 W irradiation power, 40 min microwave extraction time and 1:12 solid-liquid ratio. The yields of essential oil and lignans are 12.12±0.37 ml/kg and 250.2±38.2 mg/kg under the optimum conditions. The composition of the essential oil extracted by hydro-distillation, steam-distillation and ILMAE is analyzed by GC-MS. With ILMAE method, the energy consumption time has not only been shortened to 40 min (hydro-distillation 3.0 h for extracting essential oil and reflux extraction 4.0 h for extracting lignans, respectively), but also the extraction efficiency has been improved (extraction of lignans and distillation of essential oil at the same time) and reduces the environmental pollution. S. chinensis materials treated by different methods are observed by scanning electronic microscopy. Micrographs provide more evidence to prove that ILMAE is a better and faster method. The experimental results also indicate that ILMAE is a simple and efficient technique for sample preparation.

  14. Mathematical modeling of liquid/liquid hollow fiber membrane contactor accounting for interfacial transport phenomena: Extraction of lanthanides as a surrogate for actinides

    Energy Technology Data Exchange (ETDEWEB)

    Rogers, J.D.

    1994-08-04

    This report is divided into two parts. The second part is divided into the following sections: experimental protocol; modeling the hollow fiber extractor using film theory; Graetz model of the hollow fiber membrane process; fundamental diffusive-kinetic model; and diffusive liquid membrane device-a rigorous model. The first part is divided into: membrane and membrane process-a concept; metal extraction; kinetics of metal extraction; modeling the membrane contactor; and interfacial phenomenon-boundary conditions-applied to membrane transport.

  15. Solvent bar micro-extraction with graphite atomic absorption spectrometry for the determination of silver in ocean water.

    Science.gov (United States)

    López-López, José A; Herce-Sesa, Belén; Moreno, Carlos

    2016-10-01

    Main drawbacks for silver determination in seawater are the effects of samples matrix and that Ag appears in the sub ng L(-1). Available methods for sample preparation in Ag analysis are based on solid and liquid extraction using tedious process that increase the cost of analysis and the risk of sample contamination, producing important waste amounts. Solvent bar micro-extraction (SBME) allows the pre-concentration of Ag in a micro-volume of the ionic liquid Aliquat 336® in kerosene solution. For this reason, it is considered as a green alternative to standard methods. The method has been optimized using synthetic seawater samples, offering the highest response for samples at pH=2, using 5% Aliquat 336® dissolved in kerosene containing 5% dodecan-1-ol as acceptor solution and after 1h stirring at 800rpm. The method exhibited linearity up to 50ngL(-1), with a limit of detection of 0.09ngL(-1), covering the concentration range of interest for environmental studies. Finally, it was applied for determination of Ag in real seawater samples, and the results were compared with the reference method of liquid-liquid extraction with 1-pyrrolidine-dithiocarbamate and diethylammonium-diethyldithiocarbamate, showing the applicability of ionic liquid based SBME using Aliquat 336(®) for the simple monitoring of silver ultra-traces in seawater analysis.

  16. Analysis of 30 synthetic cannabinoids in serum by liquid chromatography-electrospray ionization tandem mass spectrometry after liquid-liquid extraction.

    Science.gov (United States)

    Kneisel, Stefan; Auwärter, Volker

    2012-07-01

    The analysis of synthetic cannabinoids in human matrices is of particular importance in the fields of forensic and clinical toxicology since cannabis users partly shift to the consumption of 'herbal mixtures' as a legal alternative to cannabis products in order to circumvent drug testing. However, comprehensive methods covering the majority of synthetic cannabinoids already identified on the drug market are still lacking. In this article, we present a fully validated method for the analysis of 30 synthetic cannabinoids in human serum utilizing liquid-liquid extraction and liquid chromatography-electrospray ionization tandem mass spectrometry. The method proved to be suitable for the quantification of 27 substances. The limits of detection ranged from 0.01 to 2.0 ng/mL, whereas the lower limits of quantification were in the range from 0.1 to 2.0 ng/mL. The presented method was successfully applied to 833 authentic serum samples during routine analysis between August 2011 and January 2012. A total of 227 (27%) samples was tested positive for at least one of the following synthetic cannabinoids: JWH-018, JWH-019, JWH-073, JWH-081, JWH-122, JWH-200, JWH-203, JWH-210, JWH-307, AM-2201 and RCS-4. The most prevalent compounds in positive samples were JWH-210 (80%), JWH-122 (63%) as well as AM-2201 (29%). Median serum concentrations were all below 1.0 ng/mL. These findings demonstrate a significant shift of the market of synthetic cannabinoids towards substances featuring a higher CB(1) binding affinity and clearly emphasize that the analysis of synthetic cannabinoids in serum or blood samples requires highly sensitive analytical methods covering a wide spectrum of substances. Copyright © 2012 John Wiley & Sons, Ltd.

  17. Ultrasound-assisted low-density solvent dispersive liquid-liquid extraction for the determination of alkanolamines and alkylamines in cosmetics with ion chromatography.

    Science.gov (United States)

    Zhong, Zhixiong; Li, Gongke; Zhong, Xiuhua; Luo, Zhibin; Zhu, Binghui

    2013-10-15

    A new one-step sample preparation technique termed ultrasound-assisted low-density solvent dispersive liquid-liquid extraction (UA-LDS-DLLE) coupled with ion chromatography (IC) was developed for the determination of three alkanolamines and two alkylamines in complex samples. Sample matrices were rapidly dissolved and dispersed to form cloudy solutions by using two solvents, where target analytes were transferred into acid solutions, while liposoluble substances were dissolved in cyclohexane. The obtained extracts could be used directly for injection analysis without any additional purification because the potential matrix interferences had been effectively eliminated in extraction process. The extraction efficiency could be markedly enhanced and the extraction could be quickly accomplished within 13 min under the synergistic effects of ultrasound radiation, vibration and heating. Various parameters influencing extraction efficiency were evaluated using orthogonal array experimental design. The extraction performance of the approach was demonstrated for the determination of target analytes in 15 commercial cosmetics covering very different matrices. Linearity ranges of 0.3-50 mg L(-1) and limits of detection varying from 0.072 to 0.12 mg L(-1) were achieved. The recoveries ranged from 86.9-108.5% with the relative standard deviations (RSDs) of 1.2-6.2%. The method was proved to be a simple and effective extraction technique that provided an attractive alternative to the analysis of trace amounts of target analytes in large numbers of cosmetics. Copyright © 2013. Published by Elsevier B.V.

  18. Partition Behavior of Penicillin in Three-liquid-phase Extraction System

    Institute of Scientific and Technical Information of China (English)

    谭显东; 季清荣; 常志东

    2006-01-01

    Partition behavior of penicillins G and V was studied in a novel three-liquid-phase extraction system, which is composed of butyl acetate (BA), polyethylene glycol (PEG), ammonia sulfate [(NH4)2SO4] and water (H2O). The main components in the top, middle and bottom phases are butyl acetate, polyethylene glycol aqueous solution and ammonia sulfate aqueous solution, respectively. Some parameters such as partition coefficients Di/j and mass fractions Ei ofpenicillins G and V were determined at the room temperature, respectively. Experimental efforts have been made to investigate the partition behavior of penicillin in the three-liquid-phase extraction system, including initial concentrations of phase-forming components [PEG and (NH4)2SO4], PEG molecular weight, pH, initial concentration of penicillin. The results indicated that penicillins G and V have the similar partition behavior. They preferentially distribute into the middle phase with the increase of initial concentration of phase-forming components and into the top phase with the decrease of pH, while partition coefficient Dm/b is hardly affected by pH value. The variation of PEG molecular weight has little effect on mass fractions of penicillin. The increase of initial concentration of penicillins G and V could lead to the increase of Dt/b, Dm/b and the decrease of Dt/m, while their mass fractions in all phases were almost independent on their initial concentrations.

  19. Laboratory Production of Lemon Liqueur (Limoncello) by Conventional Maceration and a Two-Syringe System to Illustrate Rapid Solid-Liquid Dynamic Extraction

    Science.gov (United States)

    Naviglio, Daniele; Montesano, Domenico; Gallo, Monica

    2015-01-01

    Two experimental techniques of solid-liquid extraction are compared relating to the lab-scale production of lemon liqueur, most commonly named "limoncello"; the first is the official method of maceration for the solid-liquid extraction of analytes and is widely used to extract active ingredients from a great variety of natural products;…

  20. Guanidinium ionic liquid-based surfactants as low cytotoxic extractants: Analytical performance in an in-situ dispersive liquid-liquid microextraction method for determining personal care products.

    Science.gov (United States)

    Pacheco-Fernández, Idaira; Pino, Verónica; Ayala, Juan H; Afonso, Ana M

    2017-05-01

    The IL-based surfactant octylguanidinium chloride (C8Gu-Cl) was designed and synthetized with the purpose of obtaining a less harmful surfactant: containing guanidinium as core cation and a relatively short alkyl chain. Its interfacial and aggregation behavior was evaluated through conductivity and fluorescence measurements, presenting a critical micelle concentration value of 42.5 and 44.6mmolL(-1), respectively. Cytotoxicity studies were carried out with C8Gu-Cl and other IL-based and conventional surfactants, specifically the analogue 1-octyl-3-methylimidazolium chloride (C8MIm-Cl), and other imidazolium- (C16MIm-Br) and pyridinium- (C16Py-Cl) based surfactants, together with the conventional cationic CTAB and the conventional anionic SDS. From these studies, C8Gu-Cl was the only one to achieve the classification of low cytotoxicity. An in situ dispersive liquid-liquid microextraction (DLLME) method based on transforming the water-soluble C8Gu-Cl IL-based surfactant into a water-insoluble IL microdroplet via a simple metathesis reaction was then selected as the extraction/preconcentration method for a group of 6 personal care products (PCPs) present in cosmetic samples. The method was carried out in combination with high-performance liquid chromatography (HPLC) and diode array detection (DAD). The method was properly optimized, requiring the use of only 30μL of C8Gu-Cl for 10mL of aqueous sample with a NaCl content of 8% (w/v) to adjust the ionic strength and pH value of 5. The metathesis reaction required the addition of the anion exchange reagent (bis[(trifluoromethyl)sulfonyl]imide - 1:1 molar ratio), followed by vortex and centrifugation, and dilution of the final microdroplet up to 60μL with acetonitrile before the injection in the HPLC-DAD system. The optimum in situ DLLME-HPLC-DAD method takes ∼10min for the extraction step and ∼22min for the chromatographic separation, with analytical features of low detection limits: down to 0.4μgL(-1); high

  1. Selective liquid CO2 extraction of purine alkaloids in different Ilex paraguariensis progenies grown under environmental influences.

    Science.gov (United States)

    Cardozo, Euclides Lara; Cardozo-Filho, Lucio; Filho, Osvaldo Ferrarese; Zanoelo, Everton Fernando

    2007-08-22

    In this investigation, liquid carbon dioxide at 20 degrees C and 150 bar was used for the selective extraction of caffeine and theobromine from dry leaves of mate. A comparison between the chromatograms from CO2 extraction and traditional solvent extraction supports the selectivity of carbon dioxide for these purine alkaloids. The advantages of selective liquid CO2 extraction in terms of speed and resolution of UV/HPLC is also evidenced. A randomized block design of experiments was proposed to investigate the influence of 16 progenies of Ilex paraguariensis grown in 3 diverse sites on the contents of caffeine and theobromine in liquors of mate leaves obtained by extraction with compressed CO2. A significant effect of both these factors on the parameters investigated was observed by involving the F distribution in the statistical analysis. A cluster analysis based on the experimental uncertainties in the contents of these two methylxanthines has identified from four to six different groups of mate progenies.

  2. Multi-residue quantification of veterinary drugs in milk with a novel extraction and cleanup technique: salting out supported liquid extraction (SOSLE).

    Science.gov (United States)

    Kaufmann, A; Butcher, P; Maden, K; Walker, S; Widmer, M

    2014-04-11

    A quantitative liquid chromatography coupled with high-resolution mass spectrometry method was developed for the determination of more than one hundred compounds belonging to a variety of veterinary drug classes in bovine milk. Salting out supported liquid extraction (SOSLE), a novel extraction and cleanup technique, was introduced to ensure high extraction efficiency and good sample cleanup. The high salt (ammonium sulfate) concentration in the aqueous donor phase permits supported liquid/liquid extraction (SLE) with a relative polar organic acceptor phase (acetonitrile). This is different from traditional SLE, in which the need for phase separation results in the selection of organic solvents with intermediate polarities (e.g., ethyl acetate or dichloromethane). Hence, SOSLE is more efficient in recovering polar analytes than conventional SLE. SOSLE was also compared to classical approaches like solid phase extraction, QuEChERS and ultra-filtration. The proposed technique resulted in extracts of equal or superior cleanliness and with higher average recoveries than those obtained with QuEChERS or SPE. The recovery (median for all compounds) was 73% for QuEChERS, 83% for SPE and 91% for SOSLE. The most significant improvements were observed for polar analytes (penicillines, quinolones and tetracyclines) which are hardly recovered by QuEChERS. The chromatographic separation and detection was based on an ultra-high-performance liquid chromatography Q-Orbitrap system (Q-Exactive plus). The developed analytical method has been validated (based on the commission decision 2002/957/EC) as required for quantitative veterinary drug methods.

  3. Application of Ionic Liquids in the Microwave-Assisted Extraction of Proanthocyanidins from Larix gmelini Bark

    Directory of Open Access Journals (Sweden)

    Yuangang Zu

    2012-04-01

    Full Text Available Ionic liquid based, microwave-assisted extraction (ILMAE was successfully applied to the extraction of proanthocyanidins from Larix gmelini bark. In this work, in order to evaluate the performance of ionic liquids in the microwave-assisted extraction process, a series of 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were evaluated for extraction yield, and 1-butyl-3-methylimidazolium bromide was selected as the optimal solvent. In addition, the ILMAE procedure for the proanthocyanidins was optimized and compared with other conventional extraction techniques. Under the optimized conditions, satisfactory extraction yield of the proanthocyanidins was obtained. Relative to other methods, the proposed approach provided higher extraction yield and lower energy consumption. The Larix gmelini bark samples before and after extraction were analyzed by Thermal gravimetric analysis, Fourier-transform infrared spectroscopy and characterized by scanning electron microscopy. The results showed that the ILMAE method is a simple and efficient technique for sample preparation.

  4. PEG-salt aqueous two-phase systems: an attractive and versatile liquid-liquid extraction technology for the downstream processing of proteins and enzymes.

    Science.gov (United States)

    Glyk, Anna; Scheper, Thomas; Beutel, Sascha

    2015-08-01

    Nowadays, there is an increasing demand to establish new feasible, efficient downstream processing (DSP) techniques in biotechnology and related fields. Although several conventional DSP technologies have been widely employed, they are usually expensive and time-consuming and often provide only low recovery yields. Hence, the DSP is one major bottleneck for the commercialization of biological products. In this context, polyethylene glycol (PEG)-salt aqueous two-phase systems (ATPS) represent a promising, efficient liquid-liquid extraction technology for the DSP of various biomolecules, such as proteins and enzymes. Furthermore, ATPS can overcome the limitations of traditional DSP techniques and have gained importance for applications in several fields of biotechnology due to versatile advantages over conventional DSP methods, such as biocompatibility, technical simplicity, and easy scale-up potential. In the present review, various practical applications of PEG-salt ATPS are presented to highlight their feasibility to operate as an attractive and versatile liquid-liquid extraction technology for the DSP of proteins and enzymes, thus facilitating the approach of new researchers to this technique. Thereby, single- and multi-stage extraction, several process integration methods, as well as large-scale extraction and purification of proteins regarding technical aspects, scale-up, recycling of process chemicals, and economic aspects are discussed.

  5. Comparison of ultrasound-assisted cloud point extraction and ultrasound-assisted dispersive liquid liquid microextraction for copper coupled with spectrophotometric determination.

    Science.gov (United States)

    Yang, Shengchun; Fang, Xiang; Duan, Liju; Yang, Shu; Lei, Zirong; Wen, Xiaodong

    2015-09-01

    In this work, ultrasound-assisted cloud point extraction (UA-CPE) and ultrasound-assisted dispersive liquid liquid microextraction (UA-DLLME) were investigated and compared firstly as ultrasound-assisted liquid phase microextraction methods, which were coupled with spectrophotometer for copper preconcentration and detection. Compared to conventional CPE and DLLME, the extraction patterns were changed and improved by the effect of ultrasound. As novel methods, their applications were expanded and the analytical performance of spectrophotometric determination for copper was considerably improved. The influence factors of UA-CPE and UA-DLLME were studied in detail. Under the optimal conditions, the limits of detection (LODs) for copper were 0.7 μg L(-1) of UA-CPE and 0.8 μg L(-1) of UA-DLLME with sensitivity enhancement factors (EFs) of 17 and 16. The developed methods were applied to the determination of trace copper in real water samples with satisfactory analytical results.

  6. Comparison of ultrasound-assisted cloud point extraction and ultrasound-assisted dispersive liquid liquid microextraction for copper coupled with spectrophotometric determination

    Science.gov (United States)

    Yang, Shengchun; Fang, Xiang; Duan, Liju; Yang, Shu; Lei, Zirong; Wen, Xiaodong

    2015-09-01

    In this work, ultrasound-assisted cloud point extraction (UA-CPE) and ultrasound-assisted dispersive liquid liquid microextraction (UA-DLLME) were investigated and compared firstly as ultrasound-assisted liquid phase microextraction methods, which were coupled with spectrophotometer for copper preconcentration and detection. Compared to conventional CPE and DLLME, the extraction patterns were changed and improved by the effect of ultrasound. As novel methods, their applications were expanded and the analytical performance of spectrophotometric determination for copper was considerably improved. The influence factors of UA-CPE and UA-DLLME were studied in detail. Under the optimal conditions, the limits of detection (LODs) for copper were 0.7 μg L-1 of UA-CPE and 0.8 μg L-1 of UA-DLLME with sensitivity enhancement factors (EFs) of 17 and 16. The developed methods were applied to the determination of trace copper in real water samples with satisfactory analytical results.

  7. Method for determination of uranium isotopes in environmental samples by liquid-liquid extraction with triisooctylamine/xylene in hydrochloric media and alpha spectrometry.

    Science.gov (United States)

    Popov, L

    2012-10-01

    Alternative method for determination of uranium isotopes in various environmental samples is presented. The method is based on total decomposition of the solid materials and preconcentration of liquid samples. The separation of uranium from interfering radionuclides and stable matrix elements is attained by liquid-liquid extraction with triisooctylamine/xylene in hydrochloric media. After the additional removal of stable iron by extraction with diisopropyl ether, purified uranium is electrodeposited on stainless steel disks and measured by alpha spectrometry. The analytical method has been successfully applied to the determination of uranium isotopes in water and bottom sediments from the rivers Danube, Ogosta and Tzibritza in Northwestern Bulgaria. The analytical quality was checked by analyzing reference materials with different matrices.

  8. EPA Method 8321B (SW-846): Solvent-Extractable Nonvolatile Compounds by High Performance Liquid Chromatography-Thermospray-Mass Spectrometry (HPLC-TS-MS) or Ultraviolet (UV) Detection

    Science.gov (United States)

    Method 8321B describes procedures for preparation and analysis of solid, aqueous liquid, drinking water and wipe samples using high performance liquid chromatography and mass spectrometry for extractable non-volatile compounds.

  9. Direct extraction of genomic DNA from maize with aqueous ionic liquid buffer systems for applications in genetically modified organisms analysis.

    Science.gov (United States)

    Gonzalez García, Eric; Ressmann, Anna K; Gaertner, Peter; Zirbs, Ronald; Mach, Robert L; Krska, Rudolf; Bica, Katharina; Brunner, Kurt

    2014-12-01

    To date, the extraction of genomic DNA is considered a bottleneck in the process of genetically modified organisms (GMOs) detection. Conventional DNA isolation methods are associated with long extraction times and multiple pipetting and centrifugation steps, which makes the entire procedure not only tedious and complicated but also prone to sample cross-contamination. In recent times, ionic liquids have emerged as innovative solvents for biomass processing, due to their outstanding properties for dissolution of biomass and biopolymers. In this study, a novel, easily applicable, and time-efficient method for the direct extraction of genomic DNA from biomass based on aqueous-ionic liquid solutions was developed. The straightforward protocol relies on extraction of maize in a 10 % solution of ionic liquids in aqueous phosphate buffer for 5 min at room temperature, followed by a denaturation step at 95 °C for 10 min and a simple filtration to remove residual biopolymers. A set of 22 ionic liquids was tested in a buffer system and 1-ethyl-3-methylimidazolium dimethylphosphate, as well as the environmentally benign choline formate, were identified as ideal candidates. With this strategy, the quality of the genomic DNA extracted was significantly improved and the extraction protocol was notably simplified compared with a well-established method.

  10. Ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME)-a fast new approach to measure phthalate metabolites in nails.

    Science.gov (United States)

    Alves, Andreia; Vanermen, Guido; Covaci, Adrian; Voorspoels, Stefan

    2016-09-01

    A new, fast, and environmentally friendly method based on ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME) was developed and optimized for assessing the levels of seven phthalate metabolites (including the mono(ethyl hexyl) phthalate (MEHP), mono(2-ethyl-5-hydroxyhexyl) phthalate (5-OH-MEHP), mono(2-ethyl-5-oxohexyl) phthalate (5-oxo-MEHP), mono-n-butyl phthalate (MnBP), mono-isobutyl phthalate (MiBP), monoethyl phthalate (MEP), and mono-benzyl phthalate (MBzP)) in human nails by UPLC-MS/MS. The optimiza