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Sample records for ionic liquid-based ultrasound-assisted

  1. Ultrasound-assisted ionic liquid-based homogeneous liquid-liquid microextraction high-performance liquid chromatography for determination of tanshinones in Salvia miltiorrhiza Bge. root.

    Science.gov (United States)

    Wang, Zhibing; Cao, Bocheng; Yu, Aimin; Zhang, Hanqi; Qiu, Fangping

    2015-02-01

    The ultrasound-assisted ionic liquid-based homogeneous liquid-liquid microextraction has been developed and applied to the extraction of four tanshinones, including dihydrotanshinone, tanshinone I, cryptotanshinone and tanshinone IIA in Salvia miltiorrhiza Bge. root. High performance liquid chromatography was applied to the separation and determination of the analytes. The ionic liquid was used as extraction solvent and target analytes were extracted with help of ultrasound. Then, ion-pairing agent was added into the sample solution, which resulted in the formation of water-insoluble ionic liquid in the solution. The phase separation was performed by centrifugation. The extraction, concentration and purification of target analytes were performed simultaneously. The experimental parameters, including type and volume of ionic liquid, sample amount, the size of sample particle, pH value of extraction medium, extraction temperature, extraction time, amount of ion-pairing agent and centrifuging time, were investigated and optimized. The calibration curves showed good linear relationship (r>0.9997). The limits of detection and quantification were in the range of 0.052-0.093 and 0.17-0.31 μg mL(-1), respectively. The recoveries were between 70.45% and 94.23% with relative standard deviations lower than 5.31%. The present method is free of volatile organic solvents, and represents lower expenditures of sample, extraction time and solvent, compared with UAE and HRE. There was no obvious difference in the extraction yields of active constitutions obtained by the three extraction methods. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Rapid ionic liquid-based ultrasound assisted dual magnetic microextraction to preconcentrate and separate cadmium-4-(2-thiazolylazo)-resorcinol complex from environmental and biological samples.

    Science.gov (United States)

    Khan, Sumaira; Kazi, Tasneem Gul; Soylak, Mustafa

    2014-04-05

    A rapid and innovative microextraction technique named as, ionic liquid-based ultrasound-assisted dual magnetic microextraction (IL-UA-DMME) was developed for the preconcentration and extraction of trace cadmium from environmental and biological samples, prior to analyzed by flame atomic absorption spectrometry (FAAS). The proposed method has many obvious advantages, including evading the use of organic solvents and achieved high extraction yields by the combination of dispersive liquid-liquid microextraction (DLLME) and magnetic mediated-solid phase extraction (MM-SPE). In this approach ionic liquid (IL) 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6] play an important role to extract the cadmium-4-(2-thiazolylazo)-resorcinol (Cd-TAR) complex from acid digested sample solutions and ultrasonic irradiation was applied to assist emulsification. After then, dispersed small amount of Fe3O4 magnetic nanoparticles (MNPs) in sample solutions to salvaged the IL and complete phase separation was attained. Some analytical parameters that influencing the efficiency of proposed (IL-UA-DMME) method, such as pH, volume of IL, ligand concentration, ultra-sonication time, amount of Fe3O4 MNPs, sample volume and matrix effect were optimized. Limit of detection (LOD) and enrichment factor (EF) of the method under optimal experimental conditions were found to be 0.40μgL(-1) and 100, respectively. The relative standard deviation (RSD) of 50μgL(-1) Cd was 4.29%. The validity and accuracy of proposed method, was assessed to analyzed certified reference materials of fortified lake water TMDA-54.4, SPS-WW2 waste water, spinach leaves 1570a and also checked by standard addition method. The obtained values showed good agreement with the certified values and sufficiently high recovery were found in the range of 98.1-101% for Cd. The proposed method was facile, rapid and successfully applied for the determination of Cd in environmental and different biological samples

  3. Ionic-liquid-based ultrasound-assisted extraction of isoflavones from Belamcanda chinensis and subsequent screening and isolation of potential α-glucosidase inhibitors by ultrafiltration and semipreparative high-performance liquid chromatography.

    Science.gov (United States)

    Li, Senlin; Li, Sainan; Huang, Yu; Liu, Chunming; Chen, Lina; Zhang, Yuchi

    2017-06-01

    The separation of a compound of interest from its structurally similar homologues to produce high-purity natural products is a challenging problem. This work proposes a novel method for the separation of iristectorigenin A from its structurally similar homologues by ionic-liquid-based ultrasound-assisted extraction and the subsequent screening and isolation of potential α-glucosidase inhibitors via ultrafiltration and semipreparative high-performance liquid chromatography. Ionic-liquid-based ultrasound-assisted extraction was successfully applied to the extraction of tectorigenin, iristectorigenin A, irigenin, and irisflorentin from Belamcanda chinensis. The optimum conditions for the efficient extraction of isoflavones were determined as 1.0 M 1-ethyl-3-methylimidazolium tetrafluoroborate with extraction time of 30 min and a solvent to solid ratio of 30 mL/g. Ultrafiltration with liquid chromatography and mass spectrometry was applied to screen and identify α-glucosidase inhibitors from B. chinensis, followed by the application of semipreparative high-performance liquid chromatography to separate and isolate the active constituents. Four major compounds including tectorigenin, iristectorigenin A, irigenin, and irisflorentin were screened and identified as α-glucosidase inhibitors, and then the four active compounds abovementioned were subsequently isolated by semipreparative high-performance liquid chromatography (99.89, 88.97, 99.79, and 99.97% purity, respectively). The results demonstrate that ionic liquid extraction can be successfully applied to the extraction of isoflavones from B. chinensis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Extraction and reliable determination of acrylamide from thermally processed foods using ionic liquid-based ultrasound-assisted selective microextraction combined with spectrophotometry.

    Science.gov (United States)

    Altunay, Nail; Elik, Adil; Gürkan, Ramazan

    2018-02-01

    Acrylamide (AAm) is a carcinogenic chemical that can form in thermally processed foods by the Maillard reaction of glucose with asparagine. AAm can easily be formed especially in frequently consumed chips and cereal-based foods depending on processing conditions. Considering these properties of AAm, a new, simple and green method is proposed for the extraction of AAm from thermally processed food samples. In this study, an ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate, [Bmim][BF 4 ]) as extractant was used in the presence of a cationic phenazine group dye, 3,7-diamino-5-phenylphenazinium chloride (PSH + , phenosafranine) at pH 7.5 for the extraction of AAm as an ion-pair complex from selected samples. Under optimum conditions, the analytical features obtained for the proposed method were as follows; linear working range, the limits of detection (LOD, 3S b /m) and quantification (LOQ, 10S b /m), preconcentration factor, sensitivity enhancement factor, sample volume and recovery% were 2.2-350 µg kg -1 , 0.7 µg kg -1 , 2.3 µg kg -1 , 120, 95, 60 mL and 94.1-102.7%, respectively. The validity of the method was tested by analysis of two certified reference materials (CRMs) and intra-day and inter-day precision studies. Finally, the method was successfully applied to the determination of AAm levels in thermally processed foods using the standard addition method.

  5. Ultrasound-assisted ionic liquid-based micellar extraction combined with microcrystalline cellulose as sorbent in dispersive microextraction for the determination of phenolic compounds in propolis.

    Science.gov (United States)

    Cao, Jun; Peng, Li-Qing; Du, Li-Jing; Zhang, Qi-Dong; Xu, Jing-Jing

    2017-04-22

    An ionic liquid-(IL) based micellar extraction combined with microcrystalline cellulose- (MCC) assisted dispersive micro solid-phase extraction method was developed to extract phenolic compounds from propolis. A total of 20 target compounds were identified by ultra-high- performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry. The main extraction parameters were optimized and included the ultrasonic power, ultrasonic time, sample pH, type of IL, the concentration of [C12mim]Br, extraction time, concentration of MCC, type of sorbent and type of elution solvents. Under the optimum conditions, the proposed method exhibited good linearities (r 2  ≥ 0.999) for all plant phenolic compounds with the lower limits of detection in the range of 0.21-0.41 ng/mL. The recoveries ranged from 82.74% to 97.88% for pinocembrin, chrysin and galangin. Compared with conventional solvent extraction, the present method was simpler and more efficient and required less organic solvent and a shorter extraction time. Finally, the methodology was successfully used for the extraction and enrichment of phenolic compounds in propolis. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. 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 [C8mim]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. PMID:23109836

  7. Ultrasound-Assisted Extraction of Carnosic Acid and Rosmarinic Acid Using Ionic Liquid Solution from Rosmarinus officinalis

    Directory of Open Access Journals (Sweden)

    Chunjian Zhao

    2012-09-01

    Full Text Available 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 [C8mim]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.

  8. 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. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Ionic liquid based multifunctional double network gel

    Science.gov (United States)

    Ahmed, Kumkum; Higashihara, Tomoya; Arafune, Hiroyuki; Kamijo, Toshio; Morinaga, Takashi; Sato, Takaya; Furukawa, Hidemitsu

    2015-04-01

    Gels are a promising class of soft and wet materials with diverse application in tissue engineering and bio-medical purpose. In order to accelerate the development of gels, it is required to synthesize multi-functional gels of high mechanical strength, ultra low surface friction and suitable elastic modulus with a variety of methods and new materials. Among many types of gel ionic gel made from ionic liquids (ILs) could be used for diverse applications in electrochemical devices and in the field of tribology. IL, a promising materials for lubrication, is a salt with a melting point lower than 100 °C. As a lubricant, ILs are characterized by an extremely low vapor pressure, high thermal stability and high ion conductivity. In this work a novel approach of making double network DN ionic gel using IL has been made utilizing photo polymerization process. A hydrophobic monomer Methyl methacrylate (MMA) has been used as a first network and a hydrophobic IL monomer, N,N-diethyl-N-(2-mthacryloylethyl)-N-methylammonium bistrifluoromethylsulfonyl)imide (DEMM-TFSI) has been used as a second network using photo initiator benzophenon and crosslinker triethylene glycol dimethacrylate (TEGDMA). The resulting DN ionic gel shows transparency, flexibility, high thermal stability, good mechanical toughness and low friction coefficient value which can be a potential candidate as a gel slider in different mechanical devices and can open a new area in the field of gel tribology.

  10. Removal of residual functionalized ionic liquids from water by ultrasound-assisted zero-valent iron/activated carbon.

    Science.gov (United States)

    Zhou, Haimei; Lv, Ping; Qi, Hang; Ma, Jinqi; Wang, Jianji

    2018-03-02

    Numerous applications of ionic liquids (ILs) are often accompanied by the generation of aqueous wastes. Due to the high toxicity and poor biodegradability of ILs, effective chemical treatment is of great importance for their removal from aqueous solution. In this work, an ultrasound-assisted zero-valent iron/activated carbon (US-ZVI/AC) micro-electrolysis technique was used to degrade residual functionalized ILs, 1-butyl-3-methyl benzimidazolium bromide ([BMBIM]Br) and 1-allyl-3-methylimidazolium chloride ([AMIM]Cl) in aqueous solution, and the degradation degree, degradation kinetics and possible degradation pathways were investigated. It was shown that the degradation of these functionalized ILs was highly efficient in the US-ZVI/AC system, and the degradation degree was as high as 96.1% and 92.9% in 110 min for [BMBIM]Br and [AMIM]Cl, respectively. The degradation of [BMBIM]Br could be described by the second-order kinetics model, and [BMBIM] + was decomposed in two ways: (i) sequential cleavage of N-alkyl side chain of the cation produced three intermediates; (ii) the 2-positioned H atoms of the benzimidazolium ring were first oxidized, and then the imidazolium ring was opened. The degradation of [AMIM]Cl followed the first-order kinetics rule, and the 2,4,5-positioned H atoms of the imidazolium ring were oxidized to induce ring opening. In addition, the removal of total organic carbon was found to be >87%, which indicates that most of the ILs was mineralized in the degradation process. These results suggest that ultrasound-assisted ZVI/AC micro-electrolysis is highly effective for the removal of residual functionalized ILs from aqueous environment.

  11. New Eco-Friendly 1-Alkyl-3-(4-phenoxybutyl Imidazolium-Based Ionic Liquids Derivatives: A Green Ultrasound-Assisted Synthesis, Characterization, Antibacterial Activity and POM Analyses

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    Mouslim Messali

    2014-08-01

    Full Text Available In view of the emerging importance of the ILs as “green” materials with wide applications and our general interests in green processes, a series of a twenty five new 1-alkyl-3-(4-phenoxybutyl imidazolium-based ionic liquids (ILs derivatives is synthesized using a facile and green ultrasound-assisted procedure. Their structures were characterized by FT-IR, 1H-NMR, 13C-NMR, 11B, 19F, 31P, and mass spectrometry. Antimicrobial screens of some selected ILs were conducted against a panel of Gram-positive and Gram-negative bacteria. The antimicrobial activity of each compound was measured by determination of the minimal inhibitory concentration (MIC yielding very interesting and promising results. Their antibacterial activities are reported, and, on the basis of the experimental and virtual POM screening data available, attempt is also made to elucidate the structure activity relationship.

  12. Ultrasound-assisted temperature-controlled ionic liquid emulsification microextraction coupled with capillary electrophoresis for the determination of parabens in personal care products.

    Science.gov (United States)

    Ma, Teng; Li, Zheng; Jia, Qiong; Zhou, Weihong

    2016-07-01

    We developed a CE and ultrasound-assisted temperature-controlled ionic liquid emulsification microextraction method for the determination of four parabens (methyl paraben, ethyl paraben, propyl paraben, and butyl paraben) in personal care products including mouthwash and toning lotion. In the proposed extraction procedure, ionic liquid (IL, 1-octyl-3-methylimidazolium hexafluorophosphate) was used as extraction solvent, moreover, no disperser solvent was needed. Parameters affecting the extraction efficiency including volume of IL, heating temperature, ultrasonic time, extraction time, sample pH, ionic strength, and centrifugation time were optimized. Under the optimized conditions, the method was found to be linear over the range of 3-500 ng/mL with coefficient of determination (R(2) ) in the range of 0.9990-0.9998. The LODs and LOQs for the four parabens were 0.45-0.72 ng/mL and 1.50-2.40 ng/mL, respectively. Intraday and interday precisions (RSDs, n = 5) were in the range of 5.4-6.8% and 7.0-8.7%, respectively. The recoveries of parabens at different spiked levels ranged from 71.9 to 119.2% with RSDs less than 9.5%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Ionic Liquid-Based Ultrasonic/Microwave-Assisted Extraction of ...

    African Journals Online (AJOL)

    Conclusion: Compared with traditional methods, IL-UMAE method uses Ionic liquid-solvent which greatly shortens the extraction time. IL-UMAE as a simple, effective and environmentally friendly approach shows a broad prospect for active ingredient extraction. Keywords: Dioscorea zingiberensis Steroidal saponins, Ionic ...

  14. Determination of antimony and tin in beverages using inductively coupled plasma-optical emission spectrometry after ultrasound-assisted ionic liquid dispersive liquid-liquid phase microextraction.

    Science.gov (United States)

    Biata, N Raphael; Nyaba, Luthando; Ramontja, James; Mketo, Nomvano; Nomngongo, Philiswa N

    2017-12-15

    The aim of this study was to develop a simple and fast ultrasound-assisted ionic liquid dispersive liquid-liquid phase microextraction (UA-IL-DLLME) method for preconcetration of trace antimony and tin in beverage samples. The novelty of this study was based on the application of ligandless UA-IL-DLLME using low-density ionic liquid and organic solvents for preconcentration of Sb and Sn. The concentration of Sb and Sn were quantified using ICP-OES. Under the optimum conditions, the calibration graph was found to be LOQ-250µgL -1 (r 2 =0.9987) for Sb and LOQ-350µgL -1 for Sn. The LOD and LOQ of Sb and Sn ranged from 1.2to 2.5ngL -1 and 4.0 to 8.3ngL -1 , respectively, with high preconcentration factors. The precisions (%RSD) of the proposed method ranged from 2.1% to 2.5% and 3.9% to 4.7% for Sb and Sn, respectively. The proposed method was successfully applied for determination of Sb and Sn in beverages. Copyright © 2017 Elsevier Ltd. All rights reserved.

  15. Ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometric for selenium speciation in foods and beverages.

    Science.gov (United States)

    Tuzen, Mustafa; Pekiner, Ozlem Zeynep

    2015-12-01

    A rapid and environmentally friendly ultrasound assisted ionic liquid dispersive liquid liquid microextraction (USA-IL-DLLME) was developed for the speciation of inorganic selenium in beverages and total selenium in food samples by using graphite furnace atomic absorption spectrometry. Some analytical parameters including pH, amount of complexing agent, extraction time, volume of ionic liquid, sample volume, etc. were optimized. Matrix effects were also investigated. Enhancement factor (EF) and limit of detection (LOD) for Se(IV) were found to be 150 and 12 ng L(-1), respectively. The relative standard deviation (RSD) was found 4.2%. The accuracy of the method was confirmed with analysis of LGC 6010 Hard drinking water and NIST SRM 1573a Tomato leaves standard reference materials. Optimized method was applied to ice tea, soda and mineral water for the speciation of Se(IV) and Se(VI) and some food samples including beer, cow's milk, red wine, mixed fruit juice, date, apple, orange, grapefruit, egg and honey for the determination of total selenium. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Ionic Liquid-Based Optical and Electrochemical Carbon Dioxide Sensors

    Science.gov (United States)

    Behera, Kamalakanta; Pandey, Shubha; Kadyan, Anu; Pandey, Siddharth

    2015-01-01

    Due to their unusual physicochemical properties (e.g., high thermal stability, low volatility, high intrinsic conductivity, wide electrochemical windows and good solvating ability), ionic liquids have shown immense application potential in many research areas. Applications of ionic liquid in developing various sensors, especially for the sensing of biomolecules, such as nucleic acids, proteins and enzymes, gas sensing and sensing of various important ions, among other chemosensing platforms, are currently being explored by researchers worldwide. The use of ionic liquids for the detection of carbon dioxide (CO2) gas is currently a major topic of research due to the associated importance of this gas with daily human life. This review focuses on the application of ionic liquids in optical and electrochemical CO2 sensors. The design, mechanism, sensitivity and detection limit of each type of sensor are highlighted in this review. PMID:26690155

  17. Ionic Liquid-Based Optical and Electrochemical Carbon Dioxide Sensors

    Directory of Open Access Journals (Sweden)

    Kamalakanta Behera

    2015-12-01

    Full Text Available Due to their unusual physicochemical properties (e.g., high thermal stability, low volatility, high intrinsic conductivity, wide electrochemical windows and good solvating ability, ionic liquids have shown immense application potential in many research areas. Applications of ionic liquid in developing various sensors, especially for the sensing of biomolecules, such as nucleic acids, proteins and enzymes, gas sensing and sensing of various important ions, among other chemosensing platforms, are currently being explored by researchers worldwide. The use of ionic liquids for the detection of carbon dioxide (CO2 gas is currently a major topic of research due to the associated importance of this gas with daily human life. This review focuses on the application of ionic liquids in optical and electrochemical CO2 sensors. The design, mechanism, sensitivity and detection limit of each type of sensor are highlighted in this review.

  18. Ionic-Liquid Based Separation of Azeotropic Mixtures

    DEFF Research Database (Denmark)

    Kulajanpeng, Kusuma; Suriyapraphadilok, Uthaiporn; Gani, Rafiqul

    2014-01-01

    [C1MIM][DMP]. For the final evaluation, the best candidates for aqueous systems were used as entrainers, and then the vapor-liquid equilibrium (VLE) of the ternary systems containing ILs was predicted by the Non Random Two Liquids (NRTL) model to confirm the breaking of the azeotrope. Based......methodology for the screening of ionic liquids (ILs) as entrainers for ILs-based separation processes in binary aqueous azeotropic systems (e.g., water + ethanol and water + isopropanol) is presented. Ionic liquids as entrainers were first screened based on a combination of criteria...... step. The best candidates for aqueous systems were selected for final evaluation as follows: 1-ethyl-3-methylimidazolium ethylsulfate [C2MIM][EtSO4], 1-ethyl-3-methylimidazolium acetate [C2MIM][Ac], 1-ethyl-3-methylimidazolium dicyanamide [C2MIM][N(CN)2], and 1,3-dimethylimidazolium dimethyl phosphate...

  19. Selective determination of inorganic cobalt in nutritional supplements by ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Berton, Paula; Martinis, Estefania M. [Analytical Chemistry Research and Development Group (QUIANID), (LISAMEN-CCT-CONICET-Mendoza), Av. Ruiz Leal S/N Parque General San Martin, M 5502 IRA Mendoza (Argentina); Martinez, Luis D. [INQUISAL-CONICET, Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, San Luis (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar [Analytical Chemistry Research and Development Group (QUIANID), (LISAMEN-CCT-CONICET-Mendoza), Av. Ruiz Leal S/N Parque General San Martin, M 5502 IRA Mendoza (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)

    2012-02-03

    Highlights: Black-Right-Pointing-Pointer Synergy of ultrasound energy and TILDLME technique for improved metal extraction. Black-Right-Pointing-Pointer Highly selective determination of inorganic Co species at trace levels. Black-Right-Pointing-Pointer Speciation analysis of Co in several nutritional supplements with highly complex matrices. Black-Right-Pointing-Pointer Development of an environmentally friendly microextraction technique with minimal waste production and sample consumption. - Abstract: In the present work, a simple and rapid analytical method based on application of ionic liquids (ILs) for inorganic Co(II) species (iCo) microextraction in a variety of nutrient supplements was developed. Inorganic Co was initially chelated with 1-nitroso-2-naphtol (1N2N) reagent followed by a modern technique named ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction (USA-TILDLME). The extraction was performed with 1-hexyl-3-methylimidazolium hexafluorophosphate [C{sub 6}mim][PF{sub 6}] with the aid of ultrasound to improve iCo recovery. Finally, the iCo-enriched IL phase was solubilized in methanol and directly injected into an electrothermal atomic absorption spectrometer (ETAAS). Several parameters that could influence iCo microextraction and detection were carefully studied. Since the main difficulty in these samples is caused by high concentrations of potential interfering ions, different approaches were evaluated to eliminate interferences. The limit of detection (LOD) was 5.4 ng L{sup -1}, while the relative standard deviation (RSD) was 4.7% (at 0.5 {mu}g L{sup -1} Co level and n = 10), calculated from the peak height of absorbance signals. Selective microextraction of iCo species was achieved only by controlling the pH value during the procedure. The method was thus successfully applied for determination of iCo species in nutritional supplements.

  20. Ionic liquid-based green processes for energy production.

    Science.gov (United States)

    Zhang, Suojiang; Sun, Jian; Zhang, Xiaochun; Xin, Jiayu; Miao, Qingqing; Wang, Jianji

    2014-11-21

    To mitigate the growing pressure on resource depletion and environment degradation, the development of green processes for the production of renewable energy is highly required. As a class of novel and promising media, ionic liquids (ILs) have shown infusive potential applications in energy production. Aiming to offer a critical overview regarding the new challenges and opportunities of ILs for developing green processes of renewable energy, this article emphasises the role of ILs as catalysts, solvents, or electrolytes in three broadly interesting energy production processes from renewable resources, such as CO2 conversion to fuels and fuel additives, biomass pretreatment and conversion to biofuels, as well as solar energy and energy storage. It is expected that this article will stimulate a generation of new ideas and new technologies in IL-based renewable energy production.

  1. Ionic Liquid based polymer electrolytes for electrochemical sensors

    Directory of Open Access Journals (Sweden)

    Jakub Altšmíd

    2015-09-01

    Full Text Available Amperometric NO2 printed sensor with a new type of solid polymer electrolyte and a carbon working electrode has been developed. The electrolytes based on 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonylimide [EMIM][N(Tf2], 1-butyl-3-methylimidazolium trifluoromethanesulfonate [BMIM][CF3SO3] and 1-ethyl-3-methylimidazolium tetrafluoroborate [EMIM][BF4] ionic liquids were immobilized in poly(vinylidene fluoride matrix [PVDF]. The analyte, gaseous nitrogen dioxide, was detected by reduction at -500 mV vs. platinum pseudoreference electrode. The sensors showed a linear behavior in the whole tested range, i.e., 0 - 5 ppm and their sensitivities were in order of 0.3 x∙10-6 A/ppm. The sensor sensitivity was influenced by the electric conductivity of printing formulation; the higher the conductivity, the higher the sensor sensitivity. The rise/recovery times were in order of tens of seconds. The use of  screen printing technology and platinum pseudoreference electrode simplify the sensor fabrication and it does not have any negative effect on the sensor stability.DOI: http://dx.doi.org/10.5755/j01.ms.21.3.7371

  2. 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.

  3. Peculiar surface behavior of some ionic liquids based on active pharmaceutical ingredients.

    Science.gov (United States)

    Restolho, José; Mata, José Luis; Saramago, Benilde

    2011-02-21

    The ionic liquids based on biologically active cations and anions, commonly designated by ionic liquids based on active pharmaceutical ingredients (ILs-APIs), are interesting compounds for use in pharmaceutical applications. Lidocaine docusate, ranitidine docusate, and didecyldimethylammonium ibuprofen are examples of promising ILs-APIs that were recently synthesized. They were submitted to biological testing and calorimetric measurements, but nothing is known about their surface properties. In this work, we measured the surface tension and the contact angles on both hydrophilic and hydrophobic surfaces in a temperature range as wide as possible. Based on the wettability data, the polarity fractions were estimated using the Fowkes theory. The peculiar surface behavior observed was tentatively attributed to the presence of mesophases.

  4. Peculiar surface behavior of some ionic liquids based on active pharmaceutical ingredients

    Science.gov (United States)

    Restolho, José; Mata, José Luis; Saramago, Benilde

    2011-02-01

    The ionic liquids based on biologically active cations and anions, commonly designated by ionic liquids based on active pharmaceutical ingredients (ILs-APIs), are interesting compounds for use in pharmaceutical applications. Lidocaine docusate, ranitidine docusate, and didecyldimethylammonium ibuprofen are examples of promising ILs-APIs that were recently synthesized. They were submitted to biological testing and calorimetric measurements, but nothing is known about their surface properties. In this work, we measured the surface tension and the contact angles on both hydrophilic and hydrophobic surfaces in a temperature range as wide as possible. Based on the wettability data, the polarity fractions were estimated using the Fowkes theory. The peculiar surface behavior observed was tentatively attributed to the presence of mesophases.

  5. 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.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

    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.

  7. Ionic liquids-lithium salts pretreatment followed by ultrasound-assisted extraction of vitexin-4″-O-glucoside, vitexin-2″-O-rhamnoside and vitexin from Phyllostachys edulis leaves.

    Science.gov (United States)

    Hou, Kexin; Chen, Fengli; Zu, Yuangang; Yang, Lei

    2016-01-29

    An efficient method for the extraction of vitexin, vitexin-4″-O-glucoside, and vitexin-2″-O-rhamnoside from Phyllostachys edulis leaves comprises heat treatment using an ionic liquid-lithium salt mixture (using 1-butyl-3-methylimidazolium bromide as the solvent and lithium chloride as the additive), followed by ultrasound-assisted extraction. To obtain higher extraction yields, the effects of the relevant experimental parameters (including heat treatment temperature and time, relative amounts of 1-butyl-3-methylimidazolium bromide and lithium chloride, power and time of the ultrasound irradiation, and the liquid-solid ratio) are evaluated and response surface methodology is used to optimize the significant factors. The morphologies of the treated and untreated P. edulis leaves are studied by scanning electron microscopy. The improved extraction method proposed provides high extraction yield, good repeatability and precision, and has wide potential applications in the analysis of plant samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Determination of heat capacity of ionic liquid based nanofluids using group method of data handling technique

    Science.gov (United States)

    Sadi, Maryam

    2018-01-01

    In this study a group method of data handling model has been successfully developed to predict heat capacity of ionic liquid based nanofluids by considering reduced temperature, acentric factor and molecular weight of ionic liquids, and nanoparticle concentration as input parameters. In order to accomplish modeling, 528 experimental data points extracted from the literature have been divided into training and testing subsets. The training set has been used to predict model coefficients and the testing set has been applied for model validation. The ability and accuracy of developed model, has been evaluated by comparison of model predictions with experimental values using different statistical parameters such as coefficient of determination, mean square error and mean absolute percentage error. The mean absolute percentage error of developed model for training and testing sets are 1.38% and 1.66%, respectively, which indicate excellent agreement between model predictions and experimental data. Also, the results estimated by the developed GMDH model exhibit a higher accuracy when compared to the available theoretical correlations.

  9. Ionic Liquid-Based Liquid-Liquid Microextraction for Benzodiazepine Analysis in Postmortem Blood Samples.

    Science.gov (United States)

    De Boeck, Marieke; Dehaen, Wim; Tytgat, Jan; Cuypers, Eva

    2018-03-24

    Sample preparation is rapidly improving to fulfill the need for faster and more environmentally friendly alternatives. In this respect, ionic liquid-based dispersive liquid-liquid microextraction (IL-DLLME) is an interesting technique. However, it has not yet been evaluated for the analysis of postmortem samples, which are frequently analyzed in forensic toxicology. This study investigates the applicability of IL-DLLME coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS), for the analysis of benzodiazepines in postmortem blood of 11 forensic cases. The method was compared with a validated solid-phase extraction (SPE) method. Bland-Altman analysis was performed on 24 benzodiazepine measurements. Both methods gave comparable results, except for flurazepam and temazepam (>55% difference). A feasible explanation is high postmortem matrix variability that was not considered during IL-DLLME validation experiments. Another issue could be the use of a single nondeuterated SPE internal standard. Overall, IL-DLLME has proven its usability for the analysis of postmortem blood. © 2018 American Academy of Forensic Sciences.

  10. 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.

  11. Self-Supporting, Hydrophobic, Ionic Liquid-Based Reference Electrodes Prepared by Polymerization-Induced Microphase Separation.

    Science.gov (United States)

    Chopade, Sujay A; Anderson, Evan L; Schmidt, Peter W; Lodge, Timothy P; Hillmyer, Marc A; Bühlmann, Philippe

    2017-10-27

    Interfaces of ionic liquids and aqueous solutions exhibit stable electrical potentials over a wide range of aqueous electrolyte concentrations. This makes ionic liquids suitable as bridge materials that separate in electroanalytical measurements the reference electrode from samples with low and/or unknown ionic strengths. However, methods for the preparation of ionic liquid-based reference electrodes have not been explored widely. We have designed a convenient and reliable synthesis of ionic liquid-based reference electrodes by polymerization-induced microphase separation. This technique allows for a facile, single-pot synthesis of ready-to-use reference electrodes that incorporate ion conducting nanochannels filled with either 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide or 1-dodecyl-3-methylimidazolium bis(trifluoromethyl sulfonyl)imide as ionic liquid, supported by a mechanically robust cross-linked polystyrene phase. This synthesis procedure allows for the straightforward design of various reference electrode geometries. These reference electrodes exhibit a low resistance as well as good reference potential stability and reproducibility when immersed into aqueous solutions varying from deionized, purified water to 100 mM KCl, while requiring no correction for liquid junction potentials.

  12. Self-Supporting, Hydrophobic, Ionic Liquid-Based Reference Electrodes Prepared by Polymerization-Induced Microphase Separation

    Energy Technology Data Exchange (ETDEWEB)

    Chopade, Sujay A.; Anderson, Evan L.; Schmidt, Peter W.; Lodge, Timothy P.; Hillmyer, Marc A.; Bühlmann, Philippe (UMM)

    2017-09-25

    Interfaces of ionic liquids and aqueous solutions exhibit stable electrical potentials over a wide range of aqueous electrolyte concentrations. This makes ionic liquids suitable as bridge materials that separate in electroanalytical measurements the reference electrode from samples with low and/or unknown ionic strengths. However, methods for the preparation of ionic liquid-based reference electrodes have not been explored widely. We have designed a convenient and reliable synthesis of ionic liquid-based reference electrodes by polymerization-induced microphase separation. This technique allows for a facile, single-pot synthesis of ready-to-use reference electrodes that incorporate ion conducting nanochannels filled with either 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide or 1-dodecyl-3-methylimidazolium bis(trifluoromethyl sulfonyl)imide as ionic liquid, supported by a mechanically robust cross-linked polystyrene phase. This synthesis procedure allows for the straightforward design of various reference electrode geometries. These reference electrodes exhibit a low resistance as well as good reference potential stability and reproducibility when immersed into aqueous solutions varying from deionized, purified water to 100 mM KCl, while requiring no correction for liquid junction potentials.

  13. Ionic liquid ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of the aqueous phase for preconcentration of heavy metals ions prior to determination by LC-UV.

    Science.gov (United States)

    Werner, Justyna

    2018-05-15

    Ionic liquid ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of the aqueous phase was used for preconcentration of Ni 2+ , Co 2+ , Cd 2+ , Cu 2+ , Pb 2+ in natural water samples prior to liquid chromatography with UV detection. In the proposed method, the ammonium pyrrolidinedithiocarbamate was used as a complexing agent and the phosphonium ionic liquid trihexyl(tetradecyl)phosphonium bis[(2,4,4-trimethyl)pentyl]phosphinate (Cyphos IL 104) was used as an extractant. Ultrasound energy was used to disperse the extractant in the aqueous phase. After microextraction, the ionic liquid and aqueous phases were separated by centrifugation. Then the aqueous phase was frozen and the lighter than water ionic liquid phase containing metal ions complexes with pyrrolidinedithiocarbamate was separated and dissolved in a small volume of methanol prior to injection into the liquid chromatograph. Several parameters including the volume of extractant, the pH of the sample, the concentration of complexing agent, the time of ultrasound energy treatment, the time and speed of centrifugation and the effect of ionic strength were optimized. Under the optimized conditions (10 µL of Cyphos IL 104, pH = 5, 0.3% w/v ammonium pyrrolidinedithiocarbamate, 60 s of ultrasound use, 5 min/5000 rpm (2516×g) of centrifugation, 2.0 mg of NaCl), preconcentration factors were 211, 210, 209, 207 and 211 for Ni 2+ , Co 2+ , Cd 2+ , Cu 2+ and Pb 2+ respectively. Linearity was observed in the ranges 0.2-75.0 µg L -1 for Pb 2+ , Cd 2+ , Co 2+ and 0.5-100.0 µg L -1 for Cu 2+ , Ni 2+ . The limits of detection were 0.03 µg L -1 for Ni 2+ , 0.03 µg L -1 for Co 2+ , 0.03 µg L -1 for Cd 2+ , 0.02 µg L -1 for Cu 2+ , 0.02 µg L -1 for Pb 2+ , respectively. The accuracy of this method was evaluated by preconcentration and determination of Ni 2+ , Co 2+ , Cd 2+ , Cu 2+ , Pb 2+ in certified reference materials (TMRAIN-04 and NIST 1643e

  14. Identification of degradation products of ionic liquids in an ultrasound assisted zero-valent iron activated carbon micro-electrolysis system and their degradation mechanism.

    Science.gov (United States)

    Zhou, Haimei; Lv, Ping; Shen, Yuanyuan; Wang, Jianji; Fan, Jing

    2013-06-15

    Ionic liquids (ILs) have potential applications in many areas of chemical industry because of their unique properties. However, it has been shown that the ILs commonly used to date are toxic and not biodegradable in nature, thus development of efficient chemical methods for the degradation of ILs is imperative. In this work, degradation of imidazolium, piperidinium, pyrrolidinium and morpholinium based ILs in an ultrasound and zero-valent iron activated carbon (ZVI/AC) micro-electrolysis system was investigated, and some intermediates generated during the degradation were identified. It was found that more than 90% of 1-alkyl-3-methylimidazolium bromide ([Cnmim]Br, n = 2, 4, 6, 8, 10) could be degraded within 110 min, and three intermediates 1-alkyl-3-methyl-2,4,5-trioxoimidazolidine, 1-alkyl-3-methylurea and N-alkylformamide were detected. On the other hand, 1-butyl-1-methylpiperidinium bromide ([C4mpip]Br), 1-butyl-1-methylpyrrolidinium bromide ([C4mpyr]Br) and N-butyl-N-methylmorpholinium bromide ([C4mmor]Br) were also effectively degraded through the sequential oxidization into hydroxyl, carbonyl and carboxyl groups in different positions of the butyl side chain, and then the N-butyl side chain was broken to form the final products of N-methylpiperidinium, N-methylpyrrolidinium and N-methylmorpholinium, respectively. Based on these intermediate products, degradation pathways of these ILs were suggested. These findings may provide fundamental information on the assessment of the factors related to the environmental fate and environmental behavior of these commonly used ILs. Copyright © 2013 Elsevier Ltd. All rights reserved.

  15. Ionic liquid-based hydrothermal synthesis of Lu2O3 and Lu2O3:Eu3+ microcrysals

    Science.gov (United States)

    Li, Yinyan; Xu, Shiqing

    2016-09-01

    Uniform and well-defined Lu2O3 and Lu2O3:Eu3+ microarchitectures have been successfully synthesized via a green and facile ionic liquid-based hydrothermal method followed by a subsequent calcination process. Novel 3D micro-rodbundles and 1D microrods of Lu2O3 and Lu2O3:Eu3+ were controllably obtained through this method. X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy and photoluminescence spectra were used to characterize the micromaterials. The proposed formation mechanisms have been investigated on the basis of a series of SEM studies of the products obtained at different hydrothermal durations. The results indicated that hydrothermal temperature and the ionic liquid-tetrabutylammonium hydroxide were two key factors for the formation as well as the morphology control of the Lu2O3 and Lu2O3:Eu3+ microarchitectures.

  16. Determination of fluoroquinolone antibiotics via ionic-liquid-based, salt-induced, dual microextraction in swine feed.

    Science.gov (United States)

    Wang, Huili; Gao, Ming; Gao, Jiajia; Yu, Nana; Huang, Hong; Yu, Qing; Wang, Xuedong

    2016-09-01

    In conventional microextraction procedures, the disperser (organic solvent or ionic liquid) is left in the aqueous phase and discarded after finishing the microextraction process. Because the disperser is water-soluble, it results in low extraction recovery for polar compounds. In this investigation, an ionic-liquid-based microextraction (ILBME) was integrated with salting-out assisted liquid-liquid microextraction (SALLME) to build an ionic-liquid-based, salt-induced, dual microextraction (ILSDME) for isolation of five fluoroquinolone antibiotics (FQs) with high polarity (log P, -1.0 to 1.0). The proposed ILSDME method incorporates a dual microextraction by converting the disperser in the ILBME to the extractor in the SALLME. Optimization of key factors was conducted by integrating single-factor experiments and central composite design. The optimized experimental parameters were 80 μL [C8MIM][PF6] as extractor, 505 μL acetone as disperser, pH = 2.0, 4.1 min extraction time, and 4.2 g of Na2SO4. Under optimized conditions, high ERs (90.6-103.2 %) and low LODs (0.07-0.61 μg kg(-1)) were determined for five FQs in swine feed. Experimental precision based on RSDs was 1.4-5.2 % for intra-day and 2.4-6.9 % for inter-day analyses. The combination of ILBME with SALLME increased FQ recoveries by 15-20 % as compared with SALLME, demonstrating that the ILSDME method can enhance extraction efficiency for polar compounds compared to single-step microextraction. Therefore, the ILSDME method developed in this study has wide application for pretreatment of moderately to highly polar pollutants in complex matrices. Graphical Abstract A dual microextraction was developed by integrating ionic-liquid-based microextraction with salting-out assisted liquid-liquid microextraction for isolation of five fluoroquinolone antibiotics (FQs) with high polarity (log P = -1.0 to 1.0). The principle of dual microextraction is based on converting the remaining disperser from

  17. Toxicity prediction of ionic liquids based on Daphnia magna by using density functional theory

    Science.gov (United States)

    Nu’aim, M. N.; Bustam, M. A.

    2018-04-01

    By using a model called density functional theory, the toxicity of ionic liquids can be predicted and forecast. It is a theory that allowing the researcher to have a substantial tool for computation of the quantum state of atoms, molecules and solids, and molecular dynamics which also known as computer simulation method. It can be done by using structural feature based quantum chemical reactivity descriptor. The identification of ionic liquids and its Log[EC50] data are from literature data that available in Ismail Hossain thesis entitled “Synthesis, Characterization and Quantitative Structure Toxicity Relationship of Imidazolium, Pyridinium and Ammonium Based Ionic Liquids”. Each cation and anion of the ionic liquids were optimized and calculated. The geometry optimization and calculation from the software, produce the value of highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO). From the value of HOMO and LUMO, the value for other toxicity descriptors were obtained according to their formulas. The toxicity descriptor that involves are electrophilicity index, HOMO, LUMO, energy gap, chemical potential, hardness and electronegativity. The interrelation between the descriptors are being determined by using a multiple linear regression (MLR). From this MLR, all descriptors being analyzed and the descriptors that are significant were chosen. In order to develop the finest model equation for toxicity prediction of ionic liquids, the selected descriptors that are significant were used. The validation of model equation was performed with the Log[EC50] data from the literature and the final model equation was developed. A bigger range of ionic liquids which nearly 108 of ionic liquids can be predicted from this model equation.

  18. Systematic screening methodology and energy efficient design of ionic liquid-based separation processes

    DEFF Research Database (Denmark)

    Kulajanpeng, Kusuma; Suriyapraphadilok, Uthaiporn; Gani, Rafiqul

    2016-01-01

    A systematic methodology for the screening of ionic liquids (ILs) as entrainers and for the design of ILs-based separation processes in various homogeneous binary azeotropic mixtures has been developed. The methodology focuses on the homogeneous binary aqueous azeotropic systems (for example, water...... based on a combination of criteria such as stability, toxicity, and their environmental impacts. All best ILs were used as entrainers, and an extractive distillation column (EDC) and ionic liquid recovery column were designed and simulated with a process simulator to determine the overall energy...

  19. Factors affecting the stability and performance of ionic liquid-based planar transient photodetectors.

    Science.gov (United States)

    Dalgleish, Simon; Reissig, Louisa; Hu, Laigui; Matsushita, Michio M; Sudo, Yuki; Awaga, Kunio

    2015-05-12

    A novel planar architecture has been developed for the study of photodetectors utilizing the transient photocurrent response induced by a metal/insulator/semiconductor/metal (MISM) structured device, where the insulator is an ionic liquid (IL-MISM). Using vanadyl 2,3-naphthalocyanine, which absorbs in the communications-relevant near-infrared wavelength region (λ(max,film) ≈ 850 nm), in conjunction with C60 as a bulk heterojunction, the high capacitance of the formed electric double layers at the ionic liquid interfaces yields high charge separation efficiency within the semiconductor layer, and the minimal potential drop in the bulk ionic liquid allows the electrodes to be offset by distances of over 7 mm. Furthermore, the decrease in operational speed with increased electrode separation is beneficial for a clear modeling of the waveform of the photocurrent signal, free from the influence of measurement circuitry. Despite the use of a molecular semiconductor as the active layer in conjunction with a liquid insulating layer, devices with a stability of several days could be achieved, and the operational stability of such devices was shown to be dependent solely on the solubility of the active layer in the ionic liquid, even under atmospheric conditions. Furthermore, the greatly simplified device construction process, which does not rely on transparent electrode materials or direct electrode deposition, provides a highly reproducible platform for the study of the electronic processes within IL-MISM detectors that is largely free from architectural constraints.

  20. Hydrophobic ionic liquids based on the 1-butyl-3-methylimidazolium cation for lithium/seawater batteries

    Science.gov (United States)

    Zhang, Yancheng; Urquidi-Macdonald, Mirna

    Two hydrophobic ionic liquids (room temperature molten salts) based on 1-butyl-3-methylimidazolium cation (BMI +), BMI +PF 6- and BMI +Tf 2N -, were used in developing a highly efficient lithium anode system for lithium/seawater batteries. The lithium anode system was composed of lithium metal/ionic liquid/Celgard membrane. Both BMI +PF 6-and BMI +Tf 2N - maintained high apparent anodic efficiency (up to 100%) under potentiostatic polarization (at +0.5 V versus open-circuit potential (OCP)) in a 3% NaCl solution. Eventually, traces of water contaminated the ionic liquid and a bilayer film (LiH and LiOH) on the lithium surface was formed, decreasing the rate of lithium anodic reaction and hence the discharge current density. BMI +Tf 2N - prevented traces of water from reaching the lithium metal surface longer than BMI +PF 6- (60 h versus 7 h). However, BMI +PF 6- was better than BMI +Tf 2N - in keeping a constant current density (˜0.2 mA cm -2) before the traces of water contaminated the lithium surface due to the non-reactivity of BMI +PF 6- with the lithium metal that kept the bare lithium surface. During the discharge process, BMI +PF 6- and BMI +Tf 2N - acted as ion transport media of Li +, Cl -, OH - and H 2O, but did not react with them because of the excellent chemical stability, high conductivity, and high hydrophobicity of these two ionic liquids. Both BMI +PF 6- and BMI +Tf 2N - gels were tentative approaches used to delay the traces of water coming in contact with the lithium surface.

  1. Polymeric ionic liquid based on magnetic materials fabricated through layer-by-layer assembly as adsorbents for extraction of pesticides.

    Science.gov (United States)

    He, Lijun; Cui, Wenhang; Wang, Yali; Zhao, Wenjie; Xiang, Guoqiang; Jiang, Xiuming; Mao, Pu; He, Juan; Zhang, Shusheng

    2017-11-03

    In this study, layer-by-layer assembly of polyelectrolyte multilayer films on magnetic silica provided a convenient and controllable way to prepare polymeric ionic liquid-based magnetic adsorbents. The resulting particles were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, and magnetic measurements. The data showed that the magnetic particles had more homogeneous spherical shapes with higher saturation magnetization when compared to those obtained by free radical polymerization method. This facilitated the convenient collection of magnetic particles, with higher extraction repeatability. The extraction performance of the multilayer polymeric ionic liquid-based adsorbents was evaluated by magnetic solid-phase extraction of four pesticides including quinalphos, fenthion, phoxim, and chlorpropham. The data suggested that the extraction efficiency depended on the number of layers in the film. The parameters affecting the extraction efficiency were optimized, and good linearity ranging from 2 to 250μgL -1 was obtained with correlation coefficients of 0.9994-0.9998. Moreover, the proposed method presented low limit of detection (0.5μgL -1 , S/N=3) and limit of quantification (1.5μgL -1 , S/N=10), and good repeatability expressed by the relative standard deviation (2.0%-4.6%, n=5). The extraction recoveries of four pesticides were found to range from 58.9% to 85.8%. The reliability of the proposed method was demonstrated by analyzing environmental water samples, and the results revealed satisfactory spiked recovery, relative standard deviation, and selectivity. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Fabrication of an ionic-liquid-based polymer monolithic column and its application in the fractionation of proteins from complex biosamples.

    Science.gov (United States)

    Zhang, Doudou; Zhang, Qian; Bai, Ligai; Han, Dandan; Liu, Haiyan; Yan, Hongyuan

    2018-01-24

    An ionic-liquid-based polymer monolithic column was synthesized by free radical polymerization within the confines of a stainless-steel column (50 mm × 4.6 mm id). In the processes, ionic liquid and stearyl methacrylate were used as dual monomers, ethylene glycol dimethacrylate as the cross-linking agent, and polyethylene glycol 200 and isopropanol as co-porogens. Effects of the prepolymerization solution components on the properties of the resulting monoliths were studied in detail. Scanning electron microscopy, nitrogen adsorption-desorption measurements, and mercury intrusion porosimetry were used to investigate the morphology and pore size distribution of the prepared monoliths, which showed that the homemade ionic-liquid-based monolith column possessed a relatively uniform macropore structure with a total macropore specific surface area of 44.72 m 2 /g. Compared to a non-ionic-liquid-based monolith prepared under the same conditions, the ionic-liquid-based monolith exhibited excellent selectivity and high performance for separating proteins from complex biosamples, such as egg white, snailase, bovine serum albumin digest solution, human plasma, etc., indicating promising applications in the fractionation and analysis of proteins from the complex biosamples in proteomics research. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Instability of Ionic Liquid-Based Electrolytes in Li−O2 Batteries

    DEFF Research Database (Denmark)

    Das, Supti; Højberg, Jonathan; Knudsen, Kristian Bastholm

    2015-01-01

    of the rechargeability (OER/ORR), and thereby the Coulombic efficiency of discharge and charge. None of the IL-based electrolytes are found to behave as needed for a functional Li−O2 battery but perform better than commonly used organic solvents. Also the extent of rechargeability/reversibility has been found......Ionic liquids (ILs) have been proposed as promising solvents for Li−air battery electrolytes. Here, several ILs have been investigated using differential electrochemical mass spectrometry (DEMS) to investigate the electrochemical stability in a Li−O2 system, by means of quantitative determination...

  4. Phenyl and ionic liquid based bifunctional periodic mesoporous organosilica supported copper: An efficient nanocatalyst for clean production of polyhydroquinolines.

    Science.gov (United States)

    Elhamifar, Dawood; Ardeshirfard, Hakimeh

    2017-11-01

    A novel phenyl and ionic liquid based bifunctional periodic mesoporous organosilica supported copper (Cu@BPMO-Ph-IL) is prepared, characterized and its catalytic application is developed in the clean production of polyhydroquinolines. The Cu@BPMO-Ph-IL was prepared via chemical grafting of ionic liquid groups onto phenyl-based PMO followed by treatment with copper acetate. This nanocatalyst was characterized with transmission electron microscopy (TEM), scanning electron microscopy (SEM), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTs), thermal gravimetric analysis (TGA), powder X-ray diffraction (PXRD), nitrogen-sorption and energy dispersive X-ray (EDX) analyses. This was successfully applied in the one-pot Hantzsch condensation of aldehydes, ammonium acetate, alkylacetoacetates and dimedone to prepare a set of different derivatives of polyhydroquinolines in high yields and selectivity. The catalyst was effectively recovered and reused several times without important decrease in efficiency. The recovered catalyst was also characterized with TEM analysis to study its stability and durability under applied conditions. Copyright © 2017 Elsevier Inc. All rights reserved.

  5. Treatment of Mineral Oil Refinery Wastewater in Microbial Fuel Cells Using Ionic Liquid Based Separators

    Directory of Open Access Journals (Sweden)

    Hasna Addi

    2018-03-01

    Full Text Available Microbial fuel cells (MFCs are an environmentally friendly technology that can recover electricity directly from several wastes at ambient temperatures. This work explores the use of mineral oil refinery wastewater as feedstock in single-chamber air-cathode MFC devices. A polymer inclusion membrane based on the ionic liquid methyltrioctylammonium chloride, [MTOA+][Cl−], at a concentration of 70% w/w, was used as separator, showing a good efficiency in power production and chemical oxygen demand (COD removal. The power and the chemical oxygen demand removal reached values of 45 mW/m3 and over 80%, respectively. The evolution of other parameters of the wastewater including nitrites, phosphates and sulphates were also studied. Kjeldahl nitrogen and sulphates were significantly reduced during MFC operation. The results show that mineral oil refinery wastewater can be used as feedstock in air breathing cathode-microbial fuel cells based on polymer ionic liquid inclusion membranes. This configuration could represent a good alternative for wastewater depuration while producing energy during the process.

  6. Scaling-up and ionic liquid-based extraction of pectinases from Aspergillus flavipes cultures.

    Science.gov (United States)

    Wolf-Márquez, Vicente E; Martínez-Trujillo, M Aurora; Aguilar Osorio, Guillermo; Patiño, Faustino; Álvarez, María S; Rodríguez, Ana; Sanromán, M Ángeles; Deive, Francisco J

    2017-02-01

    The viability of the scaling-up of pectinases production by Aspergillus flavipes at 5L-bioreactor scale has been demonstrated by keeping constant the power input, and a drastic increase in the endo- and exopectinolytic enzyme production was recorded (7- and 40-fold, respectively). The main process variables were modelled by means of logistic and Gompertz equations. In order to overcome the limitations of the conventional downstream strategies, a novel extraction strategy was proposed on the basis of the adequate salting-out potential of two biocompatible cholinium-based ionic liquids (N 1112OH Cl and N 1112OH H 2 PO 4 ) in aqueous solutions of Tergitol, reaching more than 90% of extraction. Copyright © 2016 Elsevier Ltd. All rights reserved.

  7. A New Green Ionic Liquid-Based Corrosion Inhibitor for Steel in Acidic Environments

    Directory of Open Access Journals (Sweden)

    Ayman M. Atta

    2015-06-01

    Full Text Available This work examines the use of new hydrophobic ionic liquid derivatives, namely octadecylammonium tosylate (ODA-TS and oleylammonium tosylate (OA-TS for corrosion protection of steel in 1 M hydrochloric acid solution. Their chemical structures were determined from NMR analyses. The surface activity characteristics of the prepared ODA-TS and OA-TS were evaluated from conductance, surface tension and contact angle measurements. The data indicate the presence of a double bond in the chemical structure of OA-TS modified its surface activity parameters. Potentiodynamic polarization, electrochemical impedance spectroscopy (EIS measurements, scanning electron microscope (SEM, Energy dispersive X-rays (EDX analysis and contact angle measurements were utilized to investigate the corrosion protection performance of ODA-TS and OA-TS on steel in acidic solution. The OA-TS and ODA-TS compounds showed good protection performance in acidic chloride solution due to formation of an inhibitive film on the steel surface.

  8. 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.

  9. 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).

  10. 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.

  11. Carbonaceous anodes for lithium-ion batteries in combination with protic ionic liquids-based electrolytes

    Science.gov (United States)

    Menne, Sebastian; Schroeder, Matthias; Vogl, Thomas; Balducci, Andrea

    2014-11-01

    Protic ionic liquids (PILs) have been recently proposed as a new class of electrolytes for lithium-ion batteries (LIBs). So far, PILs-based electrolytes have been used in combination with several battery materials, but never with carbonaceous anodes. Since graphite is the state-of-the-art anode in LIBs, the use of PILs-based electrolyte in combination with this material appears of particular importance. In this work we showed, for the first time, that PILs-based electrolytes can be successfully used also in combination with graphite. Even if the lithium intercalation and deintercalation process of these electrode materials occur outside the ESW of PILs, the addition of film-forming additive makes possible the formation of a stable SEI and, consequently, the use of PILs-based electrolytes. The results of this study indicate that the performance of graphite electrode in PILs-based electrolytes is comparable, and even slightly higher, than that observed in AIL-based electrolytes.

  12. Simultaneous extraction and concentration of water pollution tracers using ionic-liquid-based systems.

    Science.gov (United States)

    Dinis, Teresa B V; Passos, Helena; Lima, Diana L D; Sousa, Ana C A; Coutinho, João A P; Esteves, Valdemar I; Freire, Mara G

    2017-07-29

    Human activities are responsible for the release of innumerous substances into the aquatic environment. Some of these substances can be used as pollution tracers to identify contamination sources and to prioritize monitoring and remediation actions. Thus, their identification and quantification are of high priority. However, due to their presence in complex matrices and at significantly low concentrations, a pre-treatment/concentration step is always required. As an alternative to the currently used pre-treatment methods, mainly based on solid-phase extractions, aqueous biphasic systems (ABS) composed of ionic liquids (ILs) and K 3 C 6 H 5 O 7 are here proposed for the simultaneous extraction and concentration of mixtures of two important pollution tracers, caffeine (CAF) and carbamazepine (CBZ). An initial screening of the IL chemical structure was carried out, with extraction efficiencies of both tracers to the IL-rich phase ranging between 95 and 100%, obtained in a single-step. These systems were then optimized in order to simultaneously concentrate CAF and CBZ from water samples followed by HPLC-UV analysis, for which no interferences of the ABS phase-forming components and other interferents present in a wastewater effluent sample have been found. Based on the saturation solubility data of both pollution tracers in the IL-rich phase, the maximum estimated concentration factors of CAF and CBZ are 28595- and 8259-fold. IL-based ABS can be thus envisioned as effective pre-treatment techniques of environmentally-related aqueous samples for a more accurate monitoring of mixtures of pollution tracers. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Use of an ionic liquid-based surfactant as pseudostationary phase in the analysis of carbamates by micellar electrokinetic chromatography.

    Science.gov (United States)

    Tejada-Casado, Carmen; Moreno-González, David; García-Campaña, Ana M; del Olmo-Iruela, Monsalud

    2015-03-01

    The applicability of an ionic liquid-based cationic surfactant 1-dodecyl-3-methyl-imidazolium tetrafluoroborate (C12 MImBF4 ) as pseudostationary phase in MEKC has been evaluated for the analysis of 11 carbamate pesticides (promecarb, carbofuran, metolcarb, fenobucarb, aldicarb, propoxur, asulam, benomyl, carbendazim, ethiofencarb, isoprocarb) in juice samples. Under optimum conditions (separation buffer, 35 mM NaHCO3 and 20 mM C12 MImBF4 , pH 9.0; capillary temperature 25°C; voltage -22 kV) the analysis was carried out in less than 12 min, using hydrodynamic injection (50 mbar for 7.5 s) and detection at 200 nm. For the extraction of these CRBs from juice samples, a dispersive liquid-liquid microextraction (DLLME) procedure has been proposed, by optimization of variables affecting the efficiency of the extraction. Following this treatment, sample throughput was approximately 12 samples per hour, obtaining a preconcentration factor of 20. Matrix-matched calibration curves were established using tomato juice as representative matrix (from 5 to 250 μg/L for CBZ, BY, PX, CF, FEN, ETH, ISP, and 25-250 μg/L for ASL, ALD, PRC, MTL), obtaining quantification limits ranging from 1 to 18 μg/L and recoveries from 70 to 96%, with RSDs lower than 9%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. One-pot transformation of cellobiose to formic acid and levulinic acid over ionic-liquid-based polyoxometalate hybrids.

    Science.gov (United States)

    Li, Kaixin; Bai, Linlu; Amaniampong, Prince Nana; Jia, Xinli; Lee, Jong-Min; Yang, Yanhui

    2014-09-01

    Currently, levulinic acid (LA) and formic acid (FA) are considered as important carbohydrates for the production of value-added chemicals. Their direct production from biomass will open up a new opportunity for the transformation of biomass resource to valuable chemicals. In this study, one-pot transformation of cellobiose into LA and FA was demonstrated, using a series of multiple-functional ionic liquid-based polyoxometalate (IL-POM) hybrids as catalytic materials. These IL-POMs not only markedly promoted the production of valuable chemicals including LA, FA and monosaccharides with high selectivities, but also provided great convenience of the recovery and the reuse of the catalytic materials in an environmentally friendly manner. Cellobiose conversion of 100%, LA selectivity of 46.3%, and FA selectivity of 26.1% were obtained at 423 K and 3 MPa for 3 h in presence of oxygen. A detailed catalytic mechanism for the one-pot transformation of cellobiose was also presented. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Ultra-Trace Determination of Copper and Silver in Environmental Samples by Using Ionic Liquid-Based Single Drop Microextraction-Electrothermal Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    J. Abolhasani

    2013-11-01

    Full Text Available A sensitive, selective and effective ionic liquid-based single drop microextraction technique wasdeveloped by using ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate, C6MIMPF6, coupledwith electrothermal atomic absorption spectrometry (ETAAS for the determination of copper and silver inenvironmental samples. Dithizone was used as chelating agent. Several factors that influence themicroextraction efficiency and ETAAS signal, such as pH, dithizone concentration, extraction time, amounts ofionic liquid, stirring rate, pyrolysis and atomization temperature were investigated and the microextractionconditions were established. In the optimum experimental conditions, the detection limits (3 s of the methodwere 4 and 8 ng L-1 and corresponding relative standard deviations (0.1 μg L-1, n = 6 were 4.2% and 4.8% forAg and Cu, respectively. The developed method was validated by analysis of a certified reference material andapplied to the determination of silver and copper.

  16. Np(IV) complex with task-specific ionic liquid based on CMPO: first cyclic voltammetric study

    NARCIS (Netherlands)

    Sengupta, A; Murali, M.S.; Mohapatra, P.K.; Iqbal, M.; Huskens, Jurriaan; Verboom, Willem

    2015-01-01

    A cyclic voltammetric study on Np(IV) complexes with task-specific ionic liquid with 3-dodecylimidazolium cation appended with diphenylcarbamoylmethylphosphine oxide and bis(trifluoromethyl-sulfonyl)-imide anion dissolved in the room temperature ionic liquid 1-butyl-3-methylimidazolium

  17. Development of an ionic-liquid-based dispersive liquid-liquid microextraction method for the determination of antichagasic drugs in human breast milk: Optimization by central composite design.

    Science.gov (United States)

    Padró, Juan M; Pellegrino Vidal, Rocío B; Echevarria, Romina N; Califano, Alicia N; Reta, Mario R

    2015-05-01

    Chagas disease constitutes a major public health problem in Latin America. Human breast milk is a biological sample of great importance for the analysis of therapeutic drugs, as unwanted exposure through breast milk could result in pharmacological effects in the nursing infant. Thus, the goal of breast milk drug analysis is to inquire to which extent a neonate may be exposed to a drug during lactation. In this work, we developed an analytical technique to quantify benznidazole and nifurtimox (the two antichagasic drugs currently available for medical treatment) in human breast milk, with a simple sample pretreatment followed by an ionic-liquid-based dispersive liquid-liquid microextraction combined with high-performance liquid chromatography and UV detection. For this technique, the ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate has been used as the "extraction solvent." A central composite design was used to find the optimum values for the significant variables affecting the extraction process: volume of ionic liquid, volume of dispersant solvent, ionic strength, and pH. At the optimum working conditions, the average recoveries were 77.5 and 89.7%, the limits of detection were 0.06 and 0.09 μg/mL and the interday reproducibilities were 6.25 and 5.77% for benznidazole and nifurtimox, respectively. The proposed methodology can be considered sensitive, simple, robust, accurate, and green. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Ionic Liquid-Based Ultrasonic-Assisted Extraction of Secoisolariciresinol Diglucoside from Flaxseed (Linum usitatissimum L. with Further Purification by an Aqueous Two-Phase System

    Directory of Open Access Journals (Sweden)

    Zhi-Jian Tan

    2015-09-01

    Full Text Available In this work, a two-step extraction methodology of ionic liquid-based ultrasonic-assisted extraction (IL-UAE and ionic liquid-based aqueous two-phase system (IL-ATPS was developed for the extraction and purification of secoisolariciresinol diglucoside (SDG from flaxseed. In the IL-UAE step, several kinds of ILs were investigated as the extractants, to identify the IL that affords the optimum extraction yield. The extraction conditions such as IL concentration, ultrasonic irradiation time, and liquid–solid ratio were optimized using response surface methodology (RSM. In the IL-ATPS step, ATPS formed by adding kosmotropic salts to the IL extract was used for further separation and purification of SDG. The most influential parameters (type and concentration of salt, temperature, and pH were investigated to obtain the optimum extraction efficiency. The maximum extraction efficiency was 93.35% under the optimal conditions of 45.86% (w/w IL and 8.27% (w/w Na2SO4 at 22 °C and pH 11.0. Thus, the combination of IL-UAE and IL-ATPS makes up a simple and effective methodology for the extraction and purification of SDG. This process is also expected to be highly useful for the extraction and purification of bioactive compounds from other important medicinal plants.

  19. Synthesis of Ionic Liquid Based Electrolytes, Assembly of Li-ion Batteries, and Measurements of Performance at High Temperature.

    Science.gov (United States)

    Lin, Xinrong; Chapman Varela, Jennifer; Grinstaff, Mark W

    2016-12-20

    The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion batteries for use in devices operating at elevated temperatures require thermally stable and non-flammable electrolytes. Ionic liquids (ILs), which are non-flammable, non-volatile, thermally stable molten salts, are an ideal replacement for flammable and low boiling point organic solvent electrolytes currently used today. We herein describe the procedures to: 1) synthesize mono- and di-phosphonium ionic liquids paired with chloride or bis(trifluoromethane)sulfonimide (TFSI) anions; 2) measure the thermal properties and stability of these ionic liquids by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA); 3) measure the electrochemical properties of the ionic liquids by cyclic voltammetry (CV); 4) prepare electrolytes containing lithium bis(trifluoromethane)sulfonamide; 5) measure the conductivity of the electrolytes as a function of temperature; 6) assemble a coin cell battery with two of the electrolytes along with a Li metal anode and LiCoO2 cathode; and 7) evaluate battery performance at 100 °C. We additionally describe the challenges in execution as well as the insights gained from performing these experiments.

  20. Determination of Sunset Yellow and Tartrazine in Food Samples by Combining Ionic Liquid-Based Aqueous Two-Phase System with High Performance Liquid Chromatography

    Science.gov (United States)

    Sha, Ou; Zhu, Xiashi; Feng, Yanli; Ma, Weixing

    2014-01-01

    We proposed a simple and effective method, by coupling ionic liquid-based aqueous two-phase systems (IL-ATPSs) with high performance liquid chromatography (HPLC), for the analysis of determining tartrazine and sunset yellow in food samples. Under the optimized conditions, IL-ATPSs generated an extraction efficiency of 99% for both analytes, which could then be directly analyzed by HPLC without further treatment. Calibration plots were linear in the range of 0.01–50.0 μg/mL for both Ta and SY. The limits of detection were 5.2 ng/mL for Ta and 6.9 ng/mL for SY. This method proves successful for the separation/analysis of tartrazine and sunset yellow in soft drink sample, candy sample, and instant powder drink and leads to consistent results as obtained from the Chinese national standard method. PMID:25538857

  1. Determination of Sunset Yellow and Tartrazine in Food Samples by Combining Ionic Liquid-Based Aqueous Two-Phase System with High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Ou Sha

    2014-01-01

    Full Text Available We proposed a simple and effective method, by coupling ionic liquid-based aqueous two-phase systems (IL-ATPSs with high performance liquid chromatography (HPLC, for the analysis of determining tartrazine and sunset yellow in food samples. Under the optimized conditions, IL-ATPSs generated an extraction efficiency of 99% for both analytes, which could then be directly analyzed by HPLC without further treatment. Calibration plots were linear in the range of 0.01–50.0 μg/mL for both Ta and SY. The limits of detection were 5.2 ng/mL for Ta and 6.9 ng/mL for SY. This method proves successful for the separation/analysis of tartrazine and sunset yellow in soft drink sample, candy sample, and instant powder drink and leads to consistent results as obtained from the Chinese national standard method.

  2. Determination of sunset yellow and tartrazine in food samples by combining ionic liquid-based aqueous two-phase system with high performance liquid chromatography.

    Science.gov (United States)

    Sha, Ou; Zhu, Xiashi; Feng, Yanli; Ma, Weixing

    2014-01-01

    We proposed a simple and effective method, by coupling ionic liquid-based aqueous two-phase systems (IL-ATPSs) with high performance liquid chromatography (HPLC), for the analysis of determining tartrazine and sunset yellow in food samples. Under the optimized conditions, IL-ATPSs generated an extraction efficiency of 99% for both analytes, which could then be directly analyzed by HPLC without further treatment. Calibration plots were linear in the range of 0.01-50.0 μg/mL for both Ta and SY. The limits of detection were 5.2 ng/mL for Ta and 6.9 ng/mL for SY. This method proves successful for the separation/analysis of tartrazine and sunset yellow in soft drink sample, candy sample, and instant powder drink and leads to consistent results as obtained from the Chinese national standard method.

  3. Ionic liquid-based matrix solid-phase dispersion coupled with homogeneous liquid-liquid microextraction of synthetic dyes in condiments.

    Science.gov (United States)

    Wang, Zhibing; Zhang, Liyuan; Li, Na; Lei, Lei; Shao, Mingyuan; Yang, Xiao; Song, Ying; Yu, Aimin; Zhang, Hanqi; Qiu, Fangping

    2014-06-27

    The ionic liquid-based matrix solid-phase dispersion homogeneous liquid-liquid microextraction (IL-based MSPD-HLLME) was developed and applied to the extraction of four banned dyes, including chrysoidin, safranine O, auramine O and rhodamine B, in condiment samples. High performance liquid chromatography was applied to the separation and determination of the analytes. The solid sample was directly treated by MSPD using ionic liquid as dispersant and the eluate obtained in MSPD was treated by HLLME. Some experimental parameters, including type of dispersant, ratio of sample to dispersant, type and volume of ionic liquid, type and volume of elution solvent, pH value and ionic strength of the elution solvent, amount of ion-pairing agent (NH4PF6) and extraction time, were investigated and optimized. The linearities for determining the analytes were in the range of 60-2000μgkg(-1) for chrysoidin, 40-2000μgkg(-1) for safranine O and 20-1000μgkg(-1) for auramine O and rhodamine B, with the correlation coefficients ranging from 0.9964 to 0.9991. The limits of detection for the analytes were between 6.7 and 26.8μgkg(-1) and the limits of quantification were between 15.99 and 58.48μgkg(-1). When the present method was applied to the analysis of spiked condiment samples, the recoveries of the analytes ranged from 90.69 to 113.52% and relative standard deviations were lower than 8.2%. The present method combined the advantages of MSPD and HLLME, and could be applied for the determination of synthetic dyes in condiment samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Electrodeposition of compact zinc from the hydrophobic Brønsted acidic ionic liquid-based electrolytes and the study of zinc stability along with the acidity manipulation

    International Nuclear Information System (INIS)

    Chen, Yi-Han; Yeh, Hsin-Wen; Lo, Nai-Chang; Chiu, Chen-Wei; Sun, I-Wen; Chen, Po-Yu

    2017-01-01

    Highlights: • Compact Zn with no crack is deposited from protic ionic liquid-based electrolytes. • The ionic liquid is composed of the protonated betaine ion. • This ionic liquid is hydrophobic and zinc oxide is soluble in it. • The effects of co-solvents, propylene carbonate and water, are studied. • The Zn stripping/deposition efficiency can be manipulated via acidity adjustment. - Abstract: Compact crystalline zinc was electrodeposited on stainless-steel electrode (SS) via potentiostatic/galvanostatic electrolysis from the hydrophobic Brønsted acidic ionic liquid, protonated betaine bis((trifluoromethyl)sulfonyl)imide (IL [Hbet][TFSI]), −based electrolytes containing ZnCl 2 or ZnO under argon or ambient air atmosphere. Approximate 10 wt% of propylene carbonate and water, respectively, were used as the co-solvents for [Hbet][TFSI] to form the IL-based electrolytes. The efficiency of zinc deposition/stripping, which is significantly affected by the Brønsted acidity of the IL-based electrolytes, was studied at glassy carbon electrode (GC) to evaluate the stability of the zinc electrodeposits along with the electrolyte acidity. The stability is very poor for the zinc electrodeposits obtained from ZnCl 2 solution. However, it increases with increasing the quantity of ZnO or urea in the electrolytes; the former neutralize the dissociable protons in [Hbet] cations to form water, and the latter may form H-bonding with [Hbet] or be protonated to form the weakly acidic cations [HUrea]. Both suppress the reaction between the Zn electrodeposits and protons. The stability of the Zn electrodeposits, therefore, can be improved via the manipulation of the IL acidity.

  5. Ionic liquid-based microwave-assisted dispersive liquid-liquid microextraction and derivatization of sulfonamides in river water, honey, milk, and animal plasma

    Energy Technology Data Exchange (ETDEWEB)

    Xu Xu; Su Rui; Zhao Xin; Liu Zhuang; Zhang Yupu; Li Dan; Li Xueyuan; Zhang Hanqi [College of Chemistry, Jilin University, Changchun 130012 (China); Wang Ziming, E-mail: analchem@jlu.edu.cn [College of Chemistry, Jilin University, Changchun 130012 (China)

    2011-11-30

    Graphical abstract: The extraction and derivatization efficiency of SAs is dependent on type and volume of extraction solvent, type and volume of disperser, microwave power and irradiation time, volume of derivatization reagent, pH of sample solution as well as ionic strength. Highlights: Black-Right-Pointing-Pointer A new, rapid and sensitive method for determining sulfonamides (SAs) was proposed. Black-Right-Pointing-Pointer Derivatization, extraction and preconcentration of SAs were performed in one step. Black-Right-Pointing-Pointer IL-based MADLLME and derivatization were first applied for the determination of SAs. Black-Right-Pointing-Pointer Trace SAs in river water, honey, milk, and pig plasma were determined. - Abstract: The ionic liquid-based microwave-assisted dispersive liquid-liquid microextraction (IL-based MADLLME) and derivatization was applied for the pretreatment of six sulfonamides (SAs) prior to the determination by high-performance liquid chromatography (HPLC). By adding methanol (disperser), fluorescamine solution (derivatization reagent) and ionic liquid (extraction solvent) into sample, extraction, derivatization, and preconcentration were continuously performed. Several experimental parameters, such as the type and volume of extraction solvent, the type and volume of disperser, amount of derivatization reagent, microwave power, microwave irradiation time, pH of sample solution, and ionic strength were investigated and optimized. When the microwave power was 240 W, the analytes could be derivatized and extracted simultaneously within 90 s. The proposed method was applied to the analysis of river water, honey, milk, and pig plasma samples, and the recoveries of analytes obtained were in the range of 95.0-110.8, 95.4-106.3, 95.0-108.3, and 95.7-107.7, respectively. The relative standard deviations varied between 1.5% and 7.3% (n = 5). The results showed that the proposed method was a rapid, convenient and feasible method for the determination

  6. High-Permeance Room-Temperature Ionic-Liquid-Based Membranes for CO2/N-2 Separation

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, JS; Mok, MM; Cowan, MG; McDanel, WM; Carlisle, TK; Gin, DL; Noble, RD

    2014-12-24

    We have developed and fabricated thin-film composite (TFC) membranes with an active layer consisting of a room-temperature ionic liquid/polymerized (room-temperature ionic liquid) [i.e., (RTIL)/poly(RTIL)] composite material. The resulting membrane has a CO2 permeance of 6100 +/- 400 GPU (where 1 GPU = 10(-6) cm(3)/(cm(2) s cmHg)) and an ideal CO2/N-2 selectivity of 22 +/- 2. This represents a new membrane with state-of-the-art CO2 permeance and good CO2/N-2 selectivity. To our knowledge, this is the first example of a TFC gas separation membrane composed of an RTIL-containing active layer.

  7. Targeting adequate thermal stability and fire safety in selecting ionic liquid-based electrolytes for energy storage.

    Science.gov (United States)

    Chancelier, L; Diallo, A O; Santini, C C; Marlair, G; Gutel, T; Mailley, S; Len, C

    2014-02-07

    The energy storage market relating to lithium based systems regularly grows in size and expands in terms of a portfolio of energy and power demanding applications. Thus safety focused research must more than ever accompany related technological breakthroughs regarding performance of cells, resulting in intensive research on the chemistry and materials science to design more reliable batteries. Formulating electrolyte solutions with nonvolatile and hardly flammable ionic liquids instead of actual carbonate mixtures could be safer. However, few definitions of thermal stability of electrolytes based on ionic liquids have been reported in the case of abuse conditions (fire, shortcut, overcharge or overdischarge). This work investigates thermal stability up to combustion of 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide ([C1C4Im][NTf2]) and 1-butyl-1-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide ([PYR14][NTf2]) ionic liquids, and their corresponding electrolytes containing lithium bis(trifluoromethanesulfonyl)imide LiNTf2. Their possible routes of degradation during thermal abuse testings were investigated by thermodynamic studies under several experimental conditions. Their behaviours under fire were also tested, including the analysis of emitted compounds.

  8. On-line ionic liquid-based dynamic microwave-assisted extraction-high performance liquid chromatography for the determination of lipophilic constituents in root of Salvia miltiorrhiza Bunge.

    Science.gov (United States)

    Gao, Shiqian; Yu, Wei; Yang, Xiao; Liu, Zhonglin; Jia, Yilong; Zhang, Hanqi

    2012-10-01

    On-line continuous sampling, ionic liquid-based dynamic microwave-assisted extraction high performance liquid chromatography has been developed and applied to the extraction of lipophilic constituents from root of Salvia miltiorrhiza Bunge. Several operating parameters were optimized by single-factor and Box-Behnken design experiments. The type and concentration of ionic liquids, power of microwave irradiation, flow rate of sample suspension, amount, and particle size of sample were investigated. The limits of detection for tanshin-one I, cryptotanshinone, and tanshinone II(A) are 0.014, 0.009, and 0.009 mg/g, respectively. The RSDs of interday and intraday were lower than 2.02 and 2.16%, respectively. The recoveries for target analytes were in the range of 90.7-101.8%. The homogeneity of the suspension and stability of the analytes were investigated and the results were satisfactory. The proposed method was compared with the off-line ionic liquid-based dynamic microwave-assisted extraction, off-line ethanol-based dynamic microwave-assisted extraction, ionic liquid-based ultrasonic-assisted extraction, and ionic liquid-based maceration extraction. The results indicated that the proposed method is effective for the extraction of the active components in Chinese herbal medicine and has some advantages over the other methods. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Self-Assembled Polymeric Ionic Liquid-Functionalized Cellulose Nano-crystals: Constructing 3D Ion-conducting Channels Within Ionic Liquid-based Composite Polymer Electrolytes.

    Science.gov (United States)

    Shi, Qing Xuan; Xia, Qing; Xiang, Xiao; Ye, Yun Sheng; Peng, Hai Yan; Xue, Zhi Gang; Xie, Xiao Lin; Mai, Yiu-Wing

    2017-09-04

    Composite polymeric and ionic liquid (IL) electrolytes are some of the most promising electrolyte systems for safer battery technology. Although much effort has been directed towards enhancing the transport properties of polymer electrolytes (PEs) through nanoscopic modification by incorporating nano-fillers, it is still difficult to construct ideal ion conducting networks. Here, a novel class of three-dimensional self-assembled polymeric ionic liquid (PIL)-functionalized cellulose nano-crystals (CNC) confining ILs in surface-grafted PIL polymer chains, able to form colloidal crystal polymer electrolytes (CCPE), is reported. The high-strength CNC nano-fibers, decorated with PIL polymer chains, can spontaneously form three-dimensional interpenetrating nano-network scaffolds capable of supporting electrolytes with continuously connected ion conducting networks with IL being concentrated in conducting domains. These new CCPE have exceptional ionic conductivities, low activation energies (close to bulk IL electrolyte with dissolved Li salt), high Li + transport numbers, low interface resistances and improved interface compatibilities. Furthermore, the CCPE displays good electrochemical properties and a good battery performance. This approach offers a route to leak-free, non-flammable and high ionic conductivity solid-state PE in energy conversion devices. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Preparation of CLA ascorbyl ester with improved volumetric productivity by an ionic liquid-based reaction system

    DEFF Research Database (Denmark)

    Chen, B.L.; Guo, Zheng; Let, M.B.

    2008-01-01

    A new approach to the enzymatic production Of conjugated linoleic acid (CLA) ascorbyl ester with a remarkably high volumetric productivity (120-200 g L-1) has been developed, in which strong solvation by tOMA-TFA (methyltrioctylammonium trifluoroacetate) enables a high concentration of ascorbic...... acid to be applied, and in which t-butanol enhances conversion by changing the equilibrium constant of the activity coefficients. This work has experimentally demonstrated the practicability of achieving efficient reactions of polar compounds at high concentrations in ionic liquids without significant...

  11. Ionic liquid-based air-assisted liquid-liquid microextraction followed by high performance liquid chromatography for the determination of five fungicides in juice samples.

    Science.gov (United States)

    You, Xiangwei; Chen, Xiaochu; Liu, Fengmao; Hou, Fan; Li, Yiqiang

    2018-01-15

    A novel and simple ionic liquid-based air-assisted liquid-liquid microextraction technique combined with high performance liquid chromatography was developed to analyze five fungicides in juice samples. In this method, ionic liquid was used instead of a volatile organic solvent as the extraction solvent. The emulsion was formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent repeatedly using a 10mL glass syringe. No organic dispersive solvent was required. Under the optimized conditions, the limits of detection (LODs) were 0.4-1.8μgL -1 at a signal-to-noise ratio of 3. The limits of quantification (LOQs) set as the lowest spiking levels with acceptable recovery in juices were 10μgL -1 , except for fludioxonil whose LOQ was 20μgL -1 . The proposed method was applied to determine the target fungicides in juice samples, and acceptable recoveries ranging from 74.9% to 115.4% were achieved. Copyright © 2017. Published by Elsevier Ltd.

  12. Optimization of Ionic Liquid Based Simultaneous Ultrasonic- and Microwave-Assisted Extraction of Rutin and Quercetin from Leaves of Velvetleaf (Abutilon theophrasti) by Response Surface Methodology

    Science.gov (United States)

    Zhao, Chunjian; Lu, Zhicheng; He, Xin; Li, Zhao; Shi, Kunming; Yang, Lei; Fu, Yujie; Zu, Yuangang

    2014-01-01

    An ionic liquids based simultaneous ultrasonic and microwave assisted extraction (ILs-UMAE) method has been proposed for the extraction of rutin (RU), quercetin (QU), from velvetleaf leaves. The influential parameters of the ILs-UMAE were optimized by the single factor and the central composite design (CCD) experiments. A 2.00 M 1-butyl-3-methylimidazolium bromide ([C4mim]Br) was used as the experimental ionic liquid, extraction temperature 60°C, extraction time 12 min, liquid-solid ratio 32 mL/g, microwave power of 534 W, and a fixed ultrasonic power of 50 W. Compared to conventional heating reflux extraction (HRE), the RU and QU extraction yields obtained by ILs-UMAE were, respectively, 5.49 mg/g and 0.27 mg/g, which increased, respectively, 2.01-fold and 2.34-fold with the recoveries that were in the range of 97.62–102.36% for RU and 97.33–102.21% for QU with RSDs lower than 3.2% under the optimized UMAE conditions. In addition, the shorter extraction time was used in ILs-UMAE, compared with HRE. Therefore, ILs-UMAE was a rapid and an efficient method for the extraction of RU and QU from the leaves of velvetleaf. PMID:25243207

  13. Performance analysis of absorption heat transformer cycles using ionic liquids based on imidazolium cation as absorbents with 2,2,2-trifluoroethanol as refrigerant

    International Nuclear Information System (INIS)

    Ayou, Dereje S.; Currás, Moisés R.; Salavera, Daniel; García, Josefa; Bruno, Joan C.; Coronas, Alberto

    2014-01-01

    Highlights: • TFE + [emim][BF 4 ] (or [bmim][BF 4 ]) absorption heat transformer cycles are studied. • Influence of various operating conditions on cycle’s performance is investigated. • Performance comparisons with H 2 O + LiBr and TFE + TEGDME cycles are done. • Enthalpy data for TFE + [emim][BF 4 ] (or [bmim][BF 4 ]) liquid mixtures are calculated. • TFE + [emim][BF 4 ] (or [bmim][BF 4 ]) cycles have higher gross temperature lift (GTL). - Abstract: A detailed thermodynamic performance analysis of a single-stage absorption heat transformer and double absorption heat transformer cycles using new working pairs composed of ionic liquids (1-ethyl-3-methylimidazolium tetrafluoroborate ([emim][BF 4 ]) and 1-butyl-3-methylimidazolium tetrafluoroborate ([bmim][BF 4 ])) as absorbent and 2,2,2-trifluoroethanol (TFE) as refrigerant has been studied. Several performance indicators were used to evaluate and compare the performance of the cycles using the TFE + [emim][BF 4 ] and TFE + [bmim][BF 4 ] working pairs with the conventional H 2 O + LiBr and organic TFE + TEGDME working pairs. The obtained results show that the ionic liquid based working pairs are suitable candidates to replace the conventional H 2 O + LiBr working pairs in order to avoid the disadvantages associated with it mainly crystallization and corrosion and also they perform better (higher gross temperature lift) than TFE + TEGDME working pair at several operating conditions considered in this work

  14. Characterization of a novel intrinsic luminescent room-temperature ionic liquid based on [P6,6,6,14 ][ANS].

    Science.gov (United States)

    Delgado, Joana M; Raymundo, Anabela; Vilarigues, Márcia; Branco, Luís C; Laia, César A T

    2015-01-07

    Intrinsically luminescent room-temperature ionic liquids (RTILs) can be prepared by combining a luminescent anion (more common) or cation with appropriate counter ions, rendering new luminescent soft materials. These RTILs are still new, and many of their photochemical properties are not well known. A novel intrinsic luminescent RTIL based on the 8-anilinonaphthalene-1-sulfonate ([ANS]) anion combined with the trihexyltetradecylphosphonium ([P6,6,6,14 ]) cation was prepared and characterized by spectroscopic techniques. Detailed photophysical studies highlight the influence of the ionic liquid environment on the ANS fluorescence, which together with rheological and (1) H NMR experiments illustrate the effects of both the viscosity and electrostatic interactions between the ions. This material is liquid at room temperature and possesses a glass transition temperature (Tg ) of 230.4 K. The fluorescence is not highly sensitive to factors such as temperature, but owing to its high viscosity, dynamic Stokes shift measurements reveal very slow components for the IL relaxation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Preparation of a polymeric ionic liquid-based adsorbent for stir cake sorptive extraction of preservatives in orange juices and tea drinks

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Lei; Huang, Xiaojia, E-mail: hxj@xmu.edu.cn

    2016-04-15

    In this study, a new polymeric ionic liquid-based adsorbent was prepared and used as the extraction medium of stir cake sorptive extraction (SCSE) of three organic acid preservatives, namely, p-hydroxybenzoic acid, sorbic acid and cinnamic acid. The adsorbent was synthesized by the copolymerization of 1-ally-3-vinylimidazolium chloride (AV) and divinylbenzene (DVB) in the presence of a porogen solvent containing 1-propanol and 1,4-butanediol. The effect of the content of monomer and the porogen solvent in the polymerization mixture on the extraction performance was investigated thoroughly. The adsorbent was characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. To obtain the optimal extraction conditions of SCSE/AVDVB for target analytes, key parameters including desorption solvent, adsorption and desorption time, ionic strength and pH value in sample matrix were studied in detail. The results showed that under the optimized conditions, the SCSE/AVDVB could extract the preservatives effectively through multiply interactions. At the same time, a simple and sensitive method by combining SCSE/AVDVB and high-performance liquid chromatography with diode array detection was developed for the simultaneous analysis of the target preservatives in orange juices and tea drinks. Low limits of detection (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target analytes were achieved within the range of 0.012–0.23 μg/L and 0.039–0.42 μg/L, respectively. The precision of the proposed method was evaluated in terms of intra- and inter-assay variability calculated as relative standard deviation (RSD), and it was found that the values were all below 10%. Finally, the proposed method was used to detect preservatives in different orange juice and tea drink samples successfully. The recoveries were in the range of 71.9–116%, and the RSDs were below 10% in the all cases

  16. Effect of lithium salts addition on the ionic liquid based extraction of essential oil from Farfarae Flos.

    Science.gov (United States)

    Li, Zhen-Yu; Zhang, Sha-Sha; Jie-Xing; Qin, Xue-Mei

    2015-01-01

    In this study, an ionic liquids (ILs) based extraction approach has been successfully applied to the extraction of essential oil from Farfarae Flos, and the effect of lithium chloride was also investigated. The results indicated that the oil yields can be increased by the ILs, and the extraction time can be reduced significantly (from 4h to 2h), compared with the conventional water distillation. The addition of lithium chloride showed different effect according to the structures of ILs, and the oil yields may be related with the structure of cation, while the chemical compositions of essential oil may be related with the anion. The reduction of extraction time and remarkable higher efficiency (5.41-62.17% improved) by combination of lithium salt and proper ILs supports the suitability of the proposed approach. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Influence of polyoxyethylene phytosterol addition in ionic liquid-based electrolyte on photovoltaic performance of dye-sensitized solar cells

    International Nuclear Information System (INIS)

    Takahashi, Masashi; Sato, Kei; Sakurai, Sho; Kobayashi, Koichi

    2016-01-01

    Highlights: • The ionic liquid solution of less solvophilic BPS exhibits a better surface active property and a weaker dye-desorption effect. • Photovoltaic performances of the N719- and NKX2677-sensitized DSSCs can be improved by the BPS addition to the IL-based electrolyte. • BPS added to the electrolyte plays a key role in reducing charge-transfer resistance and increasing electron lifetime in the TiO 2 electrode. - Abstract: In this work, we studied influence of polyoxyethylene phytosterol (BPS) addition in ionic liquid (IL)-based electrolyte on photovoltaic performance of dye-sensitized solar cells (DSSCs) using 1-methyl-3-propylimidazolium iodide as an IL. Surface tension, photocurrent density-voltage characteristics and electrochemical impedance spectra were measured to clarify the role of BPS in the DSSCs using three different dyes. The results showed that the IL solution of less solvophilic BPS-EO5 exhibited a better surface active property and a weaker dye-desorption effect than BPS-EO30 and BPS-PO7/EO30. Short-circuit current densities of the N719- and NKX2677-sensitized cells were found to be noticeably increased by the addition of either BPS-EO5 or BPS-EO30 to the IL-based electrolyte in the concentration range of 0.001–0.01 mol dm −3 . Enhanced photovoltaic conversion efficiencies were obtained for these DSSCs, which most likely resulted from the effects of BPS on reducing charge-transfer resistance at the TiO 2 /dye/electrolyte interface and on increasing electron lifetime within the TiO 2 photoanode.

  18. Probing the microscopic structural organization of neat ionic liquids (ILs) and ionic liquid-based gels through resonance energy transfer (RET) studies.

    Science.gov (United States)

    Majhi, Debashis; Sarkar, Moloy

    2017-08-30

    With the aim to understand the role of the ionic constituents of ionic liquids (ILs) in their structural organization, resonance energy transfer (RET) studies between ionic liquids (donor) and rhodamine 6G (acceptor) have been investigated. RET studies have been exploited for the present investigation due to the fact that the said process is extremely sensitive to the distance, and a change in the donor-acceptor distance due to a change in the structural organization can be probed. Basically, steady state and time-resolved fluorescence measurements have been carried out in two different sets of ILs, where in one set (1-ethyl-3-methyl imidazolium alkyl sulfate) the alkyl side chain length on the anionic moiety is systematically varied and in the other set variation is done on the cation (aromatic and nonaromatic). The data related to the RET events have been analyzed in light of Förster theory. A clear rise time in the fluorescence intensity decay profile of the acceptor has unequivocally established the RET process between the donor and acceptor. Interestingly, the rise times and energy transfer efficiencies are also observed to vary with a variation in the alkyl chain length as well as the nature of the cations. More interestingly, the donor-acceptor distance (R DA ) is observed to increase from 35.0 Å to 47.5 Å upon increasing the anion chain length from ethyl to octyl. However, R DA is found to decrease (40.5 Å to 34.9 Å) upon going from 1-methyl-3-butylimidazolium to 1-butyl-1-methylpyrrolidinium cations. The variation of the relevant RET parameters for the two sets of ILs has been rationalized by considering the change in the structural organization of the respective set of ILs. Additionally, observation of the RET process also in an IL-based gel system indicates the potential use of this fluorescent gel material for future applications.

  19. Synthesis and characterisation of ionic liquids based on 1-butyl-3-methylimidazolium chloride and MCl(4), M = Hf and Zr.

    Science.gov (United States)

    Campbell, Paul S; Santini, Catherine C; Bouchu, Denis; Fenet, Bernard; Rycerz, Leszek; Chauvin, Yves; Gaune-Escard, Marcelle; Bessada, Catherine; Rollet, Anne-Laure

    2010-02-07

    Dialkylimidazolium chlorometallate molten salts resulting from the combination of zirconium or hafnium tetrachloride and 1-butyl-3-methylimidazolium chloride, [C(1)C(4)Im][Cl], have been prepared with a molar fraction of MCl(4), R = n(MCl4)/n(MCl4) + n([C1C4IM][Cl]) equal to 0, 0.1, 0.2, 0.33, 0.5, 0.67. The structure and composition were studied by Differential Scanning Calorimetry (DSC), (35)Cl (263 to 333 K), (1)H and (13)C solid state and solution NMR spectroscopy, and electrospray ionisation (ESI) mass spectrometry. The primary anions of the MCl(4)-based ILs were [MCl(5)], [MCl(6)] and [M(2)Cl(9)], whose relative abundances varied with R. For R = 0.33, pure solid [C(1)C(4)Im](2)[MCl(6)], for both M = Zr and Hf are formed (m.p. = 366 and 385 K, respectively). For R = 0.67 pure ionic liquids [C(1)C(4)Im][M(2)Cl(9)] for both M = Zr and Hf are formed (T(g) = 224 and 220 K, respectively). The thermal dissociation has been attempted of [C(1)C(4)Im](2)[HfCl(6)], and [C(1)C(4)Im](2)[ZrCl(6)] monitored by (35)Cl and (91)Zr solid NMR (high temperature up to 551 K).

  20. Sensitive determination of cadmium in water samples by room temperature ionic liquid-based preconcentration and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Martinis, Estefania M. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, C.C. 131, M 5502 IRA Mendoza (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Olsina, Roberto A. [Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis (Argentina); Altamirano, Jorgelina C. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, C.C. 131, M 5502 IRA Mendoza (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina); Wuilloud, Rodolfo G. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, C.C. 131, M 5502 IRA Mendoza (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)], E-mail: rwuilloud@mendoza-conicet.gov.ar

    2008-10-17

    A sensitive preconcentration methodology for Cd determination at trace levels in water samples was developed in this work. 1-Butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}MIM][PF{sub 6}]) room temperature ionic liquid (RTIL) was successfully used for Cd preconcentration, as cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex [Cd-5-Br-PADAP]. Subsequently, Cd was back-extracted from the RTIL phase with 500 {mu}L of 0.5 mol L{sup -1} nitric acid and determined by electrothermal atomic absorption spectrometry (ETAAS). A preconcentration factor of 40 was achieved with 20 mL of sample. The limit of detection (LOD) obtained under optimum conditions was 3 ng L{sup -1} and the relative standard deviation (R.S.D.) for 10 replicates at 1 {mu}g L{sup -1} Cd{sup 2+} concentration level was 3.5%, calculated at peak heights. The calibration graph was linear from concentration levels near the detection limits up to at least 5 {mu}g L{sup -1}. A correlation coefficient of 0.9997 was achieved. Validation of the methodology was performed by standard addition method and analysis of certified reference material (CRM). The method was successfully applied to the determination of Cd in river and tap water samples.

  1. Preparation of Thermo-Responsive Poly(ionic liquids-Based Nanogels via One-Step Cross-Linking Copolymerization

    Directory of Open Access Journals (Sweden)

    Jing Zhang

    2015-09-01

    Full Text Available In this study, thermo-responsive polymeric nanogels were facilely prepared via one-step cross-linking copolymerization of ethylene glycol dimethacrylate/divinylbenzene and ionic liquid (IL-based monomers, 1,n-dialkyl-3,3′-bis-1-vinyl imidazolium bromides ([CnVIm]Br; n = 6, 8, 12 in selective solvents. The results revealed that stable and blue opalescent biimidazolium (BIm-based nanogel solutions could be obtained without any precipitation when the copolymerizations were conducted in methanol. Most importantly, these novel nanogels were thermo-response, and could reversibly transform to precipitation in methanol with temperature changes. Turbidity analysis and dynamic light scatting (DLS measurement illustrated that PIL-based nanogel solutions presented the phase transform with upper critical solution temperature (UCST in the range of 5–25 °C. The nanogels were characterized using Fourier transform infrared (FTIR, thermogravimetric analyses (TGA, and scanning electron microscopy (SEM. In addition, BIm-based nanogels could also be used as highly active catalysts in the cycloaddition reaction of CO2 and epoxides. As a result, our attributes build a robust platform suitable for the preparation of polymeric nanomaterials, as well as CO2 conversion.

  2. Ultrasonic-energy enhance the ionic liquid-based dual microextraction to preconcentrate the lead in ground and stored rain water samples as compared to conventional shaking method.

    Science.gov (United States)

    Nizamani, Sooraj; Kazi, Tasneem G; Afridi, Hassan I

    2018-01-01

    An efficient preconcentration technique based on ultrasonic-assisted ionic liquid-based dual microextraction (UA-ILDµE) method has been developed to preconcentrate the lead (Pb +2 ) in ground and stored rain water. In the current proposed method, Pb +2 was complexed with a chelating agent (dithizone), whereas an ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate) was used for extraction purpose. The ultrasonic irradiation and electrical shaking system were applied to enhance the dispersion and extraction of Pb +2 complex in aqueous samples. For second phase, dual microextraction (DµE phase), the enriched Pb +2 complex in ionic liquid, extracted back into the acidic aqueous solution and finally determined by flame atomic absorption spectrometry. Some major analytical parameters that influenced the extraction efficiency of developed method, such as pH, concentration of ligand, volume of ionic liquid and samples, time of shaking in thermostatic electrical shaker and ultrasonic bath, effect of back extracting HNO 3 volume, matrix effect, centrifugation time and rate were optimized. At the sample volume of 25mL, the calculated preconcentration factor was 62.2. The limit of detection of proposed procedure for Pb +2 ions was found to be 0.54μgL -1 . The validation of developed method was performed by the analysis of certified sample of water SRM 1643e and standard addition method in a real water sample. The extraction recovery of Pb +2 was enhanced≥2% with shaking time of 80s in ultrasonic bath as compared to used thermostatic electrical shaker, where for optimum recovery up to 10min was required. The developed procedure was successfully used for the enrichment of Pb +2 in ground and stored rain water (surface water) samples of an endemic region of Pakistan. The resulted data indicated that the ground water samples were highly contaminated with Pb +2 , while some of the surface water samples were also have higher values of Pb +2 than permissible limit of

  3. Ionic liquids based on phosphonium cations as neat lubricants or lubricant additives for a steel/steel contact.

    Science.gov (United States)

    Otero, Inés; López, Enriqueta R; Reichelt, Manuela; Villanueva, María; Salgado, Josefa; Fernández, Josefa

    2014-08-13

    After doing several miscibility essays with eight ionic liquids (ILs) and four base oils, the ILs tri(butyl)ethylphosphonium diethylphosphate [P4,4,4,2][C2C2PO4] and trihexyl(tetradecyl)phosphonium tris(pentafluoroethyl)trifluorophosphate [P6,6,6,14][(C2F5)3PF3] were selected to be studied as lubricant additives. The neat IL [P4,4,4,2][C2C2PO4], the base oils, and several blends were characterized in terms of density, viscosity, and thermal stability. The tribological performance of the miscible base oil/IL blends (1 wt %) and the neat [P4,4,4,2][C2C2PO4] were evaluated for the lubrication of an AISI 420 steel-100Cr6 steel contact pair. The friction coefficients and wear volumes obtained are also compared with those corresponding to the pure base oils and their mixtures with conventional additive zinc dialkyldithiophosphate (ZDDP). As neat lubricants, [P4,4,4,2][C2C2PO4] showed the best antifriction ability, whereas in terms of wear, better results were obtained with [P6,6,6,14][(C2F5)3PF3]. However, higher improvements in both friction and wear were found for blends containing [P4,4,4,2][C2C2PO4]. XPS analyses of the worn surfaces lubricated with these mixtures indicated the presence of phosphorus in the tribofilm formed on the wear track. However, this compound was slightly detected on tribosamples lubricated with blends containing [P6,6,6,14][(C2F5)3PF3].

  4. An ionic liquid-based nanofluid of titanium dioxide nanoparticles for effervescence-assisted dispersive liquid-liquid extraction for acaricide detection.

    Science.gov (United States)

    Wu, Xiaoling; Li, Xin; Yang, Miyi; Zeng, Haozhe; Zhang, Sanbing; Lu, Runhua; Gao, Haixiang; Xu, Donghui

    2017-05-12

    Phytophagous mites are usually considered a difficult problem for agricultural planting, and acaricides are applied to control diseases and pests. However, the overdose and misusage of acaricides causes pesticide residues. In this work, a simple and practical ionic liquid-based TiO 2 nanofluid, effervescence-assisted, dispersive liquid-liquid microextraction (EA-DLLME) method was developed to detect acaricides in honey and tea by high-performance liquid chromatography (HPLC-DAD). Oleophilic TiO 2 nanoparticles were synthesized by a facile solvothermal method to obtain greater stability of the nanofluid. The experimental parameters were optimized by a one-factor-at-a-time approach and included the effervescent tablet composition, ionic liquid selection, extractant composition, nanofluid volume, extraction temperature, extraction time and desorption conditions. Under the optimized conditions, the linear ranges of this proposed method were 0.5-500μgL -1 , with correlation coefficients in the range of 0.9985-1.0000. The extraction efficiencies for the target analytes varied from 70.70 to 84.58%. The detection and quantitation limits were in the ranges of 0.04-0.18μgL -1 and 0.13-0.60μgL -1 , respectively. The intra- and inter-day relative standard deviations (n=3) were found to range from 2.32 to 5.71%, which showed perfect repeatability. Overall, the EA-DLLME method was time-saving and environmentally friendly, with future potential for microextraction. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Simultaneous multicomponent spectrophotometric monitoring of methyl and propyl parabens using multivariate statistical methods after their preconcentration by robust ionic liquid-based dispersive liquid-liquid microextraction

    Science.gov (United States)

    Khani, Rouhollah; Ghasemi, Jahan B.; Shemirani, Farzaneh

    2014-03-01

    A powerful and efficient signal-preprocessing technique that combines local and multiscale properties of the wavelet prism with the global filtering capability of orthogonal signal correction (OSC) is applied for pretreatment of spectroscopic data of parabens as model compounds after their preconcentration by robust ionic liquid-based dispersive liquid-liquid microextraction method (IL-DLLME). In the proposed technique, a mixture of a water-immiscible ionic liquid (as extraction solvent) [Hmim][PF6] and disperser solvent is injected into an aqueous sample solution containing one of the IL's ions, NaPF6, as extraction solvent and common ion source. After preconcentration, the absorbance of the extracted compounds was measured in the wavelength range of 200-700 nm. The wavelet orthogonal signal correction with partial least squares (WOSC-PLS) method was then applied for simultaneous determination of each individual compound. Effective parameters, such as amount of IL, volume of the disperser solvent and amount of NaPF6, were inspected by central composite design to identify the most important parameters and their interactions. The effect of pH on the sensitivity and selectivity was studied according to the net analyte signal (NAS) for each component. Under optimum conditions, enrichment factors of the studied compounds were 75 for methyl paraben (MP) and 71 for propyl paraben (PP). Limits of detection for MP and PP were 4.2 and 4.8 ng mL-1, respectively. The root mean square errors of prediction for MP and PP were 0.1046 and 0.1275 μg mL-1, respectively. The practical applicability of the developed method was examined using hygienic, cosmetic, pharmaceutical and natural water samples.

  6. Ionic liquid-based electromembrane extraction and its comparison with traditional organic solvent based electromembrane extraction for the determination of strychnine and brucine in human urine.

    Science.gov (United States)

    Sun, Jian-Nan; Chen, Juan; Shi, Yan-Ping

    2014-07-25

    An ionic liquid-based electromembrane extraction (IL-EME) method was presented, and its performance was compared with 2-ethylnitrobenzene (ENB) based EME for the determination of strychnine and brucine in human urine. For the two methods, the fundamental extraction parameters such as supported liquid membrane, voltage, extraction time, pH values of sample solution and acceptor solution, temperature and salting-out effect were separately optimized. IL-EME provided 96- and 122-fold enrichment factors for strychnine and brucine, respectively, which were better than those obtained in EME (83- and 86-fold, respectively). The calibration curves were linear over the ranges of 20-720 μg L(-1) for strychnine and 20-640 μg L(-1) for brucine with the correlation coefficients higher than 0.9950. The repeatability of EME and IL-EME were evaluated by five parallel experiments giving the relative standard deviations of 5.12-6.98%. As the results indicated, compared with ENB based EME, the proposed IL-EME is more reliable and could provide better extraction performance for the determination of strychnine and brucine in human urine. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Double salt ionic liquids based on 1-ethyl-3-methylimidazolium acetate and hydroxyl-functionalized ammonium acetates: strong effects of weak interactions.

    Science.gov (United States)

    Pereira, Jorge F B; Barber, Patrick S; Kelley, Steven P; Berton, Paula; Rogers, Robin D

    2017-10-11

    The properties of double salt ionic liquids based on solutions of cholinium acetate ([Ch][OAc]), ethanolammonium acetate ([NH 3 (CH 2 ) 2 OH][OAc]), hydroxylammonium acetate ([NH 3 OH][OAc]), ethylammonium acetate ([NH 3 CH 2 CH 3 ][OAc]), and tetramethylammonium acetate ([N(CH 3 ) 4 ][OAc]) in 1-ethyl-3-methylimidazolium acetate ([C 2 mim][OAc]) were investigated by NMR spectroscopy and X-ray crystallography. Through mixture preparation, the solubility of [N(CH 3 ) 4 ][OAc] is the lowest, and [Ch][OAc] shows a 3-fold lower solubility than the other hydroxylated ammonium acetate-based salts in [C 2 mim][OAc] at room temperature. NMR and X-ray crystallographic studies of the pure salts suggest that the molecular-level mechanisms governing such miscibility differences are related to the weaker interactions between the -NH 3 groups and [OAc] - , even though three of these salts possess the same strong 1 : 1 hydrogen bonds between the cation -OH group and the [OAc] - ion. The formation of polyionic clusters between the anion and those cations with unsatisfied hydrogen bond donors seems to be a new tool by which the solubility of these salts in [C 2 mim][OAc] can be controlled.

  8. Sensitive determination of estrogens in environmental waters treated with polymeric ionic liquid-based stir cake sorptive extraction and liquid chromatographic analysis.

    Science.gov (United States)

    Chen, Lei; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

    2016-05-15

    A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057 µg/L and 0.08-0.19 µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Ultrasound-assisted sol-gel synthesis of ZrO2.

    Science.gov (United States)

    Guel, Marlene Lariza Andrade; Jiménez, Lourdes Díaz; Hernández, Dora Alicia Cortés

    2017-03-01

    Synthesis of tetragonal ZrO 2 by both conventional sol-gel and ultrasound-assisted sol-gel methods and using a non-ionic surfactant Tween-20, was performed. A porous microstructure composed of nanometric particles was observed. Tetragonal ZrO 2 was obtained using a low heat treatment temperature of powders, 500°C by both methods. A higher crystallinity and a shorter reaction time were observed when ultrasound was used in the sol-gel method due to the cavitation phenomenon. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Ultrasound-assisted dyeing of cellulose acetate.

    Science.gov (United States)

    Udrescu, C; Ferrero, F; Periolatto, M

    2014-07-01

    The possibility of reducing the use of auxiliaries in conventional cellulose acetate dyeing with Disperse Red 50 using ultrasound technique was studied as an alternative to the standard procedure. Dyeing of cellulose acetate yarn was carried out by using either mechanical agitation alone, with and without auxiliaries, or coupling mechanical and ultrasound agitation in the bath where the temperature range was maintained between 60 and 80 °C. The best results of dyeing kinetics were obtained with ultrasound coupled with mechanical agitation without auxiliaries (90% of bath exhaustion value at 80 °C). Hence the corresponding half dyeing times, absorption rate constants according to Cegarra-Puente modified equation and ultrasound efficiency were calculated confirming the synergic effect of sonication on the dyeing kinetics. Moreover the apparent activation energies were also evaluated and the positive effect of ultrasound added to mechanical agitation was evidenced by the lower value (48 kJ/mol) in comparison with 112 and 169 kJ/mol for mechanical stirring alone with auxiliaries and without, respectively. Finally, the fastness tests gave good values for samples dyed with ultrasound technique even without auxiliaries. Moreover color measurements on dyed yarns showed that the color yield obtained by ultrasound-assisted dyeing at 80 °C of cellulose acetate without using additional chemicals into the dye bath reached the same value yielded by mechanical agitation, but with remarkably shorter time. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. KINETICS OF ULTRASOUND ASSISTED EXTRACTION OF WEDELOLACTONE FROM Eclipta alba

    OpenAIRE

    Charpe, T. W.; Rathod, V. K.

    2016-01-01

    Abstract Ultrasound assisted extraction of wedelolactone, a major coumestan present in Eclipta alba, is investigated in the present work.Various process parameters such as type of solvent, power, solvent to solid ratio and extraction temperature, which affect the extraction yield, are optimized. In the ultrasound-assisted extraction with final optimized conditions, i.e., methanol as solvent, 170 W power, 60:1 solvent to solid ratio, 50 °C temperature and 60% duty cycle, amaximum extraction yi...

  12. Fully automated ionic liquid-based headspace single drop microextraction coupled to GC-MS/MS to determine musk fragrances in environmental water samples.

    Science.gov (United States)

    Vallecillos, Laura; Pocurull, Eva; Borrull, Francesc

    2012-09-15

    A fully automated ionic liquid-based headspace single drop microextraction (IL-HS-SDME) procedure has been developed for the first time to preconcentrate trace amounts of ten musk fragrances extensively used in personal care products (six polycyclic musks, three nitro musks and one polycyclic musk degradation product) from wastewater samples prior to analysis by gas chromatography and ion trap tandem mass spectrometry (GC-IT-MS/MS). Due to the low volatility of the ILs, a large internal diameter liner (3.4 mm i.d.) was used to improve the ILs evaporation. Furthermore, a piece of glass wool was introduced into the liner to avoid the entrance of the ILs in the GC column and a guard column was used to prevent analytical column damages. The main factors influencing the IL-HS-SDME were optimized. For all species, the highest enrichments factors were achieved using 1 μL of 1-octyl-3-methylimidazolium hexafluorophosphate ([OMIM][PF(6)]) ionic liquid exposed in the headspace of 10 mL water samples containing 300 g L(-1) of NaCl and stirred at 750 rpm and 60 °C for 45 min. All compounds were determined by direct injection GC-IT-MS/MS with a chromatographic time of 19 min. Method detection limits were found in the low ng mL(-1) range between 0.010 ng mL(-1) and 0.030 ng mL(-1) depending on the target analytes. Also, under optimized conditions, the method gave good levels of intra-day and inter-day repeatabilities in wastewater samples with relative standard deviations varying between 3% and 6% and 5% and 11%, respectively (n=3, 1 ng mL(-1)). The applicability of the method was tested with different wastewater samples from influent and effluent urban wastewater treatment plants (WWTPs) and one potable treatment plant (PTP). The analysis of influent urban wastewater revealed the presence of galaxolide and tonalide at concentrations of between 2.10 ng mL(-1) and 0.29 ng mL(-1) and 0.32 ng mL(-1) and MQL (Method Quantification Limit), respectively; while the remaining

  13. Application of Ultrasound-assisted Emulsification Microextraction ...

    African Journals Online (AJOL)

    Several factors influencing the extraction efficiency, such as the nature and volume of organic solvent, extraction temperature, ionic strength and centrifugation time, were investigated and optimized. Using optimum extraction conditions a detection limit of 0.1 μg L–1 and a good linearity in a calibration range of 0.25–250 μg ...

  14. Eco-friendly ionic liquid based ultrasonic assisted selective extraction coupled with a simple liquid chromatography for the reliable determination of acrylamide in food samples.

    Science.gov (United States)

    Albishri, Hassan M; El-Hady, Deia Abd

    2014-01-01

    Acrylamide in food has drawn worldwide attention since 2002 due to its neurotoxic and carcinogenic effects. These influences brought out the dual polar and non-polar characters of acrylamide as they enabled it to dissolve in aqueous blood medium or penetrate the non-polar plasma membrane. In the current work, a simple HPLC/UV system was used to reveal that the penetration of acrylamide in non-polar phase was stronger than its dissolution in polar phase. The presence of phosphate salts in the polar phase reduced the acrylamide interaction with the non-polar phase. Furthermore, an eco-friendly and costless coupling of the HPLC/UV with ionic liquid based ultrasonic assisted extraction (ILUAE) was developed to determine the acrylamide content in food samples. ILUAE was proposed for the efficient extraction of acrylamide from bread and potato chips samples. The extracts were obtained by soaking of potato chips and bread samples in 1.5 mol L(-1) 1-butyl-3-methylimmidazolium bromide (BMIMBr) for 30.0 and 60.0 min, respectively and subsequent chromatographic separation within 12.0 min using Luna C18 column and 100% water mobile phase with 0.5 mL min(-1) under 25 °C column temperature at 250 nm. The extraction and analysis of acrylamide could be achieved within 2h. The mean extraction efficiency of acrylamide showed adequate repeatability with relative standard deviation (RSD) of 4.5%. The limit of detection and limit of quantitation were 25.0 and 80.0 ng mL(-1), respectively. The accuracy of the proposed method was tested by recovery in seven food samples giving values ranged between 90.6% and 109.8%. Therefore, the methodology was successfully validated by official guidelines, indicating its reliability to be applied to analysis of real samples, proven to be useful for its intended purpose. Moreover, it served as a simple, eco-friendly and costless alternative method over hitherto reported ones. © 2013 Elsevier B.V. All rights reserved.

  15. Ultrasound-assisted anodization of aluminum in oxalic acid

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Rong; Jiang Kaiming [Department of Physics, Shanghai Maritime University, 1550 Pudong Avenue, Shanghai 200135 (China); Zhu Yun [State Key Laboratory of Functional Materials for Informatics, Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences, 865 Changning Road, Shanghai 200050 (China); Qi Haiyang [Department of Physics, Shanghai Maritime University, 1550 Pudong Avenue, Shanghai 200135 (China); Ding Guqiao, E-mail: gqding@mail.sim.ac.cn [State Key Laboratory of Functional Materials for Informatics, Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences, 865 Changning Road, Shanghai 200050 (China)

    2011-10-15

    Porous anodic alumina is an important nanoscale template for fabrication of various nanostructures. We report a new ultrasound-assisted anodization process in oxalic acid. Under the continuous irradiation of ultrasound, the one-step-anodized sample has a smooth and clean surface, and two-step-anodization brings ordered porous anodic alumina with higher growth rate of 52 {mu}m/h. The ultrasound applied during the anodization can clean the surface and enhance the nanopore growth since it can accelerate the oxide dissolving on the electrolyte/oxide interface. The ultrasound-assisted anodization may be utilized for other anodizations.

  16. Cu(II complexes of an ionic liquid-based Schiff base [1-{2-(2-hydroxy benzylidene amino ethyl}-3-methyl­imidazolium]Pf6: Synthesis, characterization and biological activities

    Directory of Open Access Journals (Sweden)

    Saha Sanjoy

    2015-01-01

    Full Text Available Two Cu(II complexes of an ionic liquid based Schiff base 1-{2-(2-hydroxybenzylideneamino ethyl}-3-methylimidazolium hexaflurophosphate, were prepared and characterized by different analytical and spectroscopic methods such as elemental analysis, magnetic susceptibility, UV-Vis, IR, NMR and mass spectroscopy. The Schiff base ligand was found to act as a potential bidentate chelating ligand with N, O donor sites and formed 1:2 metal chelates with Cu(II salts. The synthesized Cu(II complexes were tested for biological activity.

  17. The ultrasound-assisted aqueous extraction of rice bran oil.

    Science.gov (United States)

    Khoei, Maryam; Chekin, Fereshteh

    2016-03-01

    In this work, aqueous extraction of rice bran oil was done without and with ultrasound pretreatment. Key factors controlling the extraction and optimal operating conditions were identified. The highest extraction efficiency was found at pH=12, temperature of 45°C, agitation speed of 800rpm and agitation time of 15min, ultrasound treatment time of 70min and ultrasound treatment temperature of 25°C. Moreover, extraction yields were compared to ultrasound-assisted aqueous extraction and Soxhlet extraction. The results showed that the yield of rice bran oil at ultrasound-assisted aqueous extraction was close to the yield of oil extracted by hexane Soxhlet extraction. This result implied that the yield of rice bran oil was significantly influenced by ultrasound. With regard to quality, the oil extracted by ultrasound-assisted aqueous process had a lower content of free fatty acid and lower color imparting components than the hexane-extracted oil. Also, effect of parboiling of paddy on hexane and ultrasound-assisted aqueous extraction was studied. Both extraction methods gives higher percentage of oil from par boiled rice bran compared with raw rice bran. This may be due to the fact that parboiling releases the oil. Copyright © 2015 Elsevier Ltd. All rights reserved.

  18. KINETICS OF ULTRASOUND ASSISTED EXTRACTION OF WEDELOLACTONE FROM Eclipta alba

    Directory of Open Access Journals (Sweden)

    T. W. Charpe

    Full Text Available Abstract Ultrasound assisted extraction of wedelolactone, a major coumestan present in Eclipta alba, is investigated in the present work.Various process parameters such as type of solvent, power, solvent to solid ratio and extraction temperature, which affect the extraction yield, are optimized. In the ultrasound-assisted extraction with final optimized conditions, i.e., methanol as solvent, 170 W power, 60:1 solvent to solid ratio, 50 °C temperature and 60% duty cycle, amaximum extraction yieldof 0.62 mg/g is obtained in 45 minutes. The kinetic model (Peleg's model has been used for the prediction of the yield of wedelolactone in the extract at a given time for all experimental conditions. The values of predicted yields show good agreement with the experimental data for all parameters, i.e., power, solvent to solid ratio and temperature. The extraction of wedelolactone from Eclipta alba is also carried out by conventional extraction methods, i.e., Soxhlet and batch extraction. Ultrasound-assisted extraction gives higher extraction yield in less time as compared to batch extraction (0.41 mg/g in 90 min and Soxhlet extraction(0.7 mg/g in 360 min. The ultrasound-assisted extraction of wedelolactone from Eclipta alba is an effective way of extraction with the advantages of lower time and higher extraction.

  19. Optimization of ultrasound-assisted extraction of total phenol from ...

    African Journals Online (AJOL)

    Optimization of the ultrasound-assisted extraction technology for total phenol from betel (Areca catechu L.) nut seed was carried out. On the basis of one factor tests, the method of response surface analysis with 3 factors including extracting temperature, time and solvent-material ratio on the content of total phenol was ...

  20. A green ionic liquid-based vortex-forced MSPD method for the simultaneous determination of 5-HMF and iridoid glycosides from Fructus Corni by ultra-high performance liquid chromatography.

    Science.gov (United States)

    Du, Kunze; Li, Jin; Bai, Yun; An, Mingrui; Gao, Xiu-Mei; Chang, Yan-Xu

    2018-04-01

    A simple and green ionic liquid-based vortex-forced matrix solid phase dispersion (IL-VFMSPD) method was presented to simultaneously extract 5-hydroxymethyl furfurol (5-HMF) and iridoid glycosides in Fructus Corni by ultra-high performance liquid chromatography. Ionic liquid was used as a green elution reagent in vortex-forced MSPD process. A few parameters such as the type of ionic liquid, the type of sorbent, ratio of sample to sorbent, the concentration and volume of ionic liquid, grinding time and vortex time, were investigated in detail and an orthogonal design experiment was introduced to confirm the best conditions in this procedure. With the final optimized method, the recoveries of the target compounds in Fructus Corni were in the range of 95.2-103% (RSD<5.0%) and the method displayed a good linearity within the range of 0.8-200 μg mL -1 for morroniside, sweroside, loganin, cornuside and 1.2-300 μg mL -1 for 5-HMF. The limits of detection ranged from 0.02 to 0.08 μg mL -1 for all compounds. The results showed that the newly established method was efficiently applied to extract and determine iridoid glycosides and 5-HMF for quality control of Fructus Corni. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Ionic Liquid-Based Vacuum Microwave-Assisted Extraction Followed by Macroporous Resin Enrichment for the Separation of the Three Glycosides Salicin, Hyperin and Rutin from Populus Bark

    OpenAIRE

    Fengli Chen; Kailin Mo; Zhaizhi Liu; Fengjian Yang; Kexin Hou; Shuangyang Li; Yuangang Zu; Lei Yang

    2014-01-01

    An effective ionic liquid vacuum microwave-assisted method was developed for extraction of the thermo- and oxygen-sensitive glycosides salicin, hyperin and rutin from Populus bark due to the strong solvating effects of ionic liquids on plant cell walls. In this study, [C4mim]BF4 solution was selected as the extracting solution for extraction of the target analytes. After optimization by single factor experiments and response surface methodology, the optimum condition parameters were achieved,...

  2. Ultrasound assisted extraction of polyphenols from Punica granatum (Grenada) fruit

    International Nuclear Information System (INIS)

    Rodriguez Chanfrau, Jorge Enrique; Lopez Armas, Marilyn

    2014-01-01

    Extraction of bioactive compounds from vegetable materials is a classical operation applied in many industrial processes. Few studies have made reference to processes to obtain extracts from Punica granatum. This fruit is generally consumed as such or as fermented juices. In Cuba, it is known as grenade and numerous studies have shown antiviral, antioxidant and antimicrobial properties. Maceration process is the main used technology in the preparation of extracts from Punica granatum fruit, being this a long and expensive process. Ultrasound-assisted extractions have been proven to significantly decreased extraction time and increased extraction yields in many vegetable materials. However, few papers report the use of this methodology in the extraction processes of Punica granatum. To evaluate an ultrasound-assisted extraction process to extract polyphenols from Punica granatum fruit

  3. Extraction and Chromatographic Determination of Shikimic Acid in Chinese Conifer Needles with 1-Benzyl-3-methylimidazolium Bromide Ionic Liquid Aqueous Solutions

    Science.gov (United States)

    Chen, Fengli; Hou, Kexin; Li, Shuangyang; Zu, Yuangang; Yang, Lei

    2014-01-01

    An ionic liquids-based ultrasound-assisted extraction (ILUAE) method was successfully developed for extracting shikimic acid from conifer needles. Eleven 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were investigated and 1-benzyl-3-methylimidazolium bromide solution was selected as the solvent. The conditions for ILUAE, including the ionic liquid concentration, ultrasound power, ultrasound time, and liquid-solid ratio, were optimized. The proposed method had good recovery (99.37%–100.11%) and reproducibility (RSD, n = 6; 3.6%). ILUAE was an efficient, rapid, and simple sample preparation technique that showed high reproducibility. Based on the results, a number of plant species, namely, Picea koraiensis, Picea meyeri, Pinus elliottii, and Pinus banksiana, were identified as among the best resources of shikimic acid. PMID:24782942

  4. Ionic liquid-based dispersive liquid-liquid microextraction combined with high performance liquid chromatography-UV detection for simultaneous preconcentration and determination of Ni, Co, Cu and Zn in water samples

    Directory of Open Access Journals (Sweden)

    Asghari Alireza

    2014-01-01

    Full Text Available Ionic liquid-based dispersive liquid-liquid microextraction (IL-DLLME coupled with high performance liquid chromatography (HPLC-UV detection was developed for simultaneous extraction and determination of nickel, cobalt, copper and zinc ions. In the proposed approach, salophen (N,N'-bis(salisyliden-1,2-phenylenediamine was used as a chelating agent; the ionic liquid, 1-hexeyl-3-methylimidazolium hexafluorophosphate, and acetone were selected as extracting and dispersive solvents, respectively. After extraction, phase separation was performed by centrifugation and the sedimented phase (ionic liquid was solubilized in acetonitrile and directly injected into the HPLC for subsequent analysis. Baseline separation of metal ion complexes was achieved on a RP-C18 column using a gradient elution of the mixtures of methanol-acetonitrile-water as the mobile phase at a flow rate of 1.0 mL min-1. The influence of variables such as sample pH, concentration of the chelating agent, amount of ionic liquid (extraction solvent, disperser solvent volume, extraction time, salt effect and centrifugation speed were studied and optimized. Under the optimum conditions, the enrichment factor of 222 was obtained. The detection limits for Ni, Co, Cu and Zn were 0.8, 1.6, 1.9 and 2.8 μg L−1, respectively. The relative standard deviations (RSDs were in the range of 3.6-5.0 % for all of the investigated metal ions. The proposed procedure was successfully applied to the determination of the studied metal ions in water samples.

  5. Ionic liquid-based vacuum microwave-assisted extraction followed by macroporous resin enrichment for the separation of the three glycosides salicin, hyperin and rutin from Populus bark.

    Science.gov (United States)

    Chen, Fengli; Mo, Kailin; Liu, Zhaizhi; Yang, Fengjian; Hou, Kexin; Li, Shuangyang; Zu, Yuangang; Yang, Lei

    2014-07-07

    An effective ionic liquid vacuum microwave-assisted method was developed for extraction of the thermo- and oxygen-sensitive glycosides salicin, hyperin and rutin from Populus bark due to the strong solvating effects of ionic liquids on plant cell walls. In this study, [C4mim]BF4 solution was selected as the extracting solution for extraction of the target analytes. After optimization by single factor experiments and response surface methodology, the optimum condition parameters were achieved, which included 1.0 M [C4mim]BF4, 2 h soaking time, -0.08 MPa vacuum, 20 min microwave irradiation time, 400 W microwave irradiation power and 25 mL/g liquid/solid ratio. Under the optimum conditions, higher extraction yields of salicin (35.53 mg/g), hyperin (1.32 mg/g) and rutin (2.40 mg/g) were obtained. Compared with other extraction methods, the developed method provided higher yields of the three target components after a relatively shorter extraction time (20 min). No obvious degradation of the target analytes was observed under the optimum conditions in performed stability studies and the proposed method had a high reproducibility. Meanwhile, after adsorption and desorption on macroporous D101 resin, the target analytes can be effectively separated from the [C4mim]BF4 ionic liquid extraction solution and the yields of salicin, hyperin and rutin were 89%, 82% and 84%, respectively. The recovered [C4mim]BF4 ionic liquid presented a good extraction effect on the three analytes after recycling five times.

  6. Ionic Liquid-Based Vacuum Microwave-Assisted Extraction Followed by Macroporous Resin Enrichment for the Separation of the Three Glycosides Salicin, Hyperin and Rutin from Populus Bark

    Directory of Open Access Journals (Sweden)

    Fengli Chen

    2014-07-01

    Full Text Available An effective ionic liquid vacuum microwave-assisted method was developed for extraction of the thermo- and oxygen-sensitive glycosides salicin, hyperin and rutin from Populus bark due to the strong solvating effects of ionic liquids on plant cell walls. In this study, [C4mim]BF4 solution was selected as the extracting solution for extraction of the target analytes. After optimization by single factor experiments and response surface methodology, the optimum condition parameters were achieved, which included 1.0 M [C4mim]BF4, 2 h soaking time, −0.08 MPa vacuum, 20 min microwave irradiation time, 400 W microwave irradiation power and 25 mL/g liquid/solid ratio. Under the optimum conditions, higher extraction yields of salicin (35.53 mg/g, hyperin (1.32 mg/g and rutin (2.40 mg/g were obtained. Compared with other extraction methods, the developed method provided higher yields of the three target components after a relatively shorter extraction time (20 min. No obvious degradation of the target analytes was observed under the optimum conditions in performed stability studies and the proposed method had a high reproducibility. Meanwhile, after adsorption and desorption on macroporous D101 resin, the target analytes can be effectively separated from the [C4mim]BF4 ionic liquid extraction solution and the yields of salicin, hyperin and rutin were 89%, 82% and 84%, respectively. The recovered [C4mim]BF4 ionic liquid presented a good extraction effect on the three analytes after recycling five times.

  7. Design and synthesis of new family of ionic liquids based on 2-iminium-1,3-dithiolanes: A combined theoretical and experimental effort

    Science.gov (United States)

    Ziyaei Halimehjani, Azim; Shakourian-Fard, Mehdi; Farvardin, Marziye Vahdati; Raeesi, Mozhgan; Hashemi, Mohammed Mahmoodi; Behzadi, Hadi

    2014-01-01

    An efficient method for synthesis of 2-iminium-1,3-dithiolane as a new family of ionic liquids with reaction of dithiocarbamates with methyl triflouromethanesulfonate was described. Theoretical study on the synthesized ionic liquids was also performed by quantum chemistry calculation. Geometry optimization on the ion pairs was carried out with the B3LYP/6-311++G(d,p) level of theory. The interaction energies were calculated, and corrected by the basis set superposition error (BSSE) calculated by the counterpoise method. The results of natural bond orbital (NBO) and quantum theory of atoms in molecules (QTAIM) analyses indicate that the interactions occur via hydrogen bonding between oxygen atom lone pairs (lp(O)) of triflouromethanesulfonate anion and antibonding orbitals of σ*C-H of 2-iminium-1,3-dithiolane cations. Also, the results of QTAIM analysis show that the hydrogen bonds are closed shell (electrostatic) in the nature. Finally, the 1H and 13C calculated chemical shifts at the B3LYP/6-311++G** level were in agreement with experimental chemical shifts for synthesized ionic liquids.

  8. Influence of reaction conditions on formation of ionic liquid-based nanostructured Bi2O3 as an efficient visible-light-driven photocatalyst

    Science.gov (United States)

    Bagheri, Mozhgan; Heydari, Mojgan; Vaezi, Mohammad Reza

    2018-01-01

    In this study, nanostructured bismuth oxide was synthesized based on the chemical reaction of bismuth nitrate and NaOH in the ionic liquid 1-butyl-3-methylimidazolium chloride ([C4mim]Cl) under ultrasonic irradiation. The effect of sodium hydroxide with a different molar ratio of NaOH to bismuth in the range of 3-10 was investigated. The results of fourier-transform infrared spectroscopy (FT-IR) and X-ray powder diffraction (XRD) showed that NaOH has a critical role in the formation of pure α-Bi2O3. So, at high concentrations of NaOH (NaOH:Bi ≥ 7.5), the chloride anion from the ionic liquid cannot be entered into the crystalline structure of bismuth oxide, which resulted in the formation of pure bismuth oxide, while at lower concentrations of NaOH (NaOH:Bi ≤ 5), Bi3O4Cl was formed with a layered structure. The XRD results revealed that the synthesized α-Bi2O3 has a monoclinic structure and scanning electron microscopy (SEM) images showed that the sample consists of needle like particles with an average thickness of 50 nm. The ionic liquid has an important role in the prevention of an agglomeration of particles in the Bi2O3 sample. The photocatalytic activity of the synthesized Bi2O3 was investigated to study the degradation of malachite green dye as a model pollutant under visible light. The effects of various parameters such as the pH, concentration of the dye, and the catalyst on the degradation of malachite green were also investigated.

  9. Trace determination of volatile polycyclic aromatic hydrocarbons in natural waters by magnetic ionic liquid-based stir bar dispersive liquid microextraction.

    Science.gov (United States)

    Benedé, Juan L; Anderson, Jared L; Chisvert, Alberto

    2018-01-01

    In this work, a novel hybrid approach called stir bar dispersive liquid microextraction (SBDLME) that combines the advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) has been employed for the accurate and sensitive determination of ten polycyclic aromatic hydrocarbons (PAHs) in natural water samples. The extraction is carried out using a neodymium stir bar magnetically coated with a magnetic ionic liquid (MIL) as extraction device, in such a way that the MIL is dispersed into the solution at high stirring rates. Once the stirring is ceased, the MIL is magnetically retrieved onto the stir bar, and subsequently subjected to thermal desorption (TD) coupled to a gas chromatography-mass spectrometry (GC-MS) system. The main parameters involved in TD, as well as in the extraction step affecting the extraction efficiency (i.e., MIL amount, extraction time and ionic strength) were evaluated. Under the optimized conditions, the method was successfully validated showing good linearity, limits of detection and quantification in the low ng L -1 level, good intra- and inter-day repeatability (RSD < 13%) and good enrichment factors (18 - 717). This sensitive analytical method was applied to the determination of trace amounts of PAHs in three natural water samples (river, tap and rainwater) with satisfactory relative recovery values (84-115%), highlighting that the matrices under consideration do not affect the extraction process. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Room temperature ionic liquid-based microextraction for vanadium species separation and determination in water samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Berton, Paula; Martinis, Estefania M. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT-CONICET-Mendoza), Av. Ruiz Leal S/N Parque General San Martin, CC. 131, M 5502 IRA Mendoza (Argentina); Martinez, Luis D. [INQUISAL-CONICET, Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gov.ar [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT-CONICET-Mendoza), Av. Ruiz Leal S/N Parque General San Martin, CC. 131, M 5502 IRA Mendoza (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)

    2009-04-27

    A simple microextraction technique based on room temperature ionic liquids (RTILs) for trace V(IV) and V(V) species separation and preconcentration in water samples was developed in this work. Vanadium species microextraction was achieved with a minimal amount of the RTIL 1-butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}mim][PF{sub 6}]) as vanadium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (V-5-Br-PADAP) complex. The speciation analysis was performed based on a modern technique defined as temperature-controlled ionic liquid dispersive liquid phase microextraction (TILDLME). The level of V(IV) species was calculated by difference of total V and V(V) levels. Selectivity among V species was obtained with the use of 1,2-cyclohexanediaminetetraacetic acid (CDTA) as masking agent. Determination of V was developed by direct injection of the RTIL phase into the electrothermal atomic absorption spectrometer (ETAAS). A preconcentration factor of 40 was achieved with only 2 mL of sample. The limit of detection (LOD) obtained under optimum conditions was 4.9 ng L{sup -1} and the relative standard deviation for 10 replicate determinations at the 0.5 {mu}g L{sup -1} V level was 4.3%, calculated at peak heights. A correlation coefficient of 0.9961 was achieved. The method was successfully applied for the speciation analysis of V in tap and river water samples.

  11. Separators for Li-Ion and Li-Metal Battery Including Ionic Liquid Based Electrolytes Based on the TFSI− and FSI− Anions

    Directory of Open Access Journals (Sweden)

    Marija Kirchhöfer

    2014-08-01

    Full Text Available The characterization of separators for Li-ion or Li-metal batteries incorporating hydrophobic ionic liquid electrolytes is reported herein. Ionic liquids made of N-butyl-N-methylpyrrolidinium (PYR14+ or N-methoxyethyl-N-methylpyrrolidinium (PYR12O1+, paired with bis(trifluoromethanesulfonylimide (TFSI− or bis(fluorosulfonylimide (FSI− anions, were tested in combination with separators having different chemistries and morphologies in terms of wetting behavior, Gurley and McMullin number, as well as Li/(Separator + Electrolyte interfacial properties. It is shown that non-functionalized microporous polyolefin separators are poorly wetted by FSI−-based electrolytes (contrary to TFSI−-based electrolytes, while the ceramic coated separator Separion® allows good wetting with all electrolytes. Furthermore, by comparing the lithium solid electrolyte interphase (SEI resistance evolution at open circuit and during cycling, depending on separator morphologies and chemistries, it is possible to propose a scale for SEI forming properties in the order: PYR12O1FSI > PYR14FSI > PYR14TFSI > PYR12O1TFSI. Finally, the impact the separator morphology is evidenced by the SEI resistance evolution and by comparing Li electrodes cycled using separators with two different morphologies.

  12. Highly efficient extraction and selective separation of uranium (VI) from transition metals using new class of undiluted ionic liquids based on H-phosphonate anions.

    Science.gov (United States)

    Zarrougui, Ramzi; Mdimagh, Raouf; Raouafi, Nourreddine

    2018-01-15

    In this paper, we report the development of an environmental friendly process to decontaminate uranium-containing ores and nuclear wastes by using non-fluorinated ionic liquids (ILs). The main advantages of this extraction process are the absence of any organic diluent and extra extraction agents added to the organic phase. Moreover, the process is cost-effective and maybe applied as a sustainable hydrometallurgical method to recover uranium. The distribution ratio (D U ) and the extraction efficiency (%E) of uranium(VI) (UO 2 2+ ) were found to be dependent on the acidity of the aqueous phase, the extraction time, the alkyl chain length in the ILs, the concentration of the aqueous feed and molar quantity of ILs. The D U value is higher than 600 and the %E is equal to 98.6% when [HNO 3 ]=7M. The extraction reactions follows a neutral partition or ionic exchange mechanism depending on nitric acid concentration. The nature of bonding in the extracted complexes was investigated by spectroscopic techniques. The potential use of Mor 1-8 -OP for the separation of UO 2 2+ from a mixture containing transition metal ions M n+ was also examined. The UO 2 2+ ions were separated and extracted efficiently. These ILs are promising candidates for the recovery and separation of uranium. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. An Approach to Solid-State Electrical Double Layer Capacitors Fabricated with Graphene Oxide-Doped, Ionic Liquid-Based Solid Copolymer Electrolytes

    Directory of Open Access Journals (Sweden)

    N. F. A. Fattah

    2016-06-01

    Full Text Available Solid polymer electrolyte (SPE composed of semi-crystalline poly (vinylidene fluoride-hexafluoropropylene [P(VdF-HFP] copolymer, 1-ethyl-3-methylimidazolium bis (trifluoromethyl sulphonyl imide [EMI-BTI] and graphene oxide (GO was prepared and its performance evaluated. The effects of GO nano-filler were investigated in terms of enhancement in ionic conductivity along with the electrochemical properties of its electrical double layer capacitors (EDLC. The GO-doped SPE shows improvement in ionic conductivity compared to the P(VdF-HFP-[EMI-BTI] SPE system due to the existence of the abundant oxygen-containing functional group in GO that assists in the improvement of the ion mobility in the polymer matrix. The complexation of the materials in the SPE is confirmed in X-ray diffraction (XRD and thermogravimetric analysis (TGA studies. The electrochemical performance of EDLC fabricated with GO-doped SPE is examined using cyclic voltammetry and charge–discharge techniques. The maximum specific capacitance obtained is 29.6 F∙g−1, which is observed at a scan rate of 3 mV/s in 6 wt % GO-doped, SPE-based EDLC. It also has excellent cyclic retention as it is able keep the performance of the EDLC at 94% even after 3000 cycles. These results suggest GO doped SPE plays a significant role in energy storage application.

  14. Comparison of micellar extraction combined with ionic liquid based vortex-assisted liquid-liquid microextraction and modified quick, easy, cheap, effective, rugged, and safe method for the determination of difenoconazole in cowpea.

    Science.gov (United States)

    Chen, Xiaochu; Bian, Yanli; Liu, Fengmao; Teng, Peipei; Sun, Pan

    2017-10-06

    Two simple sample pretreatment for the determination of difenoconazole in cowpea was developed including micellar extraction combined with ionic liquid based vortex-assisted liquid-liquid microextraction (ME-IL-VALLME) prior to high performance liquid chromatography (HPLC), and modified quick, easy, cheap, effective, rugged, and safe method (QuEChERS) coupled with HPLC-MS/MS. In ME-IL-VALLME method, the target analyte was extracted by surfactant Tween 20 micellar solution, then the supernatant was diluted with 3mL water to decrease the solubility of micellar solution. Subsequently, the vortex-assisted liquid-liquid microextraction (VALLME) procedure was performed in the diluted extraction solution by using the ionic liquid of 1-hexyl-3-methylimidazolium hexafluorophosphate ([HMIM]PF 6 ) as the extraction solvent and Tween 20 as an emulsifier to enhance the dispersion of the water-immiscible ionic liquid into the aqueous phase. Parameters that affect the extraction have been investigated in both methods Under the optimum conditions, the limits of quantitation were 0.10 and 0.05mgkg -1 , respectively. And good linearity was achieved with the correlation coefficient higher than 0.9941. The relative recoveries ranged from 78.6 to 94.8% and 92.0 to 118.0% with the relative standard deviations (RSD) of 7.9-9.6% and 1.2-3.2%, respectively. Both methods were quick, simple and inexpensive. However, the ME-IL-VALLME method provides higher enrichment factor compared with conventional QuEChERS method. The ME-IL-VALLME method has a strong potential for the determination of difenoconazole in complex vegetable matrices with HPLC. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Ultrasound assisted manufacturing of paraffin wax nanoemulsions: process optimization.

    Science.gov (United States)

    Jadhav, A J; Holkar, C R; Karekar, S E; Pinjari, D V; Pandit, A B

    2015-03-01

    This work reports on the process optimization of ultrasound-assisted, paraffin wax in water nanoemulsions, stabilized by modified sodium dodecyl sulfate (SDS). This work focuses on the optimization of major emulsification process variables including sonication time, applied power and surfactant concentration. The effects of these variables were investigated on the basis of mean droplet diameter and stability of the prepared emulsion. It was found that the stable emulsion with droplet diameters about 160.9 nm could be formed with the surfactant concentration of 10 mg/ml and treated at 40% of applied power (power density: 0.61 W/ml) for 15 min. Scanning electron microscopy (SEM) was used to study the morphology of the emulsion droplets. The droplets were solid at room temperature, showing bright spots under polarized light and a spherical shape under SEM. The electrophoretic properties of emulsion droplets showed a negative zeta potential due to the adsorption of head sulfate groups of the SDS surfactant. For the sake of comparison, paraffin wax emulsion was prepared via emulsion inversion point method and was checked its intrinsic stability. Visually, it was found that the emulsion get separated/creamed within 30 min. while the emulsion prepared via ultrasonically is stable for more than 3 months. From this study, it was found that the ultrasound-assisted emulsification process could be successfully used for the preparation of stable paraffin wax nanoemulsions.

  16. A lipophilic ionic liquid based on formamidinium cations and TFSI: the electric response and the effect of CO2on the conductivity mechanism.

    Science.gov (United States)

    Bertasi, Federico; Giffin, Guinevere A; Vezzù, Keti; Pace, Giuseppe; Abu-Lebdeh, Yaser; Armand, Michel; Di Noto, Vito

    2017-10-04

    This work describes the preparation of the new lipophilic ionic liquid tetraoctyl-formamidinium bis(trifluoromethanesulfonyl) imide (TOFATFSI), which is miscible with lower alkanes. In particular, this work focuses on the electric behaviour of TOFATFSI in the particularly challenging highly apolar environment of supercritical CO 2 . The conductivity and relaxation phenomena are revealed through the analysis of the broadband electric spectra with a particular emphasis on the effect of temperature and CO 2 uptake on the IL conductivity. It is found that temperature boosts the conductivity via an increase in the charge carrier mobility. Also, CO 2 absorption affects both the conductivity and the permittivity of the material due to the presence of CO 2 -IL interactions that modulate the nanostructure and the size of the TOFATFSI aggregates, which increases both the mobility and the density of the charge carriers.

  17. Separation of curcuminoids using ionic liquid based aqueous two-phase system coupled with in situ dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Shu, Yang; Gao, Mingcen; Wang, Xueying; Song, Rusheng; Lu, Jun; Chen, Xuwei

    2016-01-01

    An aqueous two-phase extraction system (ATPS) combined with an in situ dispersive liquid-liquid microextraction (DLLME) method using imidazolium ionic liquids (ILs) for the separation of curcuminoids is developed. The influence of structure of IL, the type of metathesis reagents, and the back extraction agents on the extraction efficiency is investigated. 2.0mg of curcuminoids are extracted by an IL ATPS composed of 0.4g 1,3-diethylimidazolium iodine (EeimI), 0.6g potassium hydrogen phosphate, 1.0g water. Then the bis[(trifluoromethyl)sulfonyl]imide lithium (LiNTf2) aqueous solution is added to the EeimI-rich phase of the ATPS. The water-immiscible ionic liquids, 1,3-diethylimidazole bis[(trifluoromethyl)sulfonyl]imide (EeimNTf2), forms by the metathesis reaction. The in situ DLLME is triggered simultaneously and further purifies the curcuminoids. 92% of EeimI transforms into EeimNTf2 and thus the Eeim(+) cation is used for twice in this method. Finally, 0.1mol/L NaOH aqueous solution is used as the back extraction reagent. The curcuminoids precipitate is achieved with 93% of recovery when the aqueous solution is adjusted to pH 3.0. This ATPS-DLLME method is successfully applied to the separation of curcuminoids from Curcuma Longa (0.96±0.02% of extraction yield, a purity of >51% with respect to the total dry mass of the product). Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Temperature controlled ionic liquid-based dispersive micro-extraction using two ligands, for determination of aluminium in scalp hair samples of Alzheimer's patients: A multivariate study

    Science.gov (United States)

    Arain, Mariam S.; Arain, Salma A.; Kazi, Tasneem G.; Afridi, Hassan I.; Ali, Jamshaid; Naeemulllah; Arain, Sadaf S.; Brahman, Kapil Dev; Mughal, Moina Akhtar

    2015-02-01

    A green and sensitive temperature controlled dispersive liquid-liquid microextraction (TIL-DLLME) methodology based on the application of ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate, [C4mim][PF6], as an extractant solvent was proposed for the preconcentration of trace levels of aluminium (Al3+) in scalp hair samples of Alzheimer's (AD) patients, prior to analyzing by flame atomic absorption spectrometry (FAAS). The Al3+ was complexed with 8-hydrooxyquinoline (oxine) (L1) and 3,5,7,2‧-4‧ pentahydroxy flavone (morin) (L2) separately and then extracted by IL at temperature (50 ± 2.0 °C). Some effective factors that influence the TIL-DLLME efficiency such as pH, ligands concentrations, volume of IL, ionic strength, and incubation time were investigated and optimized by multivariate analysis. In the optimum experimental conditions, the limit of detection (3 s) and enhancement factor were 0.56 μg L-1, 0.64 μg L-1 and 85, 73 for both ligands, respectively. The relative standard deviation (RSD) for six replicate determinations of 100 μg L-1 Al3+ complexed with oxine and morin were found to be 3.88% and 4.74%, respectively. The developed method was validated by the analysis of certified reference material of human hair (NCSZC81002).and applied satisfactorily to the determination of Al3+ in acid digested scalp hair samples of AD patients and healthy controls. The resulted data shows significant higher level in scalp hair samples of AD male patients with related to referents of same age and socioeconomic status.

  19. Iron species determination by task-specific ionic liquid-based in situ solvent formation dispersive liquid-liquid microextraction combined with flame atomic absorption spectrometry.

    Science.gov (United States)

    Sadeghi, Susan; Ashoori, Vahid

    2017-10-01

    The task-specific ionic liquid (TSIL) of 1-ethyl-3-methylimidazolium bromide functionalized with 8-hydroxyquinoline was used as a chelating agent and extracting solvent for dispersive liquid-liquid microextraction and subsequent determination of Fe(III) by flame atomic absorption spectrometry. The in situ solvent formation of TSIL using KPF 6 provided the desired water-immiscible ionic liquid. The total Fe concentration could be determined after pre-oxidation of Fe(II) to Fe(III). Various factors affecting the proposed extraction procedure were optimized. The proposed analytical conditions were: sample pH 5, TSIL amount 0.3% (w/v), KPF 6 amount 0.15% (w/v), anti-sticking 0.1% (w/v) and salt concentration 5% (w/v). Under optimal conditions, the linear dynamic ranges for Fe(III) and total Fe were 20-80 and 20-110 ng mL -1 , respectively, with a detection limit of 6.9 ng mL -1 for Fe(III) and relative standard deviation of 2.2%. The proposed method was successfully applied to the determination of trace Fe(III) in water (underground, tap, refined water and artificial sea water) and beverage (apple, tomato, and tea) samples. The developed method offers advantages such as simplicity, ease of operation, and extraction of Fe(III) from aqueous solutions without the use of organic solvent. It was successfully applied for iron speciation in different real samples. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  20. The Influence of Anion Shape on the Electrical Double Layer Microstructure and Capacitance of Ionic Liquids-Based Supercapacitors by Molecular Simulations

    Directory of Open Access Journals (Sweden)

    Ming Chen

    2017-02-01

    Full Text Available Room-temperature ionic liquids (RTILs are an emerging class of electrolytes for supercapacitors. In this work, we investigate the effects of different supercapacitor models and anion shape on the electrical double layers (EDLs of two different RTILs: 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonylimide ([Emim][Tf2N] and 1-ethyl-3-methylimidazolium 2-(cyanopyrrolide ([Emim][CNPyr] by molecular dynamics (MD simulation. The EDL microstructure is represented by number densities of cations and anions, and the potential drop near neutral and charged electrodes reveal that the supercapacitor model with a single electrode has the same EDL structure as the model with two opposite electrodes. Nevertheless, the employment of the one-electrode model without tuning the bulk density of RTILs is more time-saving in contrast to the two-electrode one. With the one-electrode model, our simulation demonstrated that the shapes of anions significantly imposed effects on the microstructure of EDLs. The EDL differential capacitance vs. potential (C-V curves of [Emim][CNPyr] electrolyte exhibit higher differential capacitance at positive potentials. The modeling study provides microscopic insight into the EDLs structure of RTILs with different anion shapes.

  1. Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based-preconcentration and flow injection-cold vapor atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Martinis, Estefania M.; Berton, Paula [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, CC. 131, M 5502 IRA Mendoza (Argentina); Olsina, Roberto A. [INQUISAL-CONICET, Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, San Luis (Argentina); Altamirano, Jorgelina C. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, CC. 131, M 5502 IRA Mendoza (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@lab.cricyt.edu.ar [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, CC. 131, M 5502 IRA Mendoza (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)

    2009-08-15

    A liquid-liquid extraction procedure (L-L) based on room temperature ionic liquid (RTIL) was developed for the preconcentration and determination of mercury in different water samples. The analyte was quantitatively extracted with 1-butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}mim][PF{sub 6}]) under the form of Hg-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Hg-5-Br-PADAP) complex. A volume of 500 {mu}l of 9.0 mol L{sup -1} hydrochloric acid was used to back-extract the analyte from the RTIL phase into an aqueous media prior to its analysis by flow injection-cold vapor atomic absorption spectrometry (FI-CV-AAS). A preconcentration factor of 36 was achieved upon preconcentration of 20 mL of sample. The limit of detection (LOD) obtained under the optimal conditions was 2.3 ng L{sup -1} and the relative standard deviation (RSD) for 10 replicates at 1 {mu}g L{sup -1} Hg{sup 2+} was 2.8%, calculated with peaks height. The method was successfully applied to the determination of mercury in river, sea, mineral and tap water samples and a certified reference material (CRM).

  2. Multi-elemental ionic liquid-based solvent bar micro-extraction of priority and emerging trace metallic pollutants (Cd, Ag, Pd) in natural waters.

    Science.gov (United States)

    Herce-Sesa, Belén; López-López, José A; Moreno, Carlos

    2018-02-12

    Transition metals Cd, Pd and Ag are toxic even at very low concentration. Cd is considered a priority substance; while, Pd and Ag are emerging pollutants. Membrane technologies have been applied for their extraction; however, they require important amounts of reagents, time and energy. Additionally, effective reagents for metal extraction in saline natural waters are limited. In this case, hollow fiber liquid phase micro-extraction with a configuration of solvent bar (SBME) using the ionic liquid Cyphos® 101 as extractant is proposed. Optimized conditions for SBME of Cd, Ag and Pd were 50% Cyphos® 101 in the organic solution, extraction time 30 min and 800 rpm stirring rate. Leaching was in all cases lower than 0.1%. Metallic concentrations were measured by flame atomic absorption spectroscopy. The method was applied to the extraction of Ag, Cd and Pd in natural water samples. Except for waste water, Pd extraction was higher than 90% in all cases. Cd (≈100%) and Ag (93-95%) offered their best results for saline samples. Concluding, the proposed system is a low cost and green methodology that allows a simple and fast extraction of trace pollutants such as Ag, Cd and Pd in different natural waters, including highly saline samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  3. Physically Gelled Room-Temperature Ionic Liquid-Based Composite Membranes for CO2/N-2 Separation: Effect of Composition and Thickness on Membrane Properties and Performance

    Energy Technology Data Exchange (ETDEWEB)

    Nguyen, PT; Voss, BA; Wiesenauer, EF; Gin, DL; Nobe, RD

    2013-07-03

    An aspartame-based, low molecular-weight organic gelator (LMOG) was used to form melt-infused and composite membranes with two different imidazolium-based room-temperature ionic liquids (RTILs) for CO2 separation from N-2. Previous work demonstrated that LMOGs can gel RTILs at low, loading levels, and this aspartame-based LMOG was selected because it has been reported to gel a large number of RTILs. The imidazolium-based RTILs were used because of their inherent good properties for CO2/light gas separations. Analysis of the resulting bulk RTIL/LMOG physical gels showed that these materials have high sol-gel transition temperatures (ca. 135 degrees C) suitable for flue gas applications. Gas permeabilities and burst pressure measurements of thick, melt infused membranes revealed a trade-off between high CO2 permeabilities and good mechanical stability as a function of the LMOG loading. Defect-free, composite membranes of the gelled RTILs were successfully fabricated by choosing an appropriate porous membrane support (hydrophobic PTFE) using a suitable coating technique (roller coating). The thicknesses of the applied composite gel layers ranged from 10.3 to 20.7 mu m, which represents an order of magnitude decrease in active layer thickness, compared to the original melt-infused gel RTIL membranes.

  4. Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based-preconcentration and flow injection-cold vapor atomic absorption spectrometry.

    Science.gov (United States)

    Martinis, Estefanía M; Bertón, Paula; Olsina, Roberto A; Altamirano, Jorgelina C; Wuilloud, Rodolfo G

    2009-08-15

    A liquid-liquid extraction procedure (L-L) based on room temperature ionic liquid (RTIL) was developed for the preconcentration and determination of mercury in different water samples. The analyte was quantitatively extracted with 1-butyl-3-methylimidazolium hexafluorophosphate ([C(4)mim][PF(6)]) under the form of Hg-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Hg-5-Br-PADAP) complex. A volume of 500 microl of 9.0 mol L(-1) hydrochloric acid was used to back-extract the analyte from the RTIL phase into an aqueous media prior to its analysis by flow injection-cold vapor atomic absorption spectrometry (FI-CV-AAS). A preconcentration factor of 36 was achieved upon preconcentration of 20 mL of sample. The limit of detection (LOD) obtained under the optimal conditions was 2.3ngL(-1) and the relative standard deviation (RSD) for 10 replicates at 1 microg L(-1) Hg(2+) was 2.8%, calculated with peaks height. The method was successfully applied to the determination of mercury in river, sea, mineral and tap water samples and a certified reference material (CRM).

  5. Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based-preconcentration and flow injection-cold vapor atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Martinis, Estefania M.; Berton, Paula; Olsina, Roberto A.; Altamirano, Jorgelina C.; Wuilloud, Rodolfo G.

    2009-01-01

    A liquid-liquid extraction procedure (L-L) based on room temperature ionic liquid (RTIL) was developed for the preconcentration and determination of mercury in different water samples. The analyte was quantitatively extracted with 1-butyl-3-methylimidazolium hexafluorophosphate ([C 4 mim][PF 6 ]) under the form of Hg-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Hg-5-Br-PADAP) complex. A volume of 500 μl of 9.0 mol L -1 hydrochloric acid was used to back-extract the analyte from the RTIL phase into an aqueous media prior to its analysis by flow injection-cold vapor atomic absorption spectrometry (FI-CV-AAS). A preconcentration factor of 36 was achieved upon preconcentration of 20 mL of sample. The limit of detection (LOD) obtained under the optimal conditions was 2.3 ng L -1 and the relative standard deviation (RSD) for 10 replicates at 1 μg L -1 Hg 2+ was 2.8%, calculated with peaks height. The method was successfully applied to the determination of mercury in river, sea, mineral and tap water samples and a certified reference material (CRM).

  6. Ionic liquid-based observation technique for nonconductive materials in the scanning electron microscope: Application to the characterization of a rare earth ore.

    Science.gov (United States)

    Brodusch, Nicolas; Waters, Kristian; Demers, Hendrix; Gauvin, Raynald

    2014-03-01

    A new approach for preparing geological materials is proposed to reduce charging during their characterization in a scanning electron microscope. This technique was applied to a sample of the Nechalacho rare earth deposit, which contains a significant amount of the minerals fergusonite and zircon. Instead of covering the specimen surface with a conductive coating, the sample was immersed in a dilute solution of ionic liquid and then air dried prior to SEM analysis. Imaging at a wide range of accelerating voltages was then possible without evidence of charging when using the in-chamber secondary and backscattered electrons detectors, even at 1 kV. High resolution x-ray and electron backscatter diffraction mapping were successfully obtained at 20 and 5 kV with negligible image drifting and permitted the characterization of the microstructure of the zircon/fergusonite-Y aggregates encased in the matrix minerals. Because of the absence of a conductive layer at the surface of the specimen, the Kikuchi band contrast was improved and the backscatter electron signal increased at both 5 and 20 kV as confirmed by Monte Carlo modeling. These major developments led to an improvement of the spatial resolution and efficiency of the above characterization techniques applied to the rare earth ore and it is expected that they can be applied to other types of ores and minerals. Copyright © 2014 Wiley Periodicals, Inc.

  7. Correlating coating characteristics with the performance of drug-coated balloons--a comparative in vitro investigation of own established hydrogel- and ionic liquid-based coating matrices.

    Directory of Open Access Journals (Sweden)

    Sebastian Kaule

    Full Text Available Drug-coated balloons (DCB, which have emerged as a therapeutic alternative to drug-eluting stents in percutaneous cardiovascular intervention, are well described with regard to clinical efficacy and safety within a number of clinical studies. In vitro studies elucidating the correlation between coating additive and DCB performance are however rare but considered important for the understanding of DCB requirements and the improvement of established DCB. In this regard, we examined three different DCB-systems, which were developed in former studies based on the ionic liquid cetylpyridinium salicylate, the body-own hydrogel hyaluronic acid and the pharmaceutically well-established hydrogel polyvinylpyrrolidone, considering coating morphology, coating thickness, drug-loss, drug-transfer to the vessel wall, residual drug-concentration on the balloon surface and entire drug-load during simulated use in an in vitro vessel model. Moreover, we investigated particle release of the different DCB during simulated use and determined the influence of the three coatings on the mechanical behavior of the balloon catheter. We could show that coating characteristics can be indeed correlated with the performance of DCB. For instance, paclitaxel incorporation in the matrix can reduce the drug wash-off and benefit a high drug transfer. Additionally, a thin coating with a smooth surface and high but delayed solubility can reduce drug wash-off and decrease particle burden. As a result, we suggest that it is very important to characterize DCB in terms of mentioned properties in vitro in addition to their clinical efficacy in order to better understand their function and provide more data for the clinicians to improve the tool of DCB in coronary angioplasty.

  8. Hydrogen Bonding, (1)H NMR, and Molecular Electron Density Topographical Characteristics of Ionic Liquids Based on Amino Acid Cations and Their Ester Derivatives.

    Science.gov (United States)

    Rao, Soniya S; Bejoy, Namitha Brijit; Gejji, Shridhar P

    2015-08-13

    Amino acid ionic liquids (AAILs) have attracted significant attention in the recent literature owing to their ubiquitous applications in diversifying areas of modern chemistry, materials science, and biosciences. The present work focuses on unraveling the molecular interactions underlying AAILs. Electronic structures of ion pairs consisting of amino acid cations ([AA(+)], AA = Gly, Ala, Val, Leu, Ile, Pro, Ser, Thr) and their ester substituted derivatives [AAE(+)] interacting with nitrate anion [NO3(-)] have been obtained from the dispersion corrected M06-2x density functional theory. The formation of ion pair is accompanied by the transfer of proton from quaternary nitrogen to anion facilitated via hydrogen bonding. The [Ile], [Pro], [Ser], and [Thr] and their esters reveal relatively strong inter- as well as intramolecular hydrogen-bonding interactions. Consequently, the hierarchy in binding energies of [AA][NO3] ion pairs and their ester analogues turns out to be [Gly] > [Ala] > [Ser] ∼ [Val] ∼ [Ile] > [Leu] ∼ [Thr] > [Pro]. The work underlines how the interplay of intra- as well as intermolecular hydrogen-bonding interactions in [AA]- and [AAE]-based ILs manifest in their infrared and (1)H NMR spectra. Substitution of -OCH3 functional group in [AA][NO3] ILs lowers the melting point attributed to weaker hydrogen-bonding interactions, making them suitable for room temperature applications. As opposed to gas phase structures, the presence of solvent (DMSO) does not bring about any proton transfer in the ion pairs or their ester analogues. Calculated (1)H NMR chemical shifts of the solvated structures agree well with those from experiment. Correlations of decomposition temperatures in [AA]- and [AAE]-based ILs with binding energies and electron densities at the bond critical point(s) in molecular electron density topography, have been established.

  9. Scaling-Up Ionic Liquid-Based Technologies: How Much Do We Care About Their Toxicity? Prima Facie Information on 1-Ethyl-3-Methylimidazolium Acetate.

    Science.gov (United States)

    Ostadjoo, Shaghayegh; Berton, Paula; Shamshina, Julia L; Rogers, Robin D

    2018-02-01

    The potential of the ionic liquid (IL) 1-ethyl-3-methylimidazolium acetate ([C2mim][OAc]) to dissolve a variety of biopolymers such as cellulose and chitin, makes it an attractive candidate for scaled-up industrial utilization. In fact, the first steps towards its use at industrial scale have been taken. This increases the urgency to fill the knowledge gaps in its toxicity and environmental impact in order to predict and control its environmental fate. In this mini-review, we discuss the available literature surrounding this key IL. The literature (through the analysis of toxicity of the anion and the cation separately) suggests that [C2mim][OAc] is a relatively safe choice for industrial applications. However, because the IL should be considered as a compound, with unique properties arising from the interactions between the ions, comprehensive toxicity information for this particular IL is still required. To decide, prima facie, if this IL is toxic or not, evaluation of its influence on human health and ecotoxicity is needed prior to its large scale utilization. We chose in this mini-review to focus on toxicity surrounding this IL and evaluate what is known and what is not. Here with all the information in hand, we hope that the urgent need for [C2mim][OAc] toxicological assessment before it can be used in numerous technologies is highlighted. In the near future, we expect that the assessment of toxicity and environmental fate and impact can be integrated directly into any research into the industrial utilization of this IL and any others contemplated for industrial application. © The Author 2017. Published by Oxford University Press on behalf of the Society of Toxicology. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com.

  10. The AHA Moment: Assessment of the Redox Stability of Ionic Liquids Based on Aromatic Heterocyclic Anions (AHAs) for Nuclear Separations and Electric Energy Storage.

    Science.gov (United States)

    Shkrob, Ilya A; Marin, Timothy W

    2015-11-19

    Because of their extended conjugated bond network, aromatic compounds generally have higher redox stability than less saturated compounds. We conjectured that ionic liquids (ILs) consisting of aromatic heterocyclic anions (AHAs) may exhibit improved radiation and electrochemical stability. Such properties are important in applications of these ILs as diluents in radionuclide separations and electrolytes in the electric energy storage devices. In this study, we systematically examine the redox chemistry of the AHAs. Three classes of these anions have been studied: (i) simple 5-atom ring AHAs, such as the pyrazolide and triazolides, (ii) AHAs containing an adjacent benzene ring, and (iii) AHAs containing electron-withdrawing groups that were introduced to reduce their basicity and interaction with metal ions. It is shown that fragmentation in the reduced and oxidized states of these AHAs does not generally occur, and the two main products, respectively, are the H atom adduct and the imidyl radical. The latter species occurs either as an N σ-radical or as an N π-radical, depending on the length of the N-N bond, and the state that is stabilized in the solid matrix is frequently different from that having the lowest energy in the gas phase. In some instances, the formation of the sandwich π-stack dimer radical anions has been observed. For trifluoromethylated anions, H adduct formation did not occur; instead, there was facile loss of fluoride from their fluorinated groups. The latter can be problematic in nuclear separations, but beneficial in batteries. Overall, our study suggests that AHA-based ILs are viable candidates for use as radiation-exposed diluents and electrolytes.

  11. 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. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Correlating Coating Characteristics with the Performance of Drug-Coated Balloons – A Comparative In Vitro Investigation of Own Established Hydrogel- and Ionic Liquid-Based Coating Matrices

    Science.gov (United States)

    Kaule, Sebastian; Minrath, Ingo; Stein, Florian; Kragl, Udo; Schmidt, Wolfram; Schmitz, Klaus-Peter; Sternberg, Katrin; Petersen, Svea

    2015-01-01

    Drug-coated balloons (DCB), which have emerged as a therapeutic alternative to drug-eluting stents in percutaneous cardiovascular intervention, are well described with regard to clinical efficacy and safety within a number of clinical studies. In vitro studies elucidating the correlation between coating additive and DCB performance are however rare but considered important for the understanding of DCB requirements and the improvement of established DCB. In this regard, we examined three different DCB-systems, which were developed in former studies based on the ionic liquid cetylpyridinium salicylate, the body-own hydrogel hyaluronic acid and the pharmaceutically well-established hydrogel polyvinylpyrrolidone, considering coating morphology, coating thickness, drug-loss, drug-transfer to the vessel wall, residual drug-concentration on the balloon surface and entire drug-load during simulated use in an in vitro vessel model. Moreover, we investigated particle release of the different DCB during simulated use and determined the influence of the three coatings on the mechanical behavior of the balloon catheter. We could show that coating characteristics can be indeed correlated with the performance of DCB. For instance, paclitaxel incorporation in the matrix can reduce the drug wash-off and benefit a high drug transfer. Additionally, a thin coating with a smooth surface and high but delayed solubility can reduce drug wash-off and decrease particle burden. As a result, we suggest that it is very important to characterize DCB in terms of mentioned properties in vitro in addition to their clinical efficacy in order to better understand their function and provide more data for the clinicians to improve the tool of DCB in coronary angioplasty. PMID:25734818

  13. Ultrasound-Assisted Extraction of Stilbenes from Grape Canes

    Directory of Open Access Journals (Sweden)

    Zulema Piñeiro

    2016-06-01

    Full Text Available An analytical ultrasound-assisted extraction (UAE method has been optimized and validated for the rapid extraction of stilbenes from grape canes. The influence of sample pre-treatment (oven or freeze-drying and several extraction variables (solvent, sample-solvent ratio and extraction time between others on the extraction process were analyzed. The new method allowed the main stilbenes in grape canes to be extracted in just 10 min, with an extraction temperature of 75 °C and 60% ethanol in water as the extraction solvent. Validation of the extraction method was based on analytical properties. The resulting RSDs (n = 5 for interday/intraday precision were less than 10%. Furthermore, the method was successfully applied in the analysis of 20 different grape cane samples. The result showed that grape cane byproducts are potentially sources of bioactive compounds of interest for pharmaceutical and food industries.

  14. Ultrasound Assisted Endovascular Thrombolysis in Adolescents: 2 Case Reports.

    Science.gov (United States)

    Olivieri, Martin; Kurnik, Karin; Hoffmann, Florian; Reiter, Karl; Bidlingmaier, Christoph; Kuhlencordt, Peter; Treitl, Marcus

    2016-07-01

    Descending iliofemoral thrombosis in children is a rare event. Anticoagulation therapy with low-molecular-weight-heparin is standard of care. However, patency cannot be achieved in all cases, increasing the risk for rethrombosis and postthrombotic syndrome. To reduce the risk of venous valve failure in adults, local catheter-directed thrombolysis is used to reopen vessels. Two adolescent girls (17 and 15 years old) presented with acute descending iliofemoral thrombosis of the left common iliac, external, and common femoral veins. Anticoagulation with enoxaparin was started until insertion of an EkoSonic Mach 4e catheter for ultrasound-assisted local thrombolysis with recombinant tissue plasminogen activator and administration of unfractionated heparin. Success was monitored by increases in D-dimer levels and ultrasound findings. After 24 hours respectively 48 hours, complete recanalization was obtained. No complication occurred except minimal local bleeding. Screening for hereditary thrombophilia revealed a heterozygous antithrombin mutation in 1 girl (ie, the 15-year-old). May-Thurner syndrome was identified in both girls, necessitating stenting of the left common iliac veins and continuation of anticoagulation therapy with enoxaparin and acetylsalicylic acid. No rethrombosis or complications occurred during the follow-up period. Ultrasound-assisted catheter-directed local thrombolysis with the EkoSonic Mach 4e system was effective in achieving immediate recanalization of the occluded veins and should be considered in children experiencing descending iliofemoral thrombosis. The fast recanalization might reduce the incidence of postthrombotic syndrome. May-Thurner syndrome is regularly found in these patients, and if present, requires stenting of the common iliac vein to avoid early reocclusion. However, long-term patency of iliac vein stenting in children remains to be examined. Copyright © 2016 by the American Academy of Pediatrics.

  15. Ultrasound assisted extraction of polyphenols from Punica granatum (Grenada fruit

    Directory of Open Access Journals (Sweden)

    Jorge Enrique Rodríguez Chanfrau

    Full Text Available Introduction: extraction of bioactive compounds from vegetable materials is a classical operation applied in many industrial processes. Few studies have made reference to processes to obtain extracts from Punica granatum. This fruit is generally consumed as such or as fermented juices. In Cuba, it is known as grenade and numerous studies have shown antiviral, antioxidant and antimicrobial properties. Maceration process is the main used technology in the preparation of extracts from Punica granatum fruit, being this a long and expensive process. Ultrasound-assisted extractions have been proven to significantly decreased extraction time and increased extraction yields in many vegetable materials. However, few papers report the use of this methodology in the extraction processes of Punica granatum. Objective: to evaluate an ultrasound-assisted extraction process to extract polyphenols from Punica granatum fruit. Methods: an experimental surface, response 3², randomized and replicate design was made to identify the effect of the extraction time and the alcoholic concentration of the menstruum as well as an extraction study in the course of time, keeping the best extraction conditions set in the design. Results: the studied parameters did not show significant influence over the process (p= 0.0981 and p= 0.8504 for time of extraction and alcoholic content, respectively. The behaviour curve of the polyphenol extraction in time showed that top concentration values were reached at 60 minutes. Conclusions: according to results, the optimal conditions of polyphenol extraction were as follows: extraction time of 60 min, and 50 % alcoholic concentration (v/v as menstruum.

  16. Ionic liquid-based zinc oxide nanofluid for vortex assisted liquid liquid microextraction of inorganic mercury in environmental waters prior to cold vapor atomic fluorescence spectroscopic detection.

    Science.gov (United States)

    Amde, Meseret; Liu, Jing-Fu; Tan, Zhi-Qiang; Bekana, Deribachew

    2016-01-01

    Zinc oxide nanofluid (ZnO-NF) based vortex assisted liquid liquid microextraction (ZnO-NF VA-LLME) was developed and employed in extraction of inorganic mercury (Hg(2+)) in environmental water samples, followed by cold vapor atomic fluorescence spectrometry (CV-AFS). Unlike other dispersive liquid liquid microextraction techniques, ZnO-NF VA-LLME is free of volatile organic solvents and dispersive solvent consumption. Analytical signals were obtained without back-extraction from the ZnO-NF phase prior to CV-AFS determination. Some essential parameters of the ZnO-NF VA-LLME and cold vapor generation such as composition and volume of the nanofluid, vortexing time, pH of the sample solution, amount of the chelating agent, ionic strength and matrix interferences have been studied. Under optimal conditions, efficient extraction of 1ng/mL of Hg(2+) in 10mL of sample solution was achieved using 50μL of ZnO-NF. The enrichment factor before dilution, detection limits and limits of quantification of the method were about 190, 0.019 and 0.064ng/mL, respectively. The intra and inter days relative standard deviations (n=8) were found to be 4.6% and 7.8%, respectively, at 1ng/mL spiking level. The accuracy of the current method was also evaluated by the analysis of certified reference materials, and the measured Hg(2+) concentration of GBW08603 (9.6ng/mL) and GBW(E)080392 (8.9ng/mL) agreed well with their certified value (10ng/mL). The method was applied to the analysis of Hg(2+) in effluent, influent, lake and river water samples, with recoveries in the range of 79.8-92.8% and 83.6-106.1% at 1ng/mL and 5ng/mL spiking levels, respectively. Overall, ZnO-NF VA-LLME is fast, simple, cost-effective and environmentally friendly and it can be employed for efficient enrichment of the analyte from various water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. 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 (C 8 Gu-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 C 8 Gu-Cl and other IL-based and conventional surfactants, specifically the analogue 1-octyl-3-methylimidazolium chloride (C 8 MIm-Cl), and other imidazolium- (C 16 MIm-Br) and pyridinium- (C 16 Py-Cl) based surfactants, together with the conventional cationic CTAB and the conventional anionic SDS. From these studies, C 8 Gu-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 C 8 Gu-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 C 8 Gu-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 0.4

  18. Extraction and preconcentration of trace Al and Cr from vegetable samples by vortex-assisted ionic liquid-based dispersive liquid-liquid microextraction prior to atomic absorption spectrometric determination.

    Science.gov (United States)

    Altunay, Nail; Yıldırım, Emre; Gürkan, Ramazan

    2018-04-15

    In the study, a simple, and efficient microextraction approach, which is termed as vortex-assisted ionic liquid-based dispersive liquid-liquid microextraction (VA-IL-DLLME), was developed for flame atomic absorption spectrometric analysis of aluminum (Al) and chromium (Cr) in vegetables. The method is based on the formation of anionic chelate complexes of Al(III) and Cr(VI) with o-hydroxy azo dye, at pH 6.5, and then extraction of the hydrophobic ternary complexes formed in presence of cetyltrimethylammonium bromide (CTAB) into a 125 μL volume of 1-butyl-3-methylimidazolium bis(trifluorosulfonyl)imide [C 4 mim][Tf 2 N]) as extraction solvent. Under optimum conditions, the detection limits were 0.02 µg L -1 in linear working range of 0.07-100 µg L -1 for Al(III), and 0.05 µg L -1 in linear working range of 0.2-80 µg L -1 for Cr(VI). After the validation by analysis of a certified reference material (CRM), the method was successfully applied to the determination of Al and Cr in vegetables using standard addition method. Copyright © 2017 Elsevier Ltd. All rights reserved.

  19. Ionic liquid based vortex assisted liquid-liquid microextraction combined with liquid chromatography mass spectrometry for the determination of bisphenols in thermal papers with the aid of response surface methodology.

    Science.gov (United States)

    Asati, Ankita; Satyanarayana, G N V; Panchal, Smita; Thakur, Ravindra Singh; Ansari, Nasreen G; Patel, Devendra K

    2017-08-04

    A sensitive, rapid and efficient ionic liquid-based vortex assisted liquid-liquid microextraction (IL-VALLME) with Liquid Chromatography Mass spectrometry (LC-MS/MS) method is proposed for the determination of bisphenols in thermal paper. Extraction factors were systematically optimized by response surface methodology. Experimental factors showing significant effects on the analytical responses were evaluated using design of experiment. The limit of detection for Bisphenol-A (BPA) and Bisphenol-S (BPS) in thermal paper were 1.25 and 0.93μgkg -1 respectively. The dynamic linearity range for BPA was between 4 and 100μgkg -1 and the determination of coefficient (R 2 ) was 0.996. The values of the same parameters were 3-100μgkg -1 and 0.998 for BPS. The extraction recoveries of BPA and BPS in thermal paper were 101% and 99%. Percent relative standard deviation (% RSD) for matrix effect and matrix match effects were not more than 10%, for both bisphenols. The proposed method uses a statistical approach for the analysis of bisphenols in environmental samples, and is easy, rapid, requires minimum organic solvents and efficient. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Ultrasound-assisted green bromination of N-cinnamoyl amino acid amides - Structural characterization and antimicrobial evaluation

    Science.gov (United States)

    Stoykova, Boyka; Chochkova, Maya; Ivanova, Galya; Markova, Nadezhda; Enchev, Venelin; Tsvetkova, Iva; Najdenski, Hristo; Štícha, Martin; Milkova, Tsenka

    2017-05-01

    N-phenylpropenoyl amino acid amides have been brominated using two alternative sonochemically activated green chemistry procedures. The first synthetic procedure has involved an ultrasound assisted bromination in an aqueous medium using ionic liquid as a catalyst of the reaction, whereas in the second one an in situ formation of Br2 via oxidation of HBr by H2O2 has been used. For comparison, the conventional bromination procedure was also used. The newly brominated compounds were characterized by appropriate analytical techniques. A detailed NMR spectroscopic analysis and quantum chemical calculations using Density Functional Theory (DFT) methods have been used to define the stereochemistry of the products. The results confirmed the physicochemical identity and similar yields of the products obtained by the three synthetic procedures employed, and reveal the co-existence of two diastereoisomeric forms of the newly synthesized products. The antibacterial and antifungal activities of the dibrominated amides were evaluated.

  1. The preparation of trisubstituted alkenyl nucleoside phosphonates under ultrasound-assisted olefin cross-metathesis.

    Science.gov (United States)

    Sari, Ozkan; Hamada, Manabu; Roy, Vincent; Nolan, Steven P; Agrofoglio, Luigi A

    2013-09-06

    Intermolecular ultrasound-assisted olefin cross-metathesis is reported. This approach allows an easy access to challenging trisubstituted alkenyl nucleoside phosphonates. Regioselective chemoenzymatic deacetylation and Mitsunobu coupling are also described.

  2. Extraction of trace elements by ultrasound-assisted emulsification from edible oils producing detergentless microemulsions.

    OpenAIRE

    Kara, D; Fisher, A; Hill, S

    2015-01-01

    The aim of this study is to develop a new method for the extraction and preconcentration of trace elements from edible oils via an ultrasound-assisted extraction using ethylenediaminetetraacetic acid (EDTA) producing detergentless microemulsions. These were then analyzed using ICP-MS against matrix matched standards. Optimum experimental conditions were determined and the applicability of the proposed ultrasound-assisted extraction method was investigated. Under the optimal conditions, the de...

  3. Ultrasound Assisted Extraction of Phenolic Compounds from Peaches and Pumpkins

    Science.gov (United States)

    Altemimi, Ammar; Watson, Dennis G.; Choudhary, Ruplal; Dasari, Mallika R.; Lightfoot, David A.

    2016-01-01

    The ultrasound-assisted extraction (UAE) method was used to optimize the extraction of phenolic compounds from pumpkins and peaches. The response surface methodology (RSM) was used to study the effects of three independent variables each with three treatments. They included extraction temperatures (30, 40 and 50°C), ultrasonic power levels (30, 50 and 70%) and extraction times (10, 20 and 30 min). The optimal conditions for extractions of total phenolics from pumpkins were inferred to be a temperature of 41.45°C, a power of 44.60% and a time of 25.67 min. However, an extraction temperature of 40.99°C, power of 56.01% and time of 25.71 min was optimal for recovery of free radical scavenging activity (measured by 1, 1-diphenyl-2-picrylhydrazyl (DPPH) reduction). The optimal conditions for peach extracts were an extraction temperature of 41.53°C, power of 43.99% and time of 27.86 min for total phenolics. However, an extraction temperature of 41.60°C, power of 44.88% and time of 27.49 min was optimal for free radical scavenging activity (judged by from DPPH reduction). Further, the UAE processes were significantly better than solvent extractions without ultrasound. By electron microscopy it was concluded that ultrasonic processing caused damage in cells for all treated samples (pumpkin, peach). However, the FTIR spectra did not show any significant changes in chemical structures caused by either ultrasonic processing or solvent extraction. PMID:26885655

  4. Ultrasound-assisted fabrication of a biocompatible magnetic hydroxyapatite.

    Science.gov (United States)

    Zhou, Gang; Song, Wei; Hou, Yongzhao; Li, Qing; Deng, Xuliang; Fan, Yubo

    2014-10-01

    This work describes the fabrication and characterization of a biocompatible magnetic hydroxyapatite (HA) using an ultrasound-assisted co-precipitation method. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and transmission electron microscopy (TEM) were used to characterize the structure and chemical composition of the produced samples. The M-H loops of synthesized materials were traced using a vibrating sample magnetometer (VSM) and the biocompatibility was evaluated by cell culture and MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay. Furthermore, in vivo histopathological examinations were used to evaluate the potential toxicological effects of Fe₃O₄-HA composites on kidney of SD rats injected intraperitoneally with Fe₃O₄-HA particles. The results showed that magnetic iron oxide particles first replace OH ions of HA, which are parallel to the c axis, and then enter the HA crystal lattice which produces changes in the crystal surface of HA. Chemical bond interaction was observed between PO₄³⁻ groups of HA and iron ions of Fe₃O₄. The saturation magnetization (MS ) of Fe₃O₄-HA composites was 46.36 emu/g obtained from VSM data. Cell culture and MTT assays indicated that HA could affect the growth and proliferation of HEK-293 cells. This Fe₃O₄-HA composite produced no negative effects on cell morphology, viability, and proliferation and exhibited remarkable biocompatibility. Moreover, no inflammatory cell infiltration was observed in kidney histopathology slices. Therefore, this study succeeds to develop a Fe₃O₄-HA composite as a prospective biomagnetic material for future applications. © 2013 Wiley Periodicals, Inc.

  5. Ultrasound-assisted extraction of phenolic antioxidants from Acacia confusa flowers and buds.

    Science.gov (United States)

    Tung, Yu Tang; Chang, Wei Chun; Chen, Ping Sheng; Chang, Tzu Cheng; Chang, Shang Tzen

    2011-04-01

    Acacia confusa Merr. (Leguminosae), a species native to Taiwan, is widely distributed on the hills and lowlands of Taiwan, and has been used in traditional medicines. In this study, the application of ultrasound-assisted extraction was used to extract the phenolic compounds from A. confusa flowers and buds for the first time. Among the extraction methods, it can significantly enhance the contents of phenolic compounds and antioxidant activities in A. confusa flower and bud extracts using ultrasound-assisted extraction (10  min×12 times). Considering both the solvent consumption and the time needed for extraction, ultrasound-assisted extraction was found to be the most practical approach for the rapid and efficient extraction of bioactive phenolic constituents. In addition, gallic acid, myricitrin-3-rhamnoside, quercitrin-3-rhamnoside, europetin-3-rhamnoside, kaempferol-3-rhamnoside, rhamnetin-3-glucoside, and rhamnetin-3-rhamnoside were also quantified in different extracts by RP-HPLC. It is clear that ultrasound-assisted extraction is an efficient method for extracting phenolic compounds from A. confusa flowers and buds. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Quantitative Ultrasound-Assisted Extraction for Trace-Metal Determination: An Experiment for Analytical Chemistry

    Science.gov (United States)

    Lavilla, Isela; Costas, Marta; Pena-Pereira, Francisco; Gil, Sandra; Bendicho, Carlos

    2011-01-01

    Ultrasound-assisted extraction (UAE) is introduced to upper-level analytical chemistry students as a simple strategy focused on sample preparation for trace-metal determination in biological tissues. Nickel extraction in seafood samples and quantification by electrothermal atomic absorption spectrometry (ETAAS) are carried out by a team of four…

  7. Quantitative determination of oil content in small quantity of oilseed rape by ultrasound-assisted extraction combined with gas chromatography.

    Science.gov (United States)

    Wei, Fang; Gao, Gui-Zhen; Wang, Xin-Fa; Dong, Xu-Yan; Li, Ping-Ping; Hua, Wei; Wang, Xu; Wu, Xiao-Ming; Chen, Hong

    2008-09-01

    Accurately quantitative determination of oil content in oilseed rape plays an important role in varieties breeding for improving oil content in seeds. However, large quantity of oilseeds were needed in order to obtain accuracy and precision results by using standard Soxhlet extraction method, which may be a handicap in analysis of small, rare and precious samples in plant breeding. In the present work, ultrasound-assisted extraction was evaluated as a simpler and more effective alternative to conventional extraction method for the isolation of oil from small quantity of oilseed rape (oil of oilseed rape samples was extracted by ultrasound-assisted method, and then the fatty acids and total oil content of the seeds were qualitatively and quantitatively determined by gas chromatography (GC). Extraction efficiency of total oil obtained by ultrasound-assisted extraction through an orthogonal experiment (L(9) (3(4))) were investigated to get the best extraction conditions. Statistical analysis showed that the variable with the largest effect was the ultrasound-assisted extraction time which was followed by the ultrasound-assisted extraction power, and the liquid:solid ratio. A liquid:solid ratio of 1:4 (L:g), an ultrasound-assisted extraction time of 60 min and an ultrasound-assisted extraction power of 500 W were found to be optimal for oil extraction from oilseed rape. By comparing with the conventional method, it was found that the ultrasound-assisted extraction of oil from oilseed rape was about five times faster than the traditional extraction method. By the use of ultrasound-assisted extraction combined with GC analysis, the fatty acids and total oil content in small quantity of seeds (method.

  8. Ultrasound-assisted extraction of polysaccharide from Nephelium lappaceum L. fruit peel.

    Science.gov (United States)

    Maran, J Prakash; Priya, B

    2014-09-01

    In this study, ultrasound-assisted extraction technology was employed to investigate and optimize the crude polysaccharide extraction from Nephelium lappaceum L. fruit peel using three levels, four factors (LS ratio, ultrasonic power, extraction temperature and extraction time) Box-Behnken response surface design. The results showed that highest polysaccharide yield of 8.31% was obtained with an LS ratio of 32:1 ml:g, ultrasonic power of 110 W, extraction temperature of 53°C and extraction time of 41 min. The experimental yield of polysaccharide (8.29±0.03%) at optimal condition was well agreed with the predicted value. Fourier transform infrared spectroscopy (FTIR) was used for the identification of functional groups present in the extracted polysaccharide. The results suggest that ultrasound-assisted extraction could be a good alternative for the extraction of polysaccharide from N. lappaceum L. fruit peel at industrial level. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. First investigation on ultrasound-assisted preparation of food products: sensory and physicochemical characteristics.

    Science.gov (United States)

    Pingret, Daniella; Fabiano-Tixier, Anne-Sylvie; Petitcolas, Emmanuel; Canselier, Jean-Paul; Chemat, Farid

    2011-03-01

    This paper presents a comparison between manufactured food products using conventional and ultrasound-assisted procedures. Three different foam-type products, chocolate Genoise, basic sponge cake, and chocolate mousse were prepared using both methods with subsequent evaluation of the samples using both sensory and physicochemical methods. Ultrasound-assisted preparations were considered superior according to the sensory analysis, and physicochemical data confirmed this finding. This approach of applying an emerging piece of equipment, with potential industrial application to assist food preparation, consists of a new technique that could be of great interest for the development of not only other food products created by molecular gastronomy but also for practical work carried out by students.

  10. Ultrasound-Assisted Extraction of Total Phenolic Compounds from Inula helenium

    Directory of Open Access Journals (Sweden)

    Jin Wang

    2013-01-01

    Full Text Available Ultrasound-assisted extraction (UAE of phenolic compounds from Inula helenium was studied. Effects of ethanol concentration, ultrasonic time, solid-liquid ratio, and number of extractions were investigated. An orthogonal array was constructed to optimize UAE process. The optimized extraction conditions were as follows: ethanol concentration, 30%; solid-liquid ratio, 1 : 20; number of extractions, 2 times; extraction time, 30 min. Under the optimal conditions, the yield of total phenolic compounds and chlorogenic acid was 6.13±0.58 and 1.32±0.17 mg/g, respectively. The results showed that high amounts of phenolic compounds can be extracted from I. helenium by ultrasound-assisted extraction technology.

  11. Optimization of ultrasound-assisted extraction of polyphenols from spruce wood bark.

    Science.gov (United States)

    Ghitescu, Roxana-Elena; Volf, Irina; Carausu, Constantin; Bühlmann, Ana-Maria; Gilca, Iulian Andrei; Popa, Valentin I

    2015-01-01

    Here we describe the ultrasound-assisted extraction of the phenolic compounds from spruce wood bark and present a straight-forward experimental planning method, allowing the optimisation of the process. The effect of ethanol concentration, temperature and extraction time were evaluated through a 3(2)·2 experimental planning. The efficiency of the extraction process was appreciated based on factorial ANOVA results. The maximum extraction yield of total polyphenols (13.232mg gallic acid equivalents (GAE)/g of spruce bark tested) was obtained using a process time of 60min, an extraction temperature of 54°C and a concentration of ethanol of 70% respectively. These results indicate that an important quantity of bioactive compounds can be extracted from spruce wood bark by ultrasound assisted extraction technology. Copyright © 2014. Published by Elsevier B.V.

  12. Comparing Antibacterial and Antioxidant Activity of Annatto Dye Extracted by Conventional and Ultrasound-Assisted Methods

    OpenAIRE

    Mahmoud Yolmeh; Mohammad Bagher Habibi-Najafi; Shahrzad Shakouri; Fereshteh Hosseini

    2015-01-01

    Background: Annatto dye is used extensively in food industry that has antibacterial and antioxidant properties. Objectives: Aim of this paper was comparison of the antibacterial and antioxidant properties of annatto dye was extracted by conventional and ultrasound-assisted extraction (UAE) methods. Materials and Methods: In this experimental study minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of annatto dye against the bacteria were determined by ag...

  13. Improved Efficiency of Brewer’s Spent Grain Arabinoxylans by Ultrasound-Assisted Extraction

    OpenAIRE

    Reis, Sofia; Coelho, Elisabete; Coimbra, Manuel; Abu-Ghannam, Nissreen

    2014-01-01

    Arabinoxylan (AX) rich extracts from brewer’s spent grain (BSG) were produced by the application of ultrasound-assisted extraction (UAE) and conventional alkaline extraction (AKE). UAE and AKE were optimised for the production of the highest yield of ethanol insoluble material using response surface methodology (RSM). The efficiency of UAE was established by the significant reduction of time (7h to 25 min) and energy when compared to AKE, to recover similar amount of AX (60%) from BSG, leadin...

  14. Ultrasound assisted synthesis of iron doped TiO2 catalyst.

    Science.gov (United States)

    Ambati, Rohini; Gogate, Parag R

    2018-01-01

    The present work deals with synthesis of Fe (III) doped TiO 2 catalyst using the ultrasound assisted approach and conventional sol-gel approach with an objective of establishing the process intensification benefits. Effect of operating parameters such as Fe doping, type of solvent, solvent to precursor ratio and initial temperature has been investigated to get the best catalyst with minimum particle size. Comparison of the catalysts obtained using the conventional and ultrasound assisted approach under the optimized conditions has been performed using the characterization techniques like DLS, XRD, BET, SEM, EDS, TEM, FTIR and UV-Vis band gap analysis. It was established that catalyst synthesized by ultrasound assisted approach under optimized conditions of 0.4mol% doping, irradiation time of 60min, propan-2-ol as the solvent with the solvent to precursor ratio as 10 and initial temperature of 30°C was the best one with minimum particle size as 99nm and surface area as 49.41m 2 /g. SEM analysis, XRD analysis as well as the TEM analysis also confirmed the superiority of the catalyst obtained using ultrasound assisted approach as compared to the conventional approach. EDS analysis also confirmed the presence of 4.05mol% of Fe element in the sample of 0.4mol% iron doped TiO 2 . UV-Vis band gap results showed the reduction in band gap from 3.2eV to 2.9eV. Photocatalytic experiments performed to check the activity also confirmed that ultrasonically synthesized Fe doped TiO 2 catalyst resulted in a higher degradation of Acid Blue 80 as 38% while the conventionally synthesized catalyst resulted in a degradation of 31.1%. Overall, the work has clearly established importance of ultrasound in giving better catalyst characteristics as well as activity for degradation of the Acid Blue 80 dye. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Ultrasound assisted pseudo-digestion of street dust samples prior to determination by atomic absorption spectrometry.

    Science.gov (United States)

    Elik, Adil

    2005-05-15

    A sample preparation method based on ultrasound assisted pseudo-digestion of Pb, Cu, Zn and Ni from street dust samples under ultrasonic effect has been described. Parameters influencing pseudo-digestion, such as sonication time, sample mass, particle size and solvent system were fully optimized. Final solutions obtained upon sonication were analyzed by atomic absorption spectrometry. The best conditions for metal pseudo-digestion were as follows: a 25min sonication time, a 0.3g sample mass (in 25ml solvent), a particle size <63mum and a mixture of concentrated HNO(3)-HClO(4)-HF (2:1:1, v/v/v). Analytical results for the four metals by ultrasound assisted pseudo-digestion, acid bomb and conventional wet digestion methods showed a good agreement, thus indicating the possibility of using mild conditions for sample preparation instead of intensive treatments inherent with the digestion methods. In addition, this method reduces the time required for all treatments (pseudo-digestion or digestion, heating to dryness, cooling and separation) with acid bomb and conventional wet digestion methods approximately from 9 to 1h. The accuracy of the method was tested either by comparing obtained results with those of acid bomb and conventional wet digestion methods or by application on two standard reference materials. The average relative standard deviation of ultrasound assisted pseudo-digestion method varied between 0.9 and 1.8% for N=12, depending on the analyte.

  16. Removal of hexavalent chromium from contaminated waters by ultrasound-assisted aqueous solution ball milling.

    Science.gov (United States)

    Chen, Lin; Chen, Zhenhua; Chen, Ding; Xiong, Wei

    2017-02-01

    Batch mode experiments were conducted to study the removal of hexavalent chromium (Cr(VI)) from aqueous solutions using ultrasound-assisted aqueous solution ball milling. The results show that the reduction rate of Cr(VI) by ultrasound-assisted aqueous solution ball milling was significantly faster than that by ball milling or ultrasound treatment alone, and an initial Cr(VI) concentration of 166mg/L could be decreased to 0.35mg/L at 120min. The decisive factors, including initial concentration of Cr(VI), pH value, ultrasonic frequency and filling gas, were studied. It was found that the optimal ultrasonic frequency for ultrasound-assisted aqueous solution ball milling device was 20kHz, and the rate of Cr(VI) reduction as a function of filling gas followed the order: Ar>air>N 2 >O 2 . Samples were characterized by X-ray diffraction, fluorescence measurements, atomic absorption and the diphenylcarbazide colorimetric method. The Cr(VI) transformed into a precipitate that could be removed from the contaminated water, after which the water could be reused. Copyright © 2016. Published by Elsevier B.V.

  17. Glucose obtained from rice bran by ultrasound-assisted enzymatic hydrolysis

    Directory of Open Access Journals (Sweden)

    Raquel Cristine Kuhn

    2015-05-01

    Full Text Available In this work ultrasound-assisted solid-state enzymatic hydrolysis of rice bran to obtain fermentable sugars was investigated. For this purpose, process variables such as temperature, enzyme concentration and moisture content were evaluated during the enzymatic hydrolysis with and without ultrasound irradiation. The enzyme used is a blend of amylases derived from genetically modified strains of Trichoderma reesei. Kinetic of the enzymatic hydrolysis of rice bran at the constant-reaction rate period were measured. The best results for the ultrasound-assisted enzymatic hydrolysis was obtained using 3 wt% of enzyme, 60 oC and moisture content of 65 wt%, yielding 0.38 g sugar/g rice bran, whereas for the hydrolysis in the absence of ultrasound the highest yield was 0.20 g sugar/g rice bran using 3 wt% of enzyme, 60 oC and moisture content of 50 wt%. The use of ultrasound-assisted enzymatic hydrolysis of rice bran was intensified, obtaining around 74% more fermentable sugar than in the absence, showing that the use of ultrasound is a promising technology to be used in enzymatic reaction as an alternative of process intensification.

  18. Alkaline and ultrasound assisted alkaline pretreatment for intensification of delignification process from sustainable raw-material.

    Science.gov (United States)

    Subhedar, Preeti B; Gogate, Parag R

    2014-01-01

    Alkaline and ultrasound-assisted alkaline pretreatment under mild operating conditions have been investigated for intensification of delignification. The effect of NaOH concentration, biomass loading, temperature, ultrasonic power and duty cycle on the delignification has been studied. Most favorable conditions for only alkaline pretreatment were alkali concentration of 1.75 N, solid loading of 0.8% (w/v), temperature of 353 K and pretreatment time of 6 h and under these conditions, 40.2% delignification was obtained. In case of ultrasound-assisted alkaline approach, most favorable conditions obtained were alkali concentration of 1N, paper loading of 0.5% (w/v), sonication power of 100 W, duty cycle of 80% and pretreatment time of 70 min and the delignification obtained in ultrasound-assisted alkaline approach under these conditions was 80%. The material samples were characterized by FTIR, SEM, XRD and TGA technique. The lignin was recovered from solution by precipitation method and was characterized by FTIR, GPC and TGA technique. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Ionic-liquid-based dispersive liquid-liquid microextraction combined with magnetic solid-phase extraction for the determination of aflatoxins B1, B2, G1, and G2in animal feeds by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Zhao, Jiao; Zhu, Yan; Jiao, Yang; Ning, Jinyan; Yang, Yaling

    2016-10-01

    A novel two-step extraction technique combining ionic-liquid-based dispersive liquid-liquid microextraction with magnetic solid-phase extraction was developed for the preconcentration and separation of aflatoxins in animal feedstuffs before high-performance liquid chromatography coupled with fluorescence detection. In this work, ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate was used as the extractant in dispersive liquid-liquid microextraction, and hydrophobic pelargonic acid modified Fe 3 O 4 magnetic nanoparticles as an efficient adsorbent were applied to retrieve the aflatoxins-containing ionic liquid. Notably, the target of magnetic nanoparticles was the ionic liquid rather than the aflatoxins. Because of the rapid mass transfer associated with the dispersive liquid-liquid microextraction and magnetic solid phase steps, fast extraction could be achieved. The main parameters affecting the extraction recoveries of aflatoxins were investigated and optimized. Under the optimum conditions, vortexing at 2500 rpm for 1 min in the dispersive liquid-liquid microextraction and magnetic solid-phase extraction and then desorption by sonication for 2 min with acetonitrile as eluent. The recoveries were 90.3-103.7% with relative standard deviations of 3.2-6.4%. Good linearity was observed with correlation coefficients ranged from 0.9986 to 0.9995. The detection limits were 0.632, 0.087, 0.422 and 0.146 ng/mL for aflatoxins B 1 , B2, G1, and G2, respectively. The results were also compared with the pretreatment method carried out by conventional immunoaffinity columns. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Detergentless ultrasound-assisted extraction of trace elements from edible oils using lipase as an extractant.

    OpenAIRE

    Kara, D; Fisher, A; Hill, S

    2015-01-01

    A new method for the extraction and preconcentration of trace elements (Al, Ba, Cd, Cu, Fe, Mn, Mo, Ni, Ti, V and Zn) from edible oils by producing detergentless micro-emulsions via an ultrasound-assisted extraction using a water phase containing Lipase at pH 3 as an extractant was developed. The trace elements in the water phase post-extraction were determined against matrix matched standards using ICP-MS. In the first step of the work, the parameters that affect extraction, such as pH, the ...

  1. Kinetics and Thermodynamics of Ultrasound-Assisted Depolymerization of κ-Carrageenan

    Directory of Open Access Journals (Sweden)

    Ratnawati Ratnawati

    2016-03-01

    Full Text Available The ultrasound-assisted depolymerization of κ-carrageenan has been studied at various temperatures and times. The κ-carrageenan with initial molecular weight of 545 kDa was dispersed in water to form a 5 g/L solution, which was then depolymerized in an ultrasound device at various temperatures and times. The viscosity of the solution was measured using Brookfield viscometer, which was then used to find the number-average molecular weight by Mark-Houwink equation. To obtain the kinetics of κ-carrageenan depolymerization, the number-average molecular weight data was treated using midpoint-chain scission kinetics model. The pre-exponential factor and activation energies for the reaction are 2.683×10-7 mol g-1 min-1 and 6.43 kJ mol-1, respectively. The limiting molecular weight varies from 160 kDa to 240 kDa, and it is linearly correlated to temperature. The results are compared to the result of thermal depolymerization by calculating the half life. It is revealed that ultrasound assisted depolymerization of κ-carrageenan is faster than thermal depolymerization at temperatures below 72.2°C. Compared to thermal depolymerization, the ultrasound-assisted process has lower values of Ea, ΔG‡, ΔH‡, and ΔS‡, which can be attributed to the ultrasonically induced breakage of non-covalent bonds in κ-carrageenan molecules. Copyright © 2016 BCREC GROUP. All rights reserved Received: 10th November 2015; Revised: 18th January 2016; Accepted: 19th January 2016 How to Cite: Ratnawati, R., Prasetyaningrum, A., Wardhani, D.H. (2016. Kinetics and Thermodynamics of Ultrasound-Assisted Depolymerization of κ-Carrageenan. Bulletin of Chemical Reaction Engineering & Catalysis, 11(1: 48-58. (doi:10.9767/bcrec.11.1.415.48-58 Permalink/DOI: http://dx.doi.org/10.9767/bcrec.11.1.415.48-58

  2. Recent developments on ultrasound-assisted organic synthesis in aqueous medium

    Directory of Open Access Journals (Sweden)

    Banerjee Bubun

    2017-01-01

    Full Text Available In the recent past, a number of methods were reported on the application of ultrasound in organic reactions for the synthesis of diverse organic scaffolds. On the other hand, as far as green chemistry is concerned, water is the safest of all solvents. Thus, a “strong collaboration” between ultrasonic irradiation and aqueous medium holds the key to the development of an environmentally sustainable protocol. The present review summarizes the latest developments in ultrasound-assisted and water-mediated organic synthesis reported to date.

  3. Improved efficiency of brewer's spent grain arabinoxylans by ultrasound-assisted extraction.

    Science.gov (United States)

    Reis, Sofia F; Coelho, Elisabete; Coimbra, Manuel A; Abu-Ghannam, Nissreen

    2015-05-01

    Arabinoxylan (AX) rich extracts from brewer's spent grain (BSG) were produced by the application of ultrasound-assisted extraction (UAE) and conventional alkaline extraction (AKE). UAE and AKE were optimised for the production of the highest yield of ethanol insoluble material using response surface methodology (RSM). The efficiency of UAE was established by the significant reduction of time (7h to 25 min) and energy when compared to AKE, to recover similar amounts of AX (60%) from BSG, leading to the production of starch-free AX-rich extracts. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. High rate performance of flexible pseudocapacitors fabricated using ionic-liquid-based proton conducting polymer electrolyte with poly(3, 4-ethylenedioxythiophene):poly(styrene sulfonate) and its hydrous ruthenium oxide composite electrodes.

    Science.gov (United States)

    Sellam; Hashmi, S A

    2013-05-01

    We report the studies on all-solid-state flexible pseudocapacitors based on poly (3,4-ethylenedioxythiophene)-poly (styrene sulfonate) (PEDOT-PSS) and PEDOT-PSS/hydrous ruthenium oxide composite electrodes separated by nonaqueous proton conducting polymer electrolyte. Structural, thermal and electrochemical properties including high ionic conductivity (6.2 × 10(-2) S cm(-1) at 20 °C) of the polymer electrolyte, comprising ionic liquid 1-ethyl 3-methyl imidazolium hydrogen sulfate (EMIHSO4) immobilized in the blend of poly (vinyl alcohol) (PVA) and poly (vinyl pyrrolidone) (PVP), demonstrate its excellent suitability in supercapacitor fabrication. A substantial improvement in the specific capacitance (hence the specific energy) has been obtained when the PEDOT-PSS electrodes in the symmetrical pseudocapacitor are replaced by the composite electrodes PEDOT-PSS/RuO2·xH2O. High rate capability of the capacitor cell (with PEDOT-PSS electrodes) has been observed, as evidenced from the high knee frequency (∼966 Hz), low response time (∼70 ms) and high pulse power (∼10.2 kW kg(-1)), observed by impedance analysis. Almost rectangular (capacitive) cyclic voltammetric patterns for high scan rates (up to 15 V s(-1)) confirm the high rate performance of the pseudocapacitor. The PEDOT-PSS/RuO2·xH2O composite electrodes show the lower rate capability (knee frequency ∼312 Hz, response time ∼1 s, pulse power ∼3.2 kW kg(-1) and capacitive CV response up to 500 mV s(-1)) because of slow exchange of charges at the interfaces via RuO2·xH2O. However, the pseudocapacitor with composite electrodes shows higher rate performance relative to many reported RuO2·xH2O systems. About 15% improvement is noticed in the capacitance value when the capacitor with composite electrodes is initially charged and discharged up to ∼200 cycles. Thereafter, the cell shows almost constant value of specific capacitance (∼70 F g(-1)) for 1000 cycles.

  5. Optimisation of ultrasound-assisted extraction of natural antioxidants from mustard seed cultivars.

    Science.gov (United States)

    Szydłowska-Czerniak, Aleksandra; Tułodziecka, Agnieszka; Karlovits, György; Szłyk, Edward

    2015-05-01

    Modified mustard varieties can produce edible oil with reduced amounts of erucic acid and glucosinolates and enhanced antioxidant potential. Therefore, this work focused on the optimisation of the ultrasound-assisted extraction of compounds with high antioxidant capacity from three white mustard seed cultivars using response surface methodology. The predicted optimum solvent polarity (57.2, 56.5 and 57.6) and ultrasound power-to-sonication time ratio (4.5, 4.8 and 4.3 W min(-1)) resulted in antioxidant capacities determined by the ferric-reducing antioxidant power (FRAP) assay [54.37, 65.75 and 68.55 mmol Trolox equivalent (TE) kg(-1)] and the 2,2'-diphenyl-1-picrylhydrazyl (DPPH) method (141.65, 175.26 and 185.10 mmol TE kg(-1)) and total phenolics content (23.70, 27.16 and 11.29 mg sinapic acid g(-1)) for extracts obtained from one traditional and two modified mustard seed varieties. The highest FRAP and DPPH values (69.51 and 197.73 mmol TE kg(-1)) revealed 50% methanolic extract prepared from modified mustard seed cultivar without erucic acid and glucosinolates treated with ultrasound for 30 min (ultrasound power/ultrasound time = 4 W min(-1)). Ultrasound-assisted extraction was found to be a more rapid, convenient and appropriate extraction method with higher yield of antioxidants, shorter time and lower solvent consumption in comparison to conventional extraction. © 2014 Society of Chemical Industry.

  6. Optimization of ultrasound-assisted extraction of glycyrrhizic acid from licorice using response surface methodology.

    Science.gov (United States)

    Jang, Seol; Lee, A Yeong; Lee, A Reum; Choi, Goya; Kim, Ho Kyoung

    2017-12-01

    The present study optimized ultrasound-assisted extraction conditions to maximize extraction yields of glycyrrhizic acid from licorice. The optimal extraction temperature (X 1 ), extraction time (X 2 ), and methanol concentration (X 3 ) were identified using response surface methodology (RSM). A central composite design (CCD) was used for experimental design and analysis of the results to obtain the optimal processing parameters. Statistical analyses revealed that three variables and the quadratic of X 1 , X 2 , and X 3 had significant effects on the yields and were followed by significant interaction effects between the variables of X 2 and X 3 ( p response surface plot and contour plots derived from the mathematical models were applied to determine the optimal conditions. The optimum ultrasound-assisted extraction conditions were as follows: extraction temperature, 69 °C; extraction time, 34 min; and methanol concentration, 57%. Under these conditions, the experimental yield of glycyrrhizic acid was 3.414%, which agreed closely with the predicted value (3.406%). The experimental values agreed with those predicted by RSM models, thus indicating the suitability of the model employed and the success of RSM in optimizing the extraction conditions.

  7. Response Surface Methodology for Ultrasound-Assisted Extraction of Astaxanthin from Haematococcus pluvialis

    Directory of Open Access Journals (Sweden)

    Hong-Fu Wu

    2013-05-01

    Full Text Available Astaxanthin is a novel carotenoid nutraceutical occurring in many crustaceans and red yeasts. It has exhibited various biological activities including prevention or amelioration of cardiovascular disease, gastric ulcer, hypertension, and diabetic nephropathy. In this study, ultrasound-assisted extraction was developed for the effective extraction of astaxanthin from Haematococcus pluvialis. Some parameters such as extraction solvent, liquid-to-solid ratio, extraction temperature, and extraction time were optimized by single-factor experiment and response surface methodology. The optimal extraction conditions were 48.0% ethanol in ethyl acetate, the liquid-to-solid ratio was 20:1 (mL/g, and extraction for 16.0 min at 41.1 °C under ultrasound irradiation of 200 W. Under optimal conditions, the yield of astaxanthin was 27.58 ± 0.40 mg/g. The results obtained are beneficial for the full utilization of Haematococcus pluvialis, which also indicated that ultrasound-assisted extraction is a very useful method for extracting astaxanthin from marine life.

  8. Ultrasound assisted immersion freezing of broccoli (Brassica oleracea L. var. botrytis L.).

    Science.gov (United States)

    Xin, Ying; Zhang, Min; Adhikari, Benu

    2014-09-01

    The aim of this study was to research the ultrasound-assisted freezing (UAF) of broccoli. CaCl2 solution was used as freezing medium. The comparative advantage of using UAF over normal freezing on the freezing time, cell-wall bound calcium to total calcium ratio, textural properties, color, drip loss and L-ascorbic acid contents was evaluated. The application of UAF at selected acoustic intensity with a range of 0.250-0.412 W/cm(2) decreased the freezing time and the loss of cell-wall bound calcium content. Compared to normal freezing, the values of textural properties, color, L-ascorbic acid content were better preserved and the drip loss was significantly minimized by the application of UAF. However, when outside that range of acoustic intensity, the quality of the ultrasound-assisted frozen broccoli was inferior compared to that of the normally frozen samples. Selected the appropriate acoustic intensity was very important for the application of UAF. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Optimization of Ultrasound Assisted Extraction of Functional Ingredients from Stevia Rebaudiana Bertoni Leaves

    Science.gov (United States)

    Šic Žlabur, Jana; Voća, Sandra; Dobričević, Nadica; Brnčić, Mladen; Dujmić, Filip; Rimac Brnčić, Suzana

    2015-04-01

    The aim of the present study was to reveal an effective extraction procedure for maximization of the yield of steviol glycosides and total phenolic compounds as well as antioxidant activity in stevia extracts. Ultrasound assisted extraction was compared with conventional solvent extraction. The examined solvents were water (100°C/24 h) and 70% ethanol (at 70°C for 30 min). Qualitative and quantitative analyses of steviol glycosides in the extracts obtained were performed using high performance liquid chromatography. Total phenolic compounds, flavonoids, and radical scavenging capacity by 2, 2-azino-di-3-ethylbenzothialozine- sulphonic acid) assay were also determined. The highest content of steviol glycosides, total phenolic compounds, and flavonoids in stevia extracts were obtained when ultrasound assisted extraction was used. The antioxidant activity of the extracts was correlated with the total amount of phenolic compounds. The results indicated that the examined sonication parameters represented as the probe diameter (7 and 22 mm) and treatment time (2, 4, 6, 8, and 10 min) significantly contributed to the yield of steviol glycosides, total phenolic compounds, and flavonoids. The optimum conditions for the maximum yield of steviol glycosides, total phenolic compounds, and flavonoids were as follows: extraction time 10 min, probe diameter 22 mm, and temperature 81.2°C.

  10. Green ultrasound-assisted extraction of carotenoids from pomegranate wastes using vegetable oils.

    Science.gov (United States)

    Goula, Athanasia M; Ververi, Maria; Adamopoulou, Anna; Kaderides, Kyriakos

    2017-01-01

    The objective of this work was to develop a new process for pomegranate peels application in food industries based on ultrasound-assisted extraction of carotenoids using different vegetable oils as solvents. In this way, an oil enriched with antioxidants is produced. Sunflower oil and soy oil were used as alternative solvents and the effects of various parameters on extraction yield were studied. Extraction temperature, solid/oil ratio, amplitude level, and extraction time were the factors investigated with respect to extraction yield. Comparative studies between ultrasound-assisted and conventional solvent extraction were carried out in terms of processing procedure and total carotenoids content. The efficient extraction period for achieving maximum yield of pomegranate peel carotenoids was about 30min. The optimum operating conditions were found to be: extraction temperature, 51.5°C; peels/solvent ratio, 0.10; amplitude level, 58.8%; solvent, sunflower oil. A second-order kinetic model was successfully developed for describing the mechanism of ultrasound extraction under different processing parameters. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Effects of ultrasound-assisted alkaline extraction on the physiochemical and functional characteristics of chicken liver protein isolate.

    Science.gov (United States)

    Zou, Y; Li, P P; Zhang, K; Wang, L; Zhang, M H; Sun, Z L; Sun, C; Geng, Z M; Xu, W M; Wang, D Y

    2017-08-01

    This research investigated the physiochemical and functional characteristics of chicken liver protein isolate, which was extracted by alkali (CLPI) and ultrasound-assisted alkali (UCLPI), respectively. Protein yield of UCLPI was increased by 55.4% over that of CLPI (P  0.05). However, the enthalpy of denaturation in UCLPI decreased by 41.7%, which was related to the changes in its second structure. This resulted in better water/oil holding capacity and emulsifying properties for UCLPI. The changed physiochemical characteristics and improved functional properties of UCLPI demonstrated the potential utilization of ultrasound-assisted alkaline extraction in the food industries. © 2017 Poultry Science Association Inc.

  12. A remarkable enhancement in Am³⁺/Eu³⁺ selectivity by an ionic liquid based solvent containing bis-1,2,4-triazinyl pyridine derivatives: DFT validation of experimental results.

    Science.gov (United States)

    Bhattacharyya, Arunasis; Ansari, Seraj A; Gadly, Trilochan; Ghosh, Sunil K; Mohapatra, Manoj; Mohapatra, P K

    2015-04-07

    Mutual separation of trivalent actinide (An(3+)) and lanthanide (Ln(3+)) using several soft (N) donor ligands (bis(5,6-dialkyl-1,2,4-triazinyl)pyridine (R-BTP)) is attempted for the first time in room temperature ionic liquid (RTIL) medium. The results indicate a spectacular enhancement in the selectivity as compared to that in molecular diluents with a separation factor (S.F.) of >3000 for Am(3+) over Eu(3+) using the methyl derivative (Me-BTP) in RTIL medium using [C(n)mim]·[NTf2] as the diluents (where n = 2, 3, 4, 6 or 8). Such a high S.F. value has never been reported before with any of the R-BTP derivatives in molecular diluents. An opposite trend in the distribution ratio values of both Am(3+) and Eu(3+) with the increasing size of the alkyl (R) group is observed in RTIL medium when compared with that in molecular diluents. The differences in the extraction behaviour of R-BTPs in RTILs vis-à-vis molecular diluents are explained on the basis of the difference in the nature of complexes extracted in these two distinctly different media as supported by the time resolved fluorescence (TRFS) study. An unusually high extractability and selectivity for Am(3+) over Eu(3+) with Me-BTP was attributed to the formation of a 1 : 4 complex for Am(3+), which was never reported earlier with any of the R-BTP derivatives in molecular diluents. DFT studies indicated higher metal 'd' and 'f' orbital participation (covalence) in the bonding with R-BTP in the case of Am(3+) complexes as compared to that in the case of Eu(3+) complexes, which resulted in the selectivity of these classes of ligands. The observed results may have a great significance in the radioactive waste management involving the partitioning and transmutation strategy.

  13. Preparation and application of a poly (ionic liquid)-based molecularly imprinted polymer for multiple monolithic fiber solid-phase microextraction of phenolic acids in fruit juice and beer samples.

    Science.gov (United States)

    Chen, Lei; Huang, Xiaojia

    2017-10-23

    In this work, a new molecularly imprinted polymer (MIP) using a poly (ionic liquid) (PIL) as a functional monomer was prepared and utilized as the extraction medium of multiple monolithic fiber solid-phase microextraction (MMF-SPME). A PIL, 1-ally-3-vinylimidazolium chloride, was used as a functional monomer, and 3,4-dihydroxybenzenepropanoic acid (DBA) and ethylene dimethacrylate were chosen as the template molecule and cross-linker, respectively, to synthesize the PIL/MIP. Under the optimized preparation conditions, the recognition coefficient of PIL-MIP for DBA was as high as 11.6. The combination of PIL/MIP-MMF-SPME and high-performance liquid chromatography with diode array detection (HPLC/DAD) was developed for the sensitive determination of phenolic acids (PAs) in fruit juice and beer samples. Under the optimal conditions which were investigated in detail, the limits of detection (LODs, S/N = 3) for PAs in fruit juice were 0.024-0.24 μg L -1 , and the related values were 0.011-0.052 μg L -1 for the beer sample. The intra-day and inter-day precision (relative standard deviations, n = 4, %) at 1.0 and 100.0 μg L -1 spiking concentration were both less than 10%. In the analysis of PAs in fruit juice and beer samples, satisfactory recoveries and repeatability were achieved. In comparison with reported approaches, the proposed method exhibited some advantages including high selectivity, convenience, satisfactory sensitivity and environmental friendliness.

  14. Double salts of ionic-liquid-based surfactants in microextraction: application of their mixed hemimicelles as novel sorbents in magnetic-assisted micro-dispersive solid-phase extraction for the determination of phenols.

    Science.gov (United States)

    Trujillo-Rodríguez, María J; Pino, Verónica; Anderson, Jared L; Ayala, Juan H; Afonso, Ana M

    2015-11-01

    The use of mixed hemimicelles of ionic liquid (IL)-based surfactants in a magnetic-based micro-dispersive solid-phase extraction (m-μdSPE) approach is described. Not only is the symmetric monocationic IL-based surfactant 1,3-didodecylimidazolium bromide (C12C12Im-Br) studied for first time in m-μdSPE, but double-salt (DS) IL (DSIL)-based surfactants are also examined. Nine DSIL-based surfactants were formed by combination of C12C12Im-Br with other IL-based surfactants, including nonsymmetric monocationic and dicationic ILs combined at three different molar fractions. The analytical application was focused on the determination of a group of eight phenols, including bisphenol A, in water samples. The best results were obtained with the DSIL formed by C12C12Im-Br (molar fraction 0.5) and 1-hexadecyl-3-methylimidazolium bromide (C16MIm-Br), after proper optimization of the overall method in combination with high-performance liquid chromatography (HPLC) and diode-array detection (DAD). The optimum conditions for 100 mL of water samples require a small amount (10 mg) of Fe3O4 magnetic nanoparticles, a low content (5.0 mg of C12C12Im-Br and 3.9 mg of C16MIm-Br) of the selected DSIL, pH 11, a sonication time of 2.5 min, and an equilibration time of 5 min with the aid of NdFeB magnets, followed by elution of phenols, evaporation, and reconstitution with 0.5 mL of acetonitrile. The overall m-μdSPE-HPLC-DAD method is characterized for limits of detection down to 1.3 μg · L(-1), intraday relative standard deviations lower than 13 % (n = 3), and interday relative standard deviations lower than 17 % (n = 9), with a spiking level of 15 μg · L(-1); with enrichment factors between 15.7 and 141, and average relative recoveries of 99.9 %.

  15. Development and validation of a fast ionic liquid-based dispersive liquid-liquid microextraction procedure combined with LC-MS/MS analysis for the quantification of benzodiazepines and benzodiazepine-like hypnotics in whole blood.

    Science.gov (United States)

    De Boeck, Marieke; Missotten, Sophie; Dehaen, Wim; Tytgat, Jan; Cuypers, Eva

    2017-05-01

    To date, thorough clean-up of complex biological samples remains an essential part of the analytical process. The solid phase extraction (SPE) technique is the well-known standard, however, its main weaknesses are the labor-intensive and time-consuming protocols. In this respect, dispersive liquid-liquid microextractions (DLLME) seem to offer less complex and more efficient extraction procedures. Furthermore, ionic liquids (ILs) - liquid salts - are emerging as new promising extraction solvents, thanks to their non-flammable nature, negligible vapor pressure and easily adaptable physiochemical properties. In this study, we investigated whether ILs can be used as an extraction solvent in a DLLME procedure for the extraction of a broad range of benzodiazepines and benzodiazepine-like hypnotics in whole blood samples. 1.0mL whole blood was extracted using an optimized 30-min IL-based DLLME procedure, followed by LC-ESI(+)-MS/MS analysis in scheduled MRM scan mode. The optimized analytical method was successfully validated for 7-aminoflunitrazepam, alprazolam, bromazepam, clobazam, clonazepam, clotiazepam, diazepam, estazolam, ethyl loflazepate, etizolam, flurazepam, lormetazepam, midazolam, oxazepam, prazepam, temazepam, triazolam, zolpidem and zopiclone. The method showed good selectivity for endogenous interferences based on 12 sources of blank whole blood. No benzodiazepine interferences were observed, except for clorazepate and nordiazepam, which were excluded from the quantitative method. Matrix-matched calibration curves were constructed covering the whole therapeutic range, including low toxic plasma concentrations. Accuracy and precision results met the proposed acceptance criteria for the vast majority of compounds, except for brotizolam, chlordiazepoxide, cloxazolam, flunitrazepam, loprazolam, lorazepam and nitrazepam, which can only be determined in a semi-quantitative way. Recoveries were within the range of 24.7%-127.2% and matrix effects were within 20

  16. Ultrasound-assisted extraction of polysaccharides from Rhododendron aganniphum: Antioxidant activity and rheological properties.

    Science.gov (United States)

    Guo, Xiao; Shang, Xiaofei; Zhou, Xuzheng; Zhao, Baotang; Zhang, Jiyu

    2017-09-01

    In this study, we aimed to optimize the extraction of polysaccharides from the leaves of Rhododendron aganniphum and investigate its rheological properties and antioxidant activity. After optimizing the operating parameters using a Box-Behnken design (BBD), the results showed that the optimal ultrasound-assisted extraction conditions were as follows: extraction temperature, 55°C; liquid-solid ratio, 25:1; extraction time, 2.2h; and ultrasound treatment power, 200W. The optimized experimental yield of polysaccharides by ultrasound-assisted extraction (PUAE) was 9.428%, higher than that obtained by hot water extraction (PHWE) for 12h at the same liquid-solid ratio and extraction temperature. In the in vitro antioxidant activity tests, PUAE had higher positive radical scavenging activity for hydroxyl, superoxide and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radicals than PHWE. However, PUAE and PHWE solutions had similar intermolecular interactions in the steady-shear flow and dynamic viscoelasticity tests, resulting in similar macroscopic behaviour. With respect to the apparent viscosity, storage modulus (G') and loss modulus (G″) of PUAE were lower at the same shear rate or angular frequency. All PUAE solutions exhibited non-Newtonian shear-thinning pseudoplastic behaviour that was accurately described by the Carreau model but was better fit by the power-law model at high shear rates (≥1/s), which demonstrated that the variation in the apparent viscosity dependence was greater at higher concentrations and shear rates. The G' and G″ of the solutions increased as the experimental frequency increased from 0.05 to 500rad/s under all experimental concentrations, and the modulus crossover point decreased gradually with increasing PUAE concentration. The above results demonstrated that the ultrasound-assisted extraction methods gave a higher yield of polysaccharides from the leaves of R. aganniphum with a shorter extraction time than the hot water extraction method

  17. Ultrasound assisted direct transesterification of algae for biodiesel production : Analysis of emission characteristics

    Directory of Open Access Journals (Sweden)

    Namasivayam Manickam

    2014-03-01

    Full Text Available Recently, the algae-for-fuel concept has gained renewed interest with energy prices fluctuating widely. Due to some restrictions over the oil extraction from algae, direct transesterification may be considered as a good alternative. In this study, to improve the performance of direct transesterification, ultrasound induction was carried out. A sonicator probe was used to induce the direct transesterification of Cladophora fracta, a freshwater macro alga, which contains 14% lipid on dry biomass basis. Due to ultrasonication about 25% increased biodiesel yields were obtained and the biodiesel thus prepared was analyzed for emission characteristics. The analysis results showed that Cladophora biodiesel emits 18 mg/L of CO whereas petroleum diesel emits 50 mg/L. Similarly, the emission of NOx and particulate matter also were reduced to a considerable level. The Cladophora is a suitable source of biodiesel by ultrasound assisted direct transesterification in industrial level in the future.

  18. Simultaneous determination of butyltin and phenyltin species in sediments using ultrasound-assisted leaching

    Energy Technology Data Exchange (ETDEWEB)

    Carpinteiro, J.; Rodriguez, I.; Cela, R. [Dpto. Quimica Analitica, Nutricion y Bromatologia, Universidad de Santiago de Compostela (Spain)

    2001-08-01

    A fast and simple procedure is presented for the simultaneous leaching of butyl (mono, di and tributyl) and phenyl organotin species from sediment samples. Leached compounds are further ethylated with sodium tetraethylborate in aqueous medium, and analyzed by gas chromatography. After testing the stability of triphenyltin under different extraction conditions, ultrasound-assisted leaching at room temperature in the presence of acetic acid was been proposed as an extraction procedure compatible with the simultaneous determination of phenyl- and butyltin compounds in sediments. Recoveries between 70 and 90% were obtained for phenyl species in spiked samples prepared in the laboratory. Results for butyltin species were validated by use of the reference material PACS-2. Quantification limits, using GC-MIP-AES as measurement technique, were approximately 5-10 ng g{sup -1}. Precision in the consecutive analysis of three sediment samples varied between 3 and 10%. (orig.)

  19. Analyses of factors affecting nickel ferrite nanoparticles synthesis in ultrasound-assisted aqueous solution ball milling.

    Science.gov (United States)

    Yuan, Zhuang; Chen, Zhen-hua; Chen, Ding; Kang, Zhi-tao

    2015-01-01

    Ball milling experiments were conducted with and without ultrasound wave assistance in deionized water using NiCO3·2Ni(OH)2·4H2O as raw materials. In the reaction process of NiFe2O4 prepared by ultrasound-assisted aqueous solution ball milling, some influencing factors including raw materials, ultrasonic frequency, ball to powder ratio and liquid level were changed. Samples were characterized by X-ray diffraction, fluorescence measurements and electroconductivity detections. The results indicate that more hydroxyl radicals and ions can be generated under the coupling effect of ultrasonic and ball milling. The fluorescence measurements and electroconductivity detections also reflect the reaction speed, allowing for optimal parameters to be determined. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Extraction of curcumin from Curcuma longa L. using ultrasound assisted supercritical carbon dioxide

    Science.gov (United States)

    Kimthet, Chhouk; Wahyudiono, Kanda, Hideki; Goto, Motonobu

    2017-05-01

    Curcumin is one of phenolic compounds, which has been recently shown to have useful pharmacological properties such as anti-inflammatory, anti-bacterial, anti-carcinogenic, antifungal, and antimicrobial activities. The objective of this research is to extract the curcumin from Curcuma longa L. using ultrasound assisted supercritical carbon dioxide extraction (USC-CO2). The extraction was performed at 50°C, 25 MPa, CO2 flow rate of 3 mL/min with 10% cosolvent. The result of extraction, thermogravimetry (TG), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscope (SEM) showed that ultrasound power could disrupt cell wall and release the target compounds from Curcuma longa L. USC-CO2 could provide higher curcumin content in the extracts and faster extraction compared to SC-CO2 extraction without ultrasound.

  1. Ultrasound-Assisted Extraction of Total Flavonoids from Corn Silk and Their Antioxidant Activity

    Directory of Open Access Journals (Sweden)

    Ling-Li Zheng

    2016-01-01

    Full Text Available Object. Ultrasound-assisted extraction of total flavonoids from corn silk and their antioxidant activities were studied. Methods. Response surface methodology was adopted to optimize the extraction conditions and antioxidant activities of the extracted total flavonoids were detected through ferric reducing antioxidant power (FRAP assay. Results. Through a three-level, three-variable Box-Behnken design of response surface methodology (RSM adopting yield as response, the optimal conditions were determined as follows: ultrasonic power 500 W, extraction time 20 min, material solvent ratio 1 : 20, and ethanol concentration 30%. Under the optimum conditions, the extraction yield of total flavonoids was 1.13%. FRAP value of total flavonoids extracted from corn silk was 467.59 μmol/L. Conclusion. The total flavonoids of corn silk could be developed as food natural antioxidant reagents.

  2. Ultrasound-assisted powder-coating technique to improve content uniformity of low-dose solid dosage forms

    DEFF Research Database (Denmark)

    Genina, Natalja; Räikkönen, Heikki; Antikainen, Osmo

    2010-01-01

    An ultrasound-assisted powder-coating technique was used to produce a homogeneous powder formulation of a low-dose active pharmaceutical ingredient (API). The powdered particles of microcrystalline cellulose (MCC; Avicel® PH-200) were coated with a 4% m/V aqueous solution of riboflavin sodium...

  3. Combined use of ultrasound-assisted liposuction and limited-incision platysmaplasty for treatment of the aging neck

    NARCIS (Netherlands)

    Rooijens, P.P.G.M.; Zweep, H.P.; Beekman, W.H.

    2008-01-01

    Background: Many techniques have been introduced for the surgical treatment of the aging neck. In this study the combination therapy of ultrasound-assisted liposuction and limited-incision platysmaplasty for cervicofacial rejuvenation is presented. Methods: Fifteen female patients (age = 43-75

  4. Ultrasound-assisted dilute acid hydrolysis of tea processing waste for production of fermentable sugar.

    Science.gov (United States)

    Germec, Mustafa; Tarhan, Kübra; Yatmaz, Ercan; Tetik, Nedim; Karhan, Mustafa; Demirci, Ali; Turhan, Irfan

    2016-03-01

    Lignocellulosic materials that are the most abundant plant biomass in the world have the potential to become sustainable sources of the produced value added products. Tea processing waste (TPW) is a good lignocellulosic source to produce the value added products from fermentable sugars (FSs). Therefore, the present study is undertaken to produce FSs by using ultrasound-assisted dilute acid (UADA) and dilute acid (DA) hydrolysis of TPW followed by enzymatic hydrolysis. UADA hydrolysis of TPW was optimized by response surface methodology (RSM) at maximum power (900 W) for 2 h. The optimum conditions were determined as 50°C, 1:6 (w/v) solid:liquid ratio, and 1% (w/v) DA concentration, which yielded 20.34 g/L FS concentration. Furthermore, its DA hydrolysis was also optimized by using RSM for comparison and the optimized conditions were found as 120°C, 1:8 solid:liquid ratio, and 1% acid concentration, which produced 25.3 g/L FS yield. Even though the produced sugars with UADA hydrolysis are slightly less, but it can provide significant cost saving due to the lower temperature requirement and less liquid consumption. Besides, enzymatic hydrolysis applied after pretreatments of TPW were very more economic than the conventional enzymatic hydrolysis in the literature due to shorter time requiring. In conclusion, ultrasound-assisted is a promising technology that can be successfully applied for hydrolysis of biomass and can be an alternative to the other hydrolysis procedures and also TPW can be considered as suitable carbon source for the production of value-added products like biofuels, organic acids, and polysaccharides. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:393-403, 2016. © 2016 American Institute of Chemical Engineers.

  5. Optimization of Ultrasound-assisted Extraction of Phenolic Compounds from Myrcia amazonica DC. (Myrtaceae) Leaves

    Science.gov (United States)

    de Morais Rodrigues, Mariana Cristina; Borges, Leonardo Luiz; Martins, Frederico Severino; Mourão, Rosa Helena V.; da Conceição, Edemilson Cardoso

    2016-01-01

    Background: Myrcia amazonica. DC is a species predominantly found in northern Brazil, and belongs to the Myrtaceae family, which possess various species used in folk medicine to treat gastrointestinal disorders, infectious diseases, and hemorrhagic conditions and are known for their essential oil contents. Materials and Methods: This study aimed applied the Box–Behnken design combined with response surface methodology to optimize ultrasound-assisted extraction of total polyphenols, total tannins (TT), and total flavonoids (TF) from M. amazonica DC. Results: The results indicated that the best conditions to obtain highest yields of TT were in lower levels of alcohol degree (65%), time (15 min), and also solid: Liquid ratio (solid to liquid ratio; 20 mg: 5 mL). The TF could be extracted with high amounts with higher extraction times (45 min), lower values of solid: Liquid ratio (20 mg: mL), and intermediate alcohol degree level. Conclusion: The exploitation of the natural plant resources present very important impact for the economic development, and also the valorization of great Brazilian biodiversity. The knowledge obtained from this work should be useful to further exploit and apply this raw material. SUMMARY Myrcia amazonica leaves possess phenolic compounds with biological applications;Lower levels of ethanolic strength are more suitable to obtain a igher levels of phenolic compouds such as tannins;Box-Behnken design indicates to be useful to explore the best conditions of ultrasound assisted extraction. Abbreviation used: Nomenclature ES: Ethanolic strength, ET: Extraction time, SLR: Solid to liquid ratio, TFc: Total flavonoid contents, TPc: Total polyphenol contents, TTc: Total tannin contents PMID:27019555

  6. Ultrasound-Assisted Extraction, Centrifugation and Ultrafiltration: Multistage Process for Polyphenol Recovery from Purple Sweet Potatoes

    Directory of Open Access Journals (Sweden)

    Zhenzhou Zhu

    2016-11-01

    Full Text Available This work provides an evaluation of an ultrasound-assisted, combined extraction, centrifugation and ultrafiltration process for the optimal recovery of polyphenols. A purple sweet potato (PSP extract has been obtained using ultrasonic circulating extraction equipment at a power of 840 W, a frequency of 59 kHz and using water as solvent. Extract ultrafiltration, using polyethersulfone (PES, was carried out for the recovery of polyphenol, protein and anthocyanin. Pre-treatment, via the centrifugation of purple sweet potato extract at 2500 rpm over 6 min, led to better polyphenol recovery, with satisfactory protein removal (reused for future purposes, than PSP extract filtration without centrifugation. Results showed that anthocyanin was efficiently recovered (99% from permeate. The exponential model fit well with the experimental ultrafiltration data and led to the calculation of the membrane’s fouling coefficient. The optimization of centrifugation conditions showed that, at a centrifugation speed of 4000 rpm (1195× g and duration of 7.74 min, the optimized polyphenol recovery and fouling coefficient were 34.5% and 29.5 m−1, respectively. The removal of proteins in the centrifugation process means that most of the anthocyanin content (90% remained after filtration. No significant differences in the intensities of the HPLC-DAD-ESI-MS2 peaks were found in the samples taken before and after centrifugation for the main anthocyanins; peonidin-3-feruloylsophoroside-5-glucoside, peonidin-3-caffeoyl-p-hydroxybenzoylsophoroside-5-glucoside, and peonidin-3-caffeoyl-feruloyl sophoroside-5-glucoside. This proves that centrifugation is an efficient method for protein removal without anthocyanin loss. This study considers this process an ultrasound-assisted extraction-centrifugation-ultrafiltration for purple sweet potato valorization in “green” technology.

  7. Preconcentration and determination of chlordiazepoxide and diazepam drugs using dispersive nanomaterial-ultrasound assisted microextraction method followed by high performance liquid chromatography.

    Science.gov (United States)

    Pebdani, A Amiri; Khodadoust, S; Talebianpoor, M S; Zargar, H R; Zarezade, V

    2016-01-01

    Benzodiazepines (BDs) are used widely in clinical practice, due to their multiple pharmacological functions. In this study a dispersive nanomaterial-ultrasound assisted- microextraction (DNUM) method followed by high performance liquid chromatography (HPLC) was used for the preconcentration and determination of chlordiazepoxide and diazepam drugs from urine and plasma samples. Various parameters such as amount of adsorbent (mg: ZnS-AC), pH and ionic strength of sample solution, vortex and ultrasonic time (min), and desorption volume (mL) were investigated by fractional factorial design (FFD) and central composite design (CCD). Regression models and desirability functions (DF) were applied to find the best experimental conditions for providing the maximum extraction recovery (ER). Under the optimal conditions a linear calibration curve were obtained in the range of 0.005-10μgmL(-1) and 0.006-10μgmL(-1) for chlordiazepoxide and diazepam, respectively. To demonstrate the analytical performance, figures of merits of the proposed method in urine and plasma spiked with chlordiazepoxide and diazepam were investigated. The limits of detection of chlordiazepoxide and diazepam in urine and plasma were ranged from 0.0012 to 0.0015μgmL(-1), respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Ultrasound-Assisted Liposuction Does Not Compromise the Regenerative Potential of Adipose-Derived Stem Cells.

    Science.gov (United States)

    Duscher, Dominik; Atashroo, David; Maan, Zeshaan N; Luan, Anna; Brett, Elizabeth A; Barrera, Janos; Khong, Sacha M; Zielins, Elizabeth R; Whittam, Alexander J; Hu, Michael S; Walmsley, Graham G; Pollhammer, Michael S; Schmidt, Manfred; Schilling, Arndt F; Machens, Hans-Günther; Huemer, Georg M; Wan, Derrick C; Longaker, Michael T; Gurtner, Geoffrey C

    2016-02-01

    Human mesenchymal stem cells (MSCs) have recently become a focus of regenerative medicine, both for their multilineage differentiation capacity and their excretion of proregenerative cytokines. Adipose-derived mesenchymal stem cells (ASCs) are of particular interest because of their abundance in fat tissue and the ease of harvest via liposuction. However, little is known about the impact of different liposuction methods on the functionality of ASCs. Here we evaluate the regenerative abilities of ASCs harvested via a third-generation ultrasound-assisted liposuction (UAL) device versus ASCs obtained via standard suction-assisted lipoaspiration (SAL). Lipoaspirates were sorted using fluorescent assisted cell sorting based on an established surface-marker profile (CD34+/CD31-/CD45-), to obtain viable ASCs. Yield and viability were compared and the differentiation capacities of the ASCs were assessed. Finally, the regenerative potential of ASCs was examined using an in vivo model of tissue regeneration. UAL- and SAL-derived samples demonstrated equivalent ASC yield and viability, and UAL ASCs were not impaired in their osteogenic, adipogenic, or chondrogenic differentiation capacity. Equally, quantitative real-time polymerase chain reaction showed comparable expression of most osteogenic, adipogenic, and key regenerative genes between both ASC groups. Cutaneous regeneration and neovascularization were significantly enhanced in mice treated with ASCs obtained by either UAL or SAL compared with controls, but there were no significant differences in healing between cell-therapy groups. We conclude that UAL is a successful method of obtaining fully functional ASCs for regenerative medicine purposes. Cells harvested with this alternative approach to liposuction are suitable for cell therapy and tissue engineering applications. Significance: Adipose-derived mesenchymal stem cells (ASCs) are an appealing source of therapeutic progenitor cells because of their multipotency

  9. Comparison of ultrasound-assisted extraction with conventional extraction methods of oil and polyphenols from grape (Vitis vinifera L.) seeds.

    Science.gov (United States)

    Da Porto, Carla; Porretto, Erica; Decorti, Deborha

    2013-07-01

    Ultrasound-assisted extraction (US) carried out at 20 KHz, 150 W for 30 min gave grape seed oil yield (14% w/w) similar to Soxhlet extraction (S) for 6 h. No significant differences for the major fatty acids was observed in oils extracted by S and US at 150 W. Instead, K232 and K268 of US- oils resulted lower than S-oil. From grape seeds differently defatted (S and US), polyphenols and their fractions were extracted by maceration for 12 h and by ultrasound-assisted extraction for 15 min. Sonication time was optimized after kinetics study on polyphenols extraction. Grape seed extracts obtained from seeds defatted by ultrasound (US) and then extracted by maceration resulted the highest in polyphenol concentration (105.20mg GAE/g flour) and antioxidant activity (109 Eq αToc/g flour). Copyright © 2013 Elsevier B.V. All rights reserved.

  10. The production of glucose from corn stalk using hydrothermal process with pre-treatment ultrasound assisted alkaline

    Science.gov (United States)

    Yolanda, Dora; Prasutiyo, Indry; Trisanti, P. N.; Sumarno

    2015-12-01

    The production of glucose from corn stalk by using subcritical hydrothermal technology is studied in this work. Ultrasound-assisted alkaline delignification methods are used as pre-treatment. The corn stalk powder were pretreated with ultrasound-assisted alkaline (NaOH 2% w/w, solid to liquid ratio 1:22 w/v) at room temperature and 30 minutes. After pre-treatment, solid residue and liquid fractions are separated by filtration. Pretreated solids are further submitted to hydrothermal process for glucose production. Hydrothermal process was carried out at 100 Bar and 120°C in various times. The solid product was characterized by SEM and XRD. And liquid product was analysis using DNS method to determine percentage of glucose. From XRD analysis showed that crystallinity of material was lower than delignification product.

  11. Ultrasound-assisted liposuction provides a source for functional adipose-derived stromal cells.

    Science.gov (United States)

    Duscher, Dominik; Maan, Zeshaan N; Luan, Anna; Aitzetmüller, Matthias M; Brett, Elizabeth A; Atashroo, David; Whittam, Alexander J; Hu, Michael S; Walmsley, Graham G; Houschyar, Khosrow S; Schilling, Arndt F; Machens, Hans-Guenther; Gurtner, Geoffrey C; Longaker, Michael T; Wan, Derrick C

    2017-12-01

    Regenerative medicine employs human mesenchymal stromal cells (MSCs) for their multi-lineage plasticity and their pro-regenerative cytokine secretome. Adipose-derived mesenchymal stromal cells (ASCs) are concentrated in fat tissue, and the ease of harvest via liposuction makes them a particularly interesting cell source. However, there are various liposuction methods, and few have been assessed regarding their impact on ASC functionality. Here we study the impact of the two most popular ultrasound-assisted liposuction (UAL) devices currently in clinical use, VASER (Solta Medical) and Lysonix 3000 (Mentor) on ASCs. After lipoaspirate harvest and processing, we sorted for ASCs using fluorescent-assisted cell sorting based on an established surface marker profile (CD34 + CD31 - CD45 - ). ASC yield, viability, osteogenic and adipogenic differentiation capacity and in vivo regenerative performance were assessed. Both UAL samples demonstrated equivalent ASC yield and viability. VASER UAL ASCs showed higher osteogenic and adipogenic marker expression, but a comparable differentiation capacity was observed. Soft tissue healing and neovascularization were significantly enhanced via both UAL-derived ASCs in vivo, and there was no significant difference between the cell therapy groups. Taken together, our data suggest that UAL allows safe and efficient harvesting of the mesenchymal stromal cellular fraction of adipose tissue and that cells harvested via this approach are suitable for cell therapy and tissue engineering applications. Copyright © 2017 International Society for Cellular Therapy. Published by Elsevier Inc. All rights reserved.

  12. Ultrasound assisted combustion synthesis of TiC in Al-Ti-C system.

    Science.gov (United States)

    Liu, Zhiwei; Rakita, Milan; Xu, Wilson; Wang, Xiaoming; Han, Qingyou

    2015-11-01

    This research investigated the effects of high-intensity ultrasound on the combustion synthesis of TiC particles in Al-Ti-C system. The process involved that high-intensity ultrasound was applied on the surface of a compacted Al-Ti-C pellet directly through a Nb probe during the thermal explosion reaction. By comparing with the sample without ultrasonic treatment, it was found that the thermal explosion reaction for synthesizing TiC phase could take place thoroughly in the ultrasonically treated sample. During the process of synthesizing TiC phase, the dissolution of solid graphite particles into the Al-Ti melt, as well as the nucleation and growth of TiC particles could be promoted effectively due to the effects of ultrasound, leading to an enhancement of the formation of TiC particles. Ultrasound assisted combustion synthesis as a simple and effective approach was proposed for synthesizing materials in this research. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Ultrasound Assisted Extraction for the Recovery of Phenolic Compounds from Vegetable Sources

    Directory of Open Access Journals (Sweden)

    Nelly Medina-Torres

    2017-07-01

    Full Text Available Vegetable sources and agro-industrial residues represent an important source of phenolic compounds that are useful in a wide range of applications, especially those with biological activities. Conventional techniques of phytochemical extraction have been associated with a high consumption of organic solvents that limits the application of bioactive extracts, leading to the implementation of novel extraction technologies using mechanisms such as Ultrasound Assisted Extraction (UAE. In the present review, an analysis of the involved variables in the extraction yield of phenolic compounds through UAE is presented, highlighting the advantages of this technology based on the results obtained in various optimized studies. A comparison with other technologies and a proposal of its possible application for agro industrial residues as raw material of phenolic compounds is also indicated. Finally, it is concluded that UAE is a technology that is placed within the area of Sustainable Chemistry since it promotes the use of renewable raw materials through the extraction of phenolic compounds, implementing the substitution of organic solvents with solvents that do not present toxic effects, lowering the energy consumption when compared to conventional methods and minimizing process times and temperatures, which is useful for the extraction of thermo-labile compounds.

  14. Optimized Ultrasound-Assisted Extraction of Phenolic Compounds from Polygonum cuspidatum

    Directory of Open Access Journals (Sweden)

    Chia-Hung Kuo

    2013-12-01

    Full Text Available In this study the phenolic compounds piceid, resveratrol and emodin were extracted from P. cuspidatum roots using ultrasound-assisted extraction. Multiple response surface methodology was used to optimize the extraction conditions of these phenolic compounds. A three-factor and three-level Box-Behnken experimental design was employed to evaluate the effects of the operation parameters, including extraction temperature (30–70 °C, ethanol concentration (40%–80%, and ultrasonic power (90–150 W, on the extraction yields of piceid, resveratrol, and emodin. The statistical models built from multiple response surface methodology were developed for the estimation of the extraction yields of multi-phenolic components. Based on the model, the extraction yields of piceid, resveratrol, and emodin can be improved by controlling the extraction parameters. Under the optimum conditions, the extraction yields of piceid, resveratrol and emodin were 10.77 mg/g, 3.82 mg/g and 11.72 mg/g, respectively.

  15. Optimization of Ultrasound-Assisted Extraction of Natural Antioxidants from the Osmanthus fragrans Flower.

    Science.gov (United States)

    Li, An-Na; Li, Sha; Li, Ya; Xu, Dong-Ping; Li, Hua-Bin

    2016-02-18

    An ultrasound-assisted extraction (UAE) method was developed to extract natural antioxidants from the Osmanthus fragrans flower. The effect of UAE on antioxidant activity of the extract from the Osmanthus fragrans flower was studied using a Trolox equivalent antioxidant capacity (TEAC) assay. Optimization conditions were firstly determined using a single-factor experiment, and response surface methodology was then used to evaluate interaction of several experimental parameters. Analysis of the coefficient of determination showed that second-order polynomial models produced a highly satisfactory fitting of the experimental data with regard to TEAC values (R² = 0.9829, p extraction for 35.2 min at 59.4 °C. Under these conditions, the maximum TEAC value was 584.9 ± 6.0 μmol Trolox/g DW, which was higher than those obtained by the conventional extracting method (486.4 ± 12.6 μmol Trolox/g DW) and the Soxhlet extraction method (339.1 ± 16.2 μmol Trolox/g DW). The crude extract obtained could be used either as a food additive or in pharmaceuticals for the prevention and treatment of diseases caused by oxidative stress.

  16. Optimization of Ultrasound-Assisted Extraction of Antioxidants from the Mung Bean Coat.

    Science.gov (United States)

    Zhou, Yue; Zheng, Jie; Gan, Ren-You; Zhou, Tong; Xu, Dong-Ping; Li, Hua-Bin

    2017-04-15

    Mung bean ( Vigna radiata ) sprout is commonly consumed as a vegetable, while the coat of the germinated mung bean is a waste. In this paper, an ultrasound-assisted extraction method has been developed to extract natural antioxidants from the seed coat of mung bean. Several experimental parameters-which included ethanol concentration, solvent/material ratio, ultrasound extraction time, temperature, and power-were studied in single-factor experiments. The interaction of three key experimental parameters (ethanol concentration, solvent/material ratio, and ultrasonic extraction time) was further investigated by response surface method. Besides, traditional extracting methods, including maceration and Soxhlet extraction methods, were also carried out for comparison. The results suggested that the best extracting condition was 37.6% ( v / v ) of ethanol concentration, 35.1:1 mL/g of solvent/material ratio and ultrasonic extraction of 46.1 min at 70 °C under 500 W ultrasonic irradiation. The antioxidant capacity (178.28 ± 7.39 µmol Trolox/g DW) was much stronger than those obtained by the maceration extraction process (158.66 ± 4.73 µmol Trolox/g DW) and the Soxhlet extraction process (138.42 ± 3.63 µmol Trolox/g DW). In addition, several antioxidant components in the extract were identified and quantified. This study is helpful for value-added utilization of the waste from germinated mung bean.

  17. Ultrasound-assisted extraction of polyphenols from native plants in the Mexican desert.

    Science.gov (United States)

    Wong Paz, Jorge E; Muñiz Márquez, Diana B; Martínez Ávila, Guillermo C G; Belmares Cerda, Ruth E; Aguilar, Cristóbal N

    2015-01-01

    Several plants that are rich in polyphenolic compounds and exhibit biological properties are grown in the desert region of Mexico under extreme climate conditions. These compounds have been recovered by classic methodologies in these plants using organic solvents. However, little information is available regarding the use of alternative extraction technologies, such as ultrasound. In this paper, ultrasound-assisted extraction (UAE) parameters, such as the liquid:solid ratio, solvent concentration and extraction time, were studied using response surface methodology (RSM) for the extraction of polyphenols from desert plants including Jatrophadioica,Flourensiacernua, Turneradiffusa and Eucalyptuscamaldulensis. Key process variables (i.e., liquid:solid ratio and ethanol concentration) exert the greatest influence on the extraction of all of the phenolic compounds (TPC) in the studied plants. The best conditions for the extraction of TPC involved an extraction time of 40min, an ethanol concentration of 35% and a liquid:solid ratio ranging from 8 to 12mlg(-1) depending on the plant. The highest antioxidant activity was obtained in the E. camaldulensis extracts. The results indicated the ability of UAE to obtain polyphenolic antioxidant preparations from desert plants. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Ultrasound-Assisted Extraction and Characterization of Pectic Polysaccharide from Oriental Tobacco Leaves

    International Nuclear Information System (INIS)

    Liu, S.; Tian, Z.; Li, X.; He, P.; Xu, C.

    2015-01-01

    Ultrasound-assisted extraction (UAE) of pectic Polysaccharide from oriental tobacco leaves was studied by orthogonal matrix method (L9(3)4). Furthermore, the crude Polysaccharide was purified and two components (Fr-I and Fr-II) were obtained. FT-IR spectral analysis of the purified EPS revealed prominent characteristic groups. The monosaccharide composition analysis indicated the main composition between Fr-I and Fr-II was different. Furthermore, thermo gravimetric analysis (TGA) indicated the degradation temperature (Td) of the Fr-I (215 degree C) was higher than those of Fr-II (162 degree C). Detected by the pyrolysis GC/MS, though the main kinds of pyrolysis products from both Fr-I and Fr-II were similar, the larger amount of heterocycle and aromatic compounds liberated after hydrolysis of Fr-II. Finally, On the basis of the antioxidant activity test in vitro, Fr-II has stronger antioxidant activities than Fr-I. The thermal behavior and antioxidant activity might be attributed to the configuration of the sugar units and chemical compositions. (author)

  19. Ultrasound-Assisted Extraction, Antioxidant and Anticancer Activities of the Polysaccharides from Rhynchosia minima Root.

    Science.gov (United States)

    Jia, Xuejing; Zhang, Chao; Hu, Jie; He, Muxue; Bao, Jiaolin; Wang, Kai; Li, Peng; Chen, Meiwan; Wan, Jianbo; Su, Huanxing; Zhang, Qingwen; He, Chengwei

    2015-11-23

    Box-Behnken design (BBD), one of the most common response surface methodology (RSM) methods, was used to optimize the experimental conditions for ultrasound-assisted extraction of polysaccharides from Rhynchosia minima root (PRM). The antioxidant abilities and anticancer activity of purified polysaccharide fractions were also measured. The results showed that optimal extraction parameters were as follows: ultrasound exposure time, 21 min; ratio of water to material, 46 mL/g; ultrasound extraction temperature, 63 °C. Under these conditions, the maximum yield of PRM was 16.95%±0.07%. Furthermore, the main monosaccharides of purified fractions were Ara and Gal. PRM3 and PRM5 exhibited remarkable DPPH radical scavenging activities and reducing power in vitro. PRM3 showed strong inhibitory activities on the growth of MCF-7 cells in vitro. The above results indicate that polysaccharides from R. minima root have the potential to be developed as natural antioxidants and anticancer ingredients for the food and pharmaceutical industries.

  20. Batch and Continuous Ultrasound Assisted Extraction of Boldo Leaves (Peumus boldus Mol.)

    Science.gov (United States)

    Petigny, Loïc; Périno-Issartier, Sandrine; Wajsman, Joël; Chemat, Farid

    2013-01-01

    Vegetal extracts are widely used as primary ingredients for various products from creams to perfumes in the pharmaceutical, nutraceutic and cosmetic industries. Having concentrated and active extract is essential, as the process must extract as much soluble material as possible in a minimum time, using the least possible volume of solvent. The boldo leaves extract is of great interest for the industry as it holds a great anti-oxidant activity due to high levels of flavonoids and alkaloids such as boldine. Ultrasound Assisted Extraction (UAE) has been used to improve the efficiency of the plant extraction, reducing extraction time, increasing the concentration of the extract with the same amount of solvent and plant material. After a preliminary study, a response surface method has been used to optimize the extraction of soluble material from the plant. The results provided by the statistical analysis revealed that the optimized conditions were: sonication power 23 W/cm2 for 40 min and a temperature of 36 °C. The optimized parameters of the UAE provide a better extraction compared to a conventional maceration in terms of process time (30 min instead of 120 min), higher yield, more energy saving, cleanliness, safety and product quality. PMID:23481637

  1. Batch and Continuous Ultrasound Assisted Extraction of Boldo Leaves (Peumus boldus Mol.

    Directory of Open Access Journals (Sweden)

    Joël Wajsman

    2013-03-01

    Full Text Available Vegetal extracts are widely used as primary ingredients for various products from creams to perfumes in the pharmaceutical, nutraceutic and cosmetic industries. Having concentrated and active extract is essential, as the process must extract as much soluble material as possible in a minimum time, using the least possible volume of solvent. The boldo leaves extract is of great interest for the industry as it holds a great anti-oxidant activity due to high levels of flavonoids and alkaloids such as boldine. Ultrasound Assisted Extraction (UAE has been used to improve the efficiency of the plant extraction, reducing extraction time, increasing the concentration of the extract with the same amount of solvent and plant material. After a preliminary study, a response surface method has been used to optimize the extraction of soluble material from the plant. The results provided by the statistical analysis revealed that the optimized conditions were: sonication power 23 W/cm2 for 40 min and a temperature of 36 °C. The optimized parameters of the UAE provide a better extraction compared to a conventional maceration in terms of process time (30 min instead of 120 min, higher yield, more energy saving, cleanliness, safety and product quality.

  2. Ultrasound assisted lipase catalyzed synthesis of cinnamyl acetate via transesterification reaction in a solvent free medium.

    Science.gov (United States)

    Tomke, Prerana D; Rathod, Virendra K

    2015-11-01

    Cinnamyl acetate is known for its use as flavor and fragrance material in different industries such as food, pharmaceutical, cosmetic etc. This work focuses on ultrasound assisted lipase (Novozym 435) catalyzed synthesis of cinnamyl acetate via transesterification of cinnamyl alcohol and vinyl acetate in non-aqueous, solvent free system. Optimization of various parameters shows that a higher yield of 99.99% can be obtained at cinnamyl alcohol to vinyl acetate ratio of 1:2 with 0.2% of catalyst, at 40°C and 150 rpm, with lower ultrasound power input of 50 W (Ultrasound intensity 0.81 W/cm(2)), at 25 kHz frequency, 50% duty cycle. Further, the time required for the maximum conversion is reduced to 20 min as compared to 60 min of conventional process. Similarly, the enzyme can be successfully reused seven times without loss of enzyme activity. Thus, ultrasound helps to enhance the enzyme catalyzed synthesis of flavors. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Ultrasound-assisted lipase-catalyzed transesterification of soybean oil in organic solvent system.

    Science.gov (United States)

    Batistella, Luciane; Lerin, Lindomar A; Brugnerotto, Patrícia; Danielli, Angélica J; Trentin, Cláudia M; Popiolski, Ariana; Treichel, Helen; Oliveira, J Vladimir; de Oliveira, Débora

    2012-05-01

    This work reports the transesterification of soybean oil with ethanol using two commercial immobilized lipases under the influence of ultrasound irradiation. The experiments were performed in an ultrasonic water bath, following a sequence of experimental designs to assess the effects of temperature, enzyme and water concentrations, oil to ethanol molar ratio and output irradiation power on the reaction yield. Results show that ultrasound-assisted lipase-catalyzed transesterification of soybean oil with ethanol might be a potential alternative route to conventional alkali-catalyzed method, as high reaction yields (~90 wt.%) were obtained at mild irradiation power supply (~100 W), and temperature (60 °C) in a relatively short reaction time, 4h, using Lipozyme RM IM as catalyst. The repeated use of the catalyst under the optimum experimental condition resulted in a decay in both enzyme activity and product conversion after two cycles. The use of Novozym 435 led to lower conversions (about 57%) but the enzyme activity was stable after eight cycles of use, showing, however, a reduction in product conversion after the forth cycle. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Laminarin from Irish Brown Seaweeds Ascophyllum nodosum and Laminaria hyperborea: Ultrasound Assisted Extraction, Characterization and Bioactivity

    Directory of Open Access Journals (Sweden)

    Shekhar U. Kadam

    2015-07-01

    Full Text Available Ultrasound assisted extraction (UAE, purification, characterization and antioxidant activity of laminarin from Irish brown seaweeds Ascophyllum nodosum and Laminarina hyperborea were investigated. UAE was carried out using 60% ultrasonic power amplitude and 0.1 M hydrochloric acid for 15 min. Separately, solid-liquid extraction was carried in an orbital shaker using 0.1 M hydrochloric acid at 70 °C for 2.5 h. UAE with hydrochloric acid resulted in the highest concentration of laminarin, 5.82% and 6.24% on dry weight basis from A. nodosum and L. hyperborea, respectively. Purification of all extracts was carried out using molecular weight cut off dialysis at 10 kDa. Characterization of the laminarin fraction was carried out using matrix assisted laser desorption/ionization time-of-flight mass spectrometry. Antioxidant activity of A. nodosum and L. hyperborea extracts had 2,2-diphenyl-1-picrylhydrazyl (DPPH inhibition levels of 93.23% and 87.57%, respectively. Moreover, these extracts have shown inihibition of bacterial growth of Staphylcoccus aureus, Listeria monocytogenes, Escherichia coli and Salmonella typhimurium.

  5. Laminarin from Irish Brown Seaweeds Ascophyllum nodosum and Laminaria hyperborea: Ultrasound Assisted Extraction, Characterization and Bioactivity.

    Science.gov (United States)

    Kadam, Shekhar U; O'Donnell, Colm P; Rai, Dilip K; Hossain, Mohammad B; Burgess, Catherine M; Walsh, Des; Tiwari, Brijesh K

    2015-07-10

    Ultrasound assisted extraction (UAE), purification, characterization and antioxidant activity of laminarin from Irish brown seaweeds Ascophyllum nodosum and Laminarina hyperborea were investigated. UAE was carried out using 60% ultrasonic power amplitude and 0.1 M hydrochloric acid for 15 min. Separately, solid-liquid extraction was carried in an orbital shaker using 0.1 M hydrochloric acid at 70 °C for 2.5 h. UAE with hydrochloric acid resulted in the highest concentration of laminarin, 5.82% and 6.24% on dry weight basis from A. nodosum and L. hyperborea, respectively. Purification of all extracts was carried out using molecular weight cut off dialysis at 10 kDa. Characterization of the laminarin fraction was carried out using matrix assisted laser desorption/ionization time-of-flight mass spectrometry. Antioxidant activity of A. nodosum and L. hyperborea extracts had 2,2-diphenyl-1-picrylhydrazyl (DPPH) inhibition levels of 93.23% and 87.57%, respectively. Moreover, these extracts have shown inihibition of bacterial growth of Staphylcoccus aureus, Listeria monocytogenes, Escherichia coli and Salmonella typhimurium.

  6. Ultrasound-assisted extraction method for the simultaneous determination of emerging contaminants in freshwater sediments.

    Science.gov (United States)

    de Sousa, Diana Nara Ribeiro; Grosseli, Guilherme Martins; Mozeto, Antonio Aparecido; Carneiro, Renato Lajarim; Fadini, Pedro Sergio

    2015-10-01

    Sediments are the fate of several emerging organic contaminants, such as pharmaceuticals, personal care products and hormones, and therefore an important subject in environmental monitoring studies. In the present work, a simple and sensitive method was developed, validated and applied for the simultaneous extraction of atenolol, caffeine, carbamazepine, diclofenac, ibuprofen, naproxen, propranolol, triclosan, estrone, 17-β-estradiol and 17-α-ethinylestradiol using ultrasound-assisted extraction from freshwater sediment samples followed by solid-phase extraction clean-up and liquid chromatography with tandem mass spectrometry detection. The solvent type and extraction pH were evaluated to obtain the highest recoveries of the compounds. The best method shows absolute recoveries between 54.0 and 94.4% at 50 ng/g concentration. The method exhibits good precision with relative standard deviation ranging from 1.0-16%. The detection and quantification limits ranged from 0.006-0.067 and 0.016-0.336 ng/g, respectively. The developed method was successfully applied to freshwater sediment samples collected from different sites in Jundiaí River basin of São Paulo State, Brazil. The compounds atenolol, caffeine, propranolol and triclosan were detected in all the sampling sites with concentrations of 13.8, 41.0, 28.5 and 176 ng/g, respectively. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Ultrasound-assisted enzymatic extraction and antioxidant activity of polysaccharides from pumpkin (Cucurbita moschata).

    Science.gov (United States)

    Wu, Hao; Zhu, Junxiang; Diao, Wenchao; Wang, Chengrong

    2014-11-26

    An efficient ultrasound-assisted enzymatic extraction (UAEE) of Cucurbita moschata polysaccharides (CMCP) was established and the CMCP antioxidant activities were studied. The UAEE operating parameters (extraction temperature, ultrasonic power, pH, and liquid-to-material ratio) were optimized using the central composite design (CCD) and the mass transfer kinetic study in UAEE procedure was used to select the optimal extraction time. Enzymolysis and ultrasonication that were simultaneously conducted was selected as the UAEE synergistic model and the optimum extraction conditions with a maximum polysaccharide yield of 4.33 ± 0.15% were as follows: extraction temperature, 51.5 °C; ultrasonic power, 440 W; pH, 5.0; liquid-to-material ratio, 5.70:1 mL/g; and extraction time, 20 min. Evaluation of the antioxidant activity in vitro suggested that CMCP has good potential as a natural antioxidant used in the food or medicine industry because of their high reducing power and positive radical scavenging activity for DPPH radical. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. Ultrasound-assisted production of biodiesel and ethanol from spent coffee grounds.

    Science.gov (United States)

    Rocha, Maria Valderez Ponte; de Matos, Leonardo José Brandão Lima; Lima, Larissa Pinto de; Figueiredo, Pablo Marciano da Silva; Lucena, Izabelly Larissa; Fernandes, Fabiano André Narciso; Gonçalves, Luciana Rocha Barros

    2014-09-01

    This study evaluates the production of biodiesel and ethanol from spent coffee grounds (SCG). The extraction of oil from SCG, biodiesel production and ethanol production processes were studied. The liquid-to-solid ratio and temperature were evaluated in the ultrasound-assisted extraction of the oil from SCG. The highest yield (12%) was obtained using 4 mL g(-1) liquid-to-solid ratio at 60°C for 45 min. The process to produce biodiesel showed a yield of 97% into fatty acid methyl esters (FAME). The highest glucose yield (192 mg g SCG(-1)) was obtained by hydrolysis with 0.4 mol L(-1) sulfuric acid at 121°C for 15 min. The hydrolysate was used as fermentation medium for ethanol production by Saccharomyces cerevisiae obtaining 19.0 g L(-1) at 10h of process of ethanol with a yield of ethanol and productivity of 0.50 g g(-1) and 1.90 g L(-1)h(-1), respectively. Spent coffee grounds were considered a potential feedstock for biodiesel and ethanol production. Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. Mapping of an ultrasonic bath for ultrasound assisted extraction of mangiferin from Mangifera indica leaves.

    Science.gov (United States)

    Kulkarni, Vrushali M; Rathod, Virendra K

    2014-03-01

    The present work deals with the mapping of an ultrasonic bath for the maximum extraction of mangiferin from Mangifera indica leaves. I3(-) liberation experiments (chemical transformations) and extraction (physical transformations) were carried out at different locations in an ultrasonic bath and compared. The experimental findings indicated a similar trend in variation in an ultrasonic bath by both these methods. Various parameters such as position and depth of vessel in an ultrasonic bath, diameter and shape of a vessel, frequency and input power which affect the extraction yield have been studied in detail. Maximum yield of mangiferin obtained was approximately 31 mg/g at optimized parameters: distance of 2.54 cm above the bottom of the bath, 7 cm diameter of vessel, flat bottom vessel, 6.35 cm liquid height, 122 W input power and 25 kHz frequency. The present work indicates that the position and depth of vessel in an ultrasonic bath, diameter and shape of a vessel, frequency and input power have significant effect on the extraction yield. This work can be used as a base for all ultrasonic baths to obtain maximum efficiency for ultrasound assisted extraction. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Evaluation of ultrasound assisted potassium permanganate pre-treatment of spent coffee waste.

    Science.gov (United States)

    Ravindran, Rajeev; Jaiswal, Swarna; Abu-Ghannam, Nissreen; Jaiswal, Amit K

    2017-01-01

    In the present study, novel pre-treatment for spent coffee waste (SCW) has been proposed which utilises the superior oxidising capacity of alkaline KMnO 4 assisted by ultra-sonication. The pre-treatment was conducted for different exposure times (10, 20, 30 and 40min) using different concentrations of KMnO 4 (1, 2, 3, 4, 5%w/v) at room temperature with solid/liquid ratio of 1:10. Pretreating SCW with 4% KMnO 4 and exposing it to ultrasound for 20min resulted in 98% cellulose recovery and a maximum lignin removal of 46%. 1.7 fold increase in reducing sugar yield was obtained after enzymatic hydrolysis of KMnO 4 pretreated SCW as compared to raw. SEM, XRD and FTIR analysis of the pretreated SCW revealed the various effects of pretreatment. Thermal behaviour of the pretreated substrate against the native biomass was also studied using DSC. Ultrasound-assisted potassium permanganate oxidation was found to be an effective pretreatment for SCW, and can be a used as a potential feedstock pretreatment strategy for bioethanol production. Copyright © 2016 Elsevier Ltd. All rights reserved.

  11. Ultrasound-assisted extraction of polyphenols from Thymus serpyllum and its antioxidant activity

    Directory of Open Access Journals (Sweden)

    Jovanović Aleksandra A.

    2016-01-01

    Full Text Available The present study was designed to establish and optimize a method for extracting natural bioactive compounds from Thymus serpyllum which possess antioxidant, antimicrobial, antispasmotic and stimulant properties. Ultrasound-assisted extraction (UAE is a well-established method in the processing of plant material, particularly for extraction of bioactive substances such as polyphenols. The influential factors including extraction time (3, 7 and 10 minutes, solid:solvent ratio (1:10, 1:20 and 1:30 and particle size (0.3, 0.7 and 1.5 mm, have been studied to optimize the extraction process, while using 30% ethanol as an extraction medium and amplitude set to 65%. The yield of UAE was expressed via total phenol content and antioxidant activity of the obtained extracts. The optimum process paremeters were found to be: extraction time, 3 min; solid:solvent ratio, 1:30; particle size, 0.3 mm. Under these conditions, the yield of total polyphenols was raised up to 23.03 mg/L GA and the highest antioxidant activity was recorded (10.32 mmol/mg Trolox and IC50 3.00 mg/ml. [Projekat Ministarstva nauke Republike Srbije, br. 46010 i br. 46013

  12. Optimization of Ficus deltoidea Using Ultrasound-Assisted Extraction by Box-Behnken Statistical Design

    Directory of Open Access Journals (Sweden)

    L. J. Ong

    2016-09-01

    Full Text Available In this study, the effect of extraction parameters (ethanol concentration, sonication time, and solvent-to-sample ratio on Ficus deltoidea leaves was investigated using ultrasound-assisted extraction by response surface methodology (RSM. Total phenolic content (TPC of F. deltoidea extracts was identified using Folin-Ciocalteu method and expressed in gallic acid equivalent (GAE per g. Box-Behnken statistical design (BBD was the tool used to find the optimal conditions for maximum TPC. Besides, the extraction yield was measured and stated in percentage. The optimized TPC attained was 455.78 mg GAE/g at 64% ethanol concentration, 10 minutes sonication time, and 20 mL/g solvent-to-sample ratio whereas the greatest extraction yield was 33% with ethanol concentration of 70%, sonication time of 40 minutes, and solvent-to-material ratio at 40 mL/g. The determination coefficient, R2, for TPC indicates that 99.5% capriciousness in the response could be clarified by the ANOVA model and the value of 0.9681 of predicted R2 is in equitable agreement with the 0.9890 of adjusted R2. The present study shows that ethanol water as solvent, a short time of 10 minutes, and adequate solvent-to-sample ratio (20 mL/g are the best conditions for extraction.

  13. Optimization of ultrasound-assisted extraction of charantin from Momordica charantia fruits using response surface methodology.

    Science.gov (United States)

    Ahamad, Javed; Amin, Saima; Mir, Showkat R

    2015-01-01

    Momordica charantia Linn. (Cucurbitaceae) fruits are well known for their beneficial effects in diabetes that are often attributed to its bioactive component charantin. The aim of the present study is to develop and optimize an efficient protocol for the extraction of charantin from M. charantia fruits. Response surface methodology (RSM) was used for the optimization of ultrasound-assisted extraction (UAE) conditions. RSM was based on a three-level, three-variable Box-Behnken design (BBD), and the studied variables included solid to solvent ratio, extraction temperature, and extraction time. The optimal conditions predicted by the BBD were: UAE with methanol: Water (80:20, v/v) at 46°C for 120 min with solid to solvent ratio of 1:26 w/v, under which the yield of charantin was 3.18 mg/g. Confirmation trials under slightly adjusted conditions yielded 3.12 ± 0.14 mg/g of charantin on dry weight basis of fruits. The result of UAE was also compared with Soxhlet extraction method and UAE was found 2.74-fold more efficient than the Soxhlet extraction for extracting charantin. A facile UAE protocol for a high extraction yield of charantin was developed and validated.

  14. Optimization of ultrasound-assisted extraction of charantin from Momordica charantia fruits using response surface methodology

    Directory of Open Access Journals (Sweden)

    Javed Ahamad

    2015-01-01

    Full Text Available Background: Momordica charantia Linn. (Cucurbitaceae fruits are well known for their beneficial effects in diabetes that are often attributed to its bioactive component charantin. Objective: The aim of the present study is to develop and optimize an efficient protocol for the extraction of charantin from M. charantia fruits. Materials and Methods: Response surface methodology (RSM was used for the optimization of ultrasound-assisted extraction (UAE conditions. RSM was based on a three-level, three-variable Box-Behnken design (BBD, and the studied variables included solid to solvent ratio, extraction temperature, and extraction time. Results: The optimal conditions predicted by the BBD were: UAE with methanol: Water (80:20, v/v at 46°C for 120 min with solid to solvent ratio of 1:26 w/v, under which the yield of charantin was 3.18 mg/g. Confirmation trials under slightly adjusted conditions yielded 3.12 ± 0.14 mg/g of charantin on dry weight basis of fruits. The result of UAE was also compared with Soxhlet extraction method and UAE was found 2.74-fold more efficient than the Soxhlet extraction for extracting charantin. Conclusions:A facile UAE protocol for a high extraction yield of charantin was developed and validated.

  15. Optimization of ultrasound-assisted extraction of charantin from Momordica charantia fruits using response surface methodology

    Science.gov (United States)

    Ahamad, Javed; Amin, Saima; Mir, Showkat R.

    2015-01-01

    Background: Momordica charantia Linn. (Cucurbitaceae) fruits are well known for their beneficial effects in diabetes that are often attributed to its bioactive component charantin. Objective: The aim of the present study is to develop and optimize an efficient protocol for the extraction of charantin from M. charantia fruits. Materials and Methods: Response surface methodology (RSM) was used for the optimization of ultrasound-assisted extraction (UAE) conditions. RSM was based on a three-level, three-variable Box-Behnken design (BBD), and the studied variables included solid to solvent ratio, extraction temperature, and extraction time. Results: The optimal conditions predicted by the BBD were: UAE with methanol: Water (80:20, v/v) at 46°C for 120 min with solid to solvent ratio of 1:26 w/v, under which the yield of charantin was 3.18 mg/g. Confirmation trials under slightly adjusted conditions yielded 3.12 ± 0.14 mg/g of charantin on dry weight basis of fruits. The result of UAE was also compared with Soxhlet extraction method and UAE was found 2.74-fold more efficient than the Soxhlet extraction for extracting charantin. Conclusions: A facile UAE protocol for a high extraction yield of charantin was developed and validated. PMID:26681889

  16. Ultrasound assisted supercritical fluid extraction of oil and coixenolide from adlay seed.

    Science.gov (United States)

    Hu, Ai-jun; Zhao, Shuna; Liang, Hanhua; Qiu, Tai-qiu; Chen, Guohua

    2007-02-01

    Oil and coixenolide are important components of adlay seed (Coix lachrymal-jobi L. var. Adlay) with many beneficial functions to human health. In this work, a novel extraction technique--ultrasound assisted supercritical fluid extraction (USFE)--was studied. Effects of operating conditions on the extraction, including extraction temperature (T), pressure (P), time (t), CO(2) flow rate (F) and ultrasonic power (I) were investigated. There are optimum temperatures which gives the maximum extraction yields (EYs) for the supercritical fluid extractions with and without ultrasound. The effect of pressure on EYs for is similar to that of pressure on CO(2) density. Based on the yield of extraction, the favorable conditions for supercritical fluid extraction (SFE) were: T at 45 degrees C, P at 25 MPa, t at 4.0 h and F at 3.5L/h. While ultrasound was applied as in USFE, the following parameters were preferred: T at 40 degrees C, P at 20 MPa, t at 3.5h and F at 3.0 L/h, respectively. The results show that supercritical fluid extraction with the assistance of ultrasound could reduce the temperature, pressure, CO(2) flow rate, as well as time used in the process. Compared with SFE, USFE could give a 14% increase in the yield for extracting oil and coixenolide from adlay seed with less severe operating conditions.

  17. Ultrasound-Assisted Extraction, Antioxidant and Anticancer Activities of the Polysaccharides from Rhynchosia minima Root

    Directory of Open Access Journals (Sweden)

    Xuejing Jia

    2015-11-01

    Full Text Available Box-Behnken design (BBD, one of the most common response surface methodology (RSM methods, was used to optimize the experimental conditions for ultrasound-assisted extraction of polysaccharides from Rhynchosia minima root (PRM. The antioxidant abilities and anticancer activity of purified polysaccharide fractions were also measured. The results showed that optimal extraction parameters were as follows: ultrasound exposure time, 21 min; ratio of water to material, 46 mL/g; ultrasound extraction temperature, 63 °C. Under these conditions, the maximum yield of PRM was 16.95% ± 0.07%. Furthermore, the main monosaccharides of purified fractions were Ara and Gal. PRM3 and PRM5 exhibited remarkable DPPH radical scavenging activities and reducing power in vitro. PRM3 showed strong inhibitory activities on the growth of MCF-7 cells in vitro. The above results indicate that polysaccharides from R. minima root have the potential to be developed as natural antioxidants and anticancer ingredients for the food and pharmaceutical industries.

  18. Ultrasound-Assist Extrusion Methods for the Fabrication of Polymer Nanocomposites Based on Polypropylene/Multi-Wall Carbon Nanotubes

    Directory of Open Access Journals (Sweden)

    Carlos A. Ávila-Orta

    2015-11-01

    Full Text Available Isotactic polypropylenes (iPP with different melt flow indexes (MFI were used to fabricate nanocomposites (NCs with 10 wt % loadings of multi-wall carbon nanotubes (MWCNTs using ultrasound-assisted extrusion methods to determine their effect on the morphology, melt flow, and electrical properties of the NCs. Three different types of iPPs were used with MFIs of 2.5, 34 and 1200 g/10 min. Four different NC fabrication methods based on melt extrusion were used. In the first method melt extrusion fabrication without ultrasound assistance was used. In the second and third methods, an ultrasound probe attached to a hot chamber located at the exit of the die was used to subject the sample to fixed frequency and variable frequency, respectively. The fourth method is similar to the first method, with the difference being that the carbon nanotubes were treated in a fluidized air-bed with an ultrasound probe before being used in the fabrication of the NCs with no ultrasound assistance during extrusion. The samples were characterized by MFI, Optical microscopy (OM, Scanning electron microscopy (SEM, Transmission electron microscopy (TEM, electrical surface resistivity, and electric charge. MFI decreases in all cases with addition of MWCNTs with the largest decrease observed for samples with the highest MFI. The surface resistivity, which ranged from 1013 to 105 Ω/sq, and electric charge, were observed to depend on the ultrasound-assisted fabrication method as well as on the melt flow index of the iPP. A relationship between agglomerate size and area ratio with electric charge was found. Several trends in the overall data were identified and are discussed in terms of MFI and the different fabrication methods.

  19. Ultrasound-Assist Extrusion Methods for the Fabrication of Polymer Nanocomposites Based on Polypropylene/Multi-Wall Carbon Nanotubes

    Science.gov (United States)

    Ávila-Orta, Carlos A.; Quiñones-Jurado, Zoe V.; Waldo-Mendoza, Miguel A.; Rivera-Paz, Erika A.; Cruz-Delgado, Víctor J.; Mata-Padilla, José M.; González-Morones, Pablo; Ziolo, Ronald F.

    2015-01-01

    Isotactic polypropylenes (iPP) with different melt flow indexes (MFI) were used to fabricate nanocomposites (NCs) with 10 wt % loadings of multi-wall carbon nanotubes (MWCNTs) using ultrasound-assisted extrusion methods to determine their effect on the morphology, melt flow, and electrical properties of the NCs. Three different types of iPPs were used with MFIs of 2.5, 34 and 1200 g/10 min. Four different NC fabrication methods based on melt extrusion were used. In the first method melt extrusion fabrication without ultrasound assistance was used. In the second and third methods, an ultrasound probe attached to a hot chamber located at the exit of the die was used to subject the sample to fixed frequency and variable frequency, respectively. The fourth method is similar to the first method, with the difference being that the carbon nanotubes were treated in a fluidized air-bed with an ultrasound probe before being used in the fabrication of the NCs with no ultrasound assistance during extrusion. The samples were characterized by MFI, Optical microscopy (OM), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), electrical surface resistivity, and electric charge. MFI decreases in all cases with addition of MWCNTs with the largest decrease observed for samples with the highest MFI. The surface resistivity, which ranged from 1013 to 105 Ω/sq, and electric charge, were observed to depend on the ultrasound-assisted fabrication method as well as on the melt flow index of the iPP. A relationship between agglomerate size and area ratio with electric charge was found. Several trends in the overall data were identified and are discussed in terms of MFI and the different fabrication methods. PMID:28793686

  20. Comparison of ultrasound-assisted and traditional caustic leaching of spent cathode carbon (SCC) from aluminum electrolysis.

    Science.gov (United States)

    Xiao, Jin; Yuan, Jie; Tian, Zhongliang; Yang, Kai; Yao, Zhen; Yu, Bailie; Zhang, Liuyun

    2018-01-01

    The spent cathode carbon (SCC) from aluminum electrolysis was subjected to caustic leaching to investigate the different effects of ultrasound-assisted and traditional methods on element fluorine (F) leaching rate and leaching residue carbon content. Sodium hydroxide (NaOH) dissolved in deionized water was used as the reaction system. Through single-factor experiments and a comparison of two leaching techniques, the optimum F leaching rate and residue carbon content for ultrasound-assisted leaching process were obtained at a temperature of 70°C, residue time of 40min, initial mass ratio of alkali to SCC (initial alkali-to-material ratio) of 0.6, liquid-to-solid ratio of 10mL/g, and ultrasonic power of 400W, respectively. Under the optimal conditions, the leaching residue carbon content was 94.72%, 2.19% larger than the carbon content of traditional leaching residue. Leaching wastewater was treated with calcium chloride (CaCl 2 ) and bleaching powder and the treated wastewater was recycled caustic solution. All in all, benefiting from advantage of the ultrasonication effects, ultrasound-assisted caustic leaching on spent cathode carbon had 55.6% shorter residue time than the traditional process with a higher impurity removal rate. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Ultrasound-assisted extraction (UAE) and solvent extraction of papaya seed oil: yield, fatty acid composition and triacylglycerol profile.

    Science.gov (United States)

    Samaram, Shadi; Mirhosseini, Hamed; Tan, Chin Ping; Ghazali, Hasanah Mohd

    2013-10-10

    The main objective of the current work was to evaluate the suitability of ultrasound-assisted extraction (UAE) for the recovery of oil from papaya seed as compared to conventional extraction techniques (i.e., Soxhlet extraction (SXE) and solvent extraction (SE)). In the present study, the recovery yield, fatty acid composition and triacylglycerol profile of papaya seed oil obtained from different extraction methods and conditions were compared. Results indicated that both solvent extraction (SE, 12 h/25 °C) and ultrasound-assisted extraction (UAE) methods recovered relatively high yields (79.1% and 76.1% of total oil content, respectively). Analysis of fatty acid composition revealed that the predominant fatty acids in papaya seed oil were oleic (18:1, 70.5%-74.7%), palmitic (16:0, 14.9%-17.9%), stearic (18:0, 4.50%-5.25%), and linoleic acid (18:2, 3.63%-4.6%). Moreover, the most abundant triacylglycerols of papaya seed oil were triolein (OOO), palmitoyl diolein (POO) and stearoyl oleoyl linolein (SOL). In this study, ultrasound-assisted extraction (UAE) significantly (p oil, but no significant differences were observed in the fatty acid composition of papaya seed oil extracted by different extraction methods (SXE, SE and UAE) and conditions.

  2. Ultrasound-Assisted Extraction (UAE and Solvent Extraction of Papaya Seed Oil: Yield, Fatty Acid Composition and Triacylglycerol Profile

    Directory of Open Access Journals (Sweden)

    Hasanah Mohd Ghazali

    2013-10-01

    Full Text Available The main objective of the current work was to evaluate the suitability of ultrasound-assisted extraction (UAE for the recovery of oil from papaya seed as compared to conventional extraction techniques (i.e., Soxhlet extraction (SXE and solvent extraction (SE. In the present study, the recovery yield, fatty acid composition and triacylglycerol profile of papaya seed oil obtained from different extraction methods and conditions were compared. Results indicated that both solvent extraction (SE, 12 h/25 °C and ultrasound-assisted extraction (UAE methods recovered relatively high yields (79.1% and 76.1% of total oil content, respectively. Analysis of fatty acid composition revealed that the predominant fatty acids in papaya seed oil were oleic (18:1, 70.5%–74.7%, palmitic (16:0, 14.9%–17.9%, stearic (18:0, 4.50%–5.25%, and linoleic acid (18:2, 3.63%–4.6%. Moreover, the most abundant triacylglycerols of papaya seed oil were triolein (OOO, palmitoyl diolein (POO and stearoyl oleoyl linolein (SOL. In this study, ultrasound-assisted extraction (UAE significantly (p < 0.05 influenced the triacylglycerol profile of papaya seed oil, but no significant differences were observed in the fatty acid composition of papaya seed oil extracted by different extraction methods (SXE, SE and UAE and conditions.

  3. Enzymolysis kinetics and activities of ACE inhibitory peptides from wheat germ protein prepared with SFP ultrasound-assisted processing.

    Science.gov (United States)

    Qu, Wenjuan; Ma, Haile; Jia, Junqiang; He, Ronghai; Luo, Lin; Pan, Zhongli

    2012-09-01

    There is a great demand for developing efficient enzymolysis methods in order to increase the enzymolysis efficiencies and activities of angiotensin converting enzyme (ACE) inhibitory peptides from wheat germ protein. The enzymolysis kinetics, ACE inhibitory activity of peptide and conversion rate of protein were studied using sweep frequency and pulsed (SFP) ultrasound-assisted enzymolysis and the results were compared with traditional enzymolysis. The studied factors were enzymolysis time and substrate concentration. By considering the activity of ACE inhibitory peptide and operation cost, the recommended conditions of SFP ultrasound-assisted enzymolysis were enzymolysis time of 120 min and substrate concentration of 24.0 g/L, which gave high conversion rates of protein (60.7%) and ACE inhibitory activity of peptide (65.9%). Compared to traditional enzymolysis, SFP ultrasound-assisted enzymolysis significantly increased the initial reaction rate (V) by 60.0% at substrate concentration of 24.0 g/L, increased the apparent breakdown rate constant (k(A)) by 66.7%, decreased the apparent constant (K(M)) by 6.9%, and raised the conversion rate of protein by 35.5% and ACE inhibitory activity of peptides by 35.6% under the recommended conditions. It has been concluded that SFP ultrasound can remarkably raise the enzymolysis efficiency and activity of ACE inhibitory peptides from wheat germ protein. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. Ultrasound-Assisted Extraction and Identification of Natural Antioxidants from the Fruit of Melastoma sanguineum Sims.

    Science.gov (United States)

    Zhou, Tong; Xu, Dong-Ping; Lin, Sheng-Jun; Li, Ya; Zheng, Jie; Zhou, Yue; Zhang, Jiao-Jiao; Li, Hua-Bin

    2017-02-18

    The fruit of Melastoma sanguineum Sims is an edible and sweet wild fruit. In our previous study, the fruit was found to have a strong antioxidant property. In this study, an ultrasound-assisted extraction (UAE) method was developed to extract natural antioxidants from the fruit of Melastoma sanguineum Sims, and a response surface methodology was used to optimize the conditions of UAE to maximize the extraction efficiency. The influence of five independent extraction parameters (ethanol concentration, solvent/material ratio, extracting time, temperature, and ultrasound power) on the extraction efficiency were investigated using a single factor experiment, and then a central composite rotatable design was used to investigate the interaction of three key parameters. The results showed that the optimal extraction conditions were 42.98% ethanol, 28.29 mL/g solvent/material ratio, 34.29 min extracting time, 60 °C temperature, and 600 W ultrasound power. Under these conditions, the Trolox equivalent antioxidant capacity (TEAC) value of the extracts was 1074.61 ± 32.56 μmol Trolox/g dry weight (DW). Compared with conventional maceration (723.27 ± 11.61 μmol Trolox/g DW) and Soxhlet extraction methods (518.37 ± 23.23 μmol Trolox/g DW), the UAE method improved the extraction efficiency, in a shorter period of time. In addition, epicatechin gallate, epicatechin, rutin, epigallocatechin, protocatechuic acid, chlorogenic acid, and quercetin, were identified and quantified in the fruit extracts of Melastoma sanguineum Sims by UPLC-MS/MS.

  5. Ultrasound-assisted extraction and purification of taurine from the red algae Porphyra yezoensis.

    Science.gov (United States)

    Wang, Fen; Guo, Xiao-Yu; Zhang, Dan-Ni; Wu, Yue; Wu, Tao; Chen, Zhi-Gang

    2015-05-01

    The present study reports on the development of a method using ultrasound-assisted extraction (UAE) during the purification of taurine from Porphyra yezoensis. The Box-Behnken design, which is a widely used form of response surface methodology, was used to investigate the effects of parameters on the UAE process. Three independent variables of taurine purification using UAE were studied including: extraction time, temperature, and ultrasonic power. The results showed that the highest taurine yield of 13.0mg/g was obtained with an extraction time of 38.3 min, the use of 300.0 W ultrasonic power, and an extraction temperature of 40.5°C. A comparative study of taurine extraction was also conducted using either ultrasonication or mechanical agitation. The results indicated that the ultrasonic process required 9 times less time at 40°C to obtain taurine with a similar yield as compared to the conventional extraction method. Therefore, UAE can used as an alternative to the conventional extraction method used during the recovery of taurine from P. yezoensis. The UAE method has several advantages, including that it uses lower extraction temperatures and has a shorter extraction time. The taurine present in the extract supernatant was efficiently separated and purified using a combination of 732 cation exchange chromatography and crystallization. The yield of purified taurine using this process was 1.1%. The structure of the purified taurine was confirmed by FTIR, MS, and NMR. Our findings suggest that P. yezoensis can be used as a taurine-rich food or food material. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Reduction of the Areolar Diameter After Ultrasound-Assisted Liposuction for Gynecomastia.

    Science.gov (United States)

    Keskin, Mustafa; Sutcu, Mustafa; Hanci, Mustafa; Cigsar, Bulent

    2017-08-01

    One of the clinical aspects characterizing gynecomastia is the enlargement of the nipple-areolar complex (NAC) due to hypertrophic breast glands, and the excessive fatty tissue underneath. The purpose of this study was to quantify the reduction of the areolar diameter after ultrasound-assisted liposuction (UAL) of the male breast. The horizontal diameters of the NACs of 30 men who underwent UAL were measured before surgery, 1 month after surgery and 6 months after surgery in a standard fashion. Those patients with surgical gland removals of any kind were not included in this study. The mean age of the patients was 27.9 years, and all of the patients had bilateral grade I, II, or III gynecomastia. The mean diameter of the NACs before surgery was 35.36 mm (range, 26-55 mm), and after surgery, the mean diameter of the NACs was initially reduced to 28.8 mm (range, 23-44 mm) and later to 28.57 mm (range, 23-42 mm). The mean volume of breast tissue aspirated was 382 mL per breast, and the percentage of reduction was 17.3%. The reduction of areola diameter was statistically significant after first month. A significant positive correlation was identified between the liposuction volume and areolar diameter reduction. In cases of gynecomastia, the removal of the glandular and fatty tissue underneath the areola releases the expanding forces and pressure that enlarge it. In many cases of gynecomastia, UAL alone is effective in reducing the size of the NAC and allows the surgeon to avoid placing scars on the breast.

  7. Ultrasound-assisted acid hydrolysis of cellulose to chemical building blocks: Application to furfural synthesis.

    Science.gov (United States)

    Santos, Daniel; Silva, Ubiratan F; Duarte, Fabio A; Bizzi, Cezar A; Flores, Erico M M; Mello, Paola A

    2018-01-01

    In this work, the use of ultrasound energy for the production of furanic platforms from cellulose was investigated and the synthesis of furfural was demonstrated. Several systems were evaluated, as ultrasound bath, cup horn and probe, in order to investigate microcrystalline cellulose conversion using simply a diluted acid solution and ultrasound. Several acid mixtures were evaluated for hydrolysis, as diluted solutions of HNO 3 , H 2 SO 4 , HCl and H 2 C 2 O 4 . The influence of the following parameters in the ultrasound-assisted acid hydrolysis (UAAH) were studied: sonication temperature (30 to 70°C) and ultrasound amplitude (30 to 70% for a cup horn system) for 4 to 8molL -1 HNO 3 solutions. For each evaluated condition, the products were identified by ultra-performance liquid chromatography with high-resolution time-of-flight mass spectrometry (UPLC-ToF-MS), which provide accurate information regarding the products obtained from biomass conversion. The furfural structure was confirmed by nuclear magnetic resonance ( 1 H and 13 C NMR) spectroscopy. In addition, cellulosic residues from hydrolysis reaction were characterized using scanning electron microscopy (SEM), which contributed for a better understanding of physical-chemical effects caused by ultrasound. After process optimization, a 4molL -1 HNO 3 solution, sonicated for 60min at 30°C in a cup horn system at 50% of amplitude, lead to 78% of conversion to furfural. This mild temperature condition combined to the use of a diluted acid solution represents an important contribution for the selective production of chemical building blocks using ultrasound energy. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Ultrasound-assisted extraction of rare-earth elements from carbonatite rocks.

    Science.gov (United States)

    Diehl, Lisarb O; Gatiboni, Thais L; Mello, Paola A; Muller, Edson I; Duarte, Fabio A; Flores, Erico M M

    2018-01-01

    In view of the increasing demand for rare-earth elements (REE) in many areas of high technology, alternative methods for the extraction of these elements have been developed. In this work, a process based on the use of ultrasound for the extraction of REE from carbonatite (an igneous rock) is proposed to avoid the use of concentrated reagents, high temperature and excessive extraction time. In this pioneer work for REE extraction from carbonatite rocks in a preliminary investigation, ultrasonic baths, cup horn systems or ultrasound probes operating at different frequencies and power were evaluated. In addition, the power released to the extraction medium and the ultrasound amplitude were also investigated and the temperature and carbonatite mass/volume of extraction solution ratio were optimized to 70°C and 20mg/mL, respectively. Better extraction efficiencies (82%) were obtained employing an ultrasound probe operating at 20kHz for 15min, ultrasound amplitude of 40% (692Wdm -3 ) and using a diluted extraction solution (3% v/v HNO 3 +2% v/v HCl). It is important to mention that high extraction efficiency was obtained even using a diluted acid mixture and relatively low temperature in comparison to conventional extraction methods for REE. A comparison of results with those obtained by mechanical stirring (500rpm) using the same conditions (time, temperature and extraction solution) was carried out, showing that the use of ultrasound increased the extraction efficiency up to 35%. Therefore, the proposed ultrasound-assisted procedure can be considered as a suitable alternative for high efficiency extraction of REE from carbonatite rocks. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Ultrasound-Assisted Extraction and Identification of Natural Antioxidants from the Fruit of Melastoma sanguineum Sims

    Directory of Open Access Journals (Sweden)

    Tong Zhou

    2017-02-01

    Full Text Available The fruit of Melastoma sanguineum Sims is an edible and sweet wild fruit. In our previous study, the fruit was found to have a strong antioxidant property. In this study, an ultrasound-assisted extraction (UAE method was developed to extract natural antioxidants from the fruit of Melastoma sanguineum Sims, and a response surface methodology was used to optimize the conditions of UAE to maximize the extraction efficiency. The influence of five independent extraction parameters (ethanol concentration, solvent/material ratio, extracting time, temperature, and ultrasound power on the extraction efficiency were investigated using a single factor experiment, and then a central composite rotatable design was used to investigate the interaction of three key parameters. The results showed that the optimal extraction conditions were 42.98% ethanol, 28.29 mL/g solvent/material ratio, 34.29 min extracting time, 60 °C temperature, and 600 W ultrasound power. Under these conditions, the Trolox equivalent antioxidant capacity (TEAC value of the extracts was 1074.61 ± 32.56 μmol Trolox/g dry weight (DW. Compared with conventional maceration (723.27 ± 11.61 μmol Trolox/g DW and Soxhlet extraction methods (518.37 ± 23.23 μmol Trolox/g DW, the UAE method improved the extraction efficiency, in a shorter period of time. In addition, epicatechin gallate, epicatechin, rutin, epigallocatechin, protocatechuic acid, chlorogenic acid, and quercetin, were identified and quantified in the fruit extracts of Melastoma sanguineum Sims by UPLC-MS/MS.

  10. Synthesis of amine-modified zeolitic imidazolate framework-8, ultrasound-assisted dye removal and modeling.

    Science.gov (United States)

    Abdi, Jafar; Vossoughi, Manouchehr; Mahmoodi, Niyaz Mohammad; Alemzadeh, Iran

    2017-11-01

    The present research is focused on the ultrasound assisted adsorption of Acid blue 92 (AB92) and Direct red 80 (DR80) as anionic dyes in single and binary systems onto zeolitic imidazolate framework (ZIF-8) functionalized with 3-Aminopropyltrimethoxysilane (APTES). Different techniques such as Fourier transform infrared (FTIR), scanning electron microscope (SEM), field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) and thermogravimetric analyses (TGA) were used to characterize the prepared adsorbent. The individual effects and possible interactions between the various parameters including adsorbent dosage, sonication time, initial dye concentrations and pH on dyes removal efficiency were investigated by response surface methodology (RSM). The optimized experimental conditions were fixed at adsorbent dosage 0.005g for AB92 and 0.01g for DR80, pH 2.1, sonication time 15min, and initial dyes concentration 15mgL -1 to get maximum removal percentage (>95.0%). A reliable and intelligent model based on least-squares support vector machine (LS-SVM) was developed to predict dye removal efficiency. The root mean square error (RMSE) of 0.604, 0.734 and 1.549 with high determination coefficient (R 2 ) of 0.999, 0.996 and 0.997 for AB92, DR80 and binary system, respectively, were able to predict and model the adsorption process. The presented model illustrates better performance in predicting dye removal efficiency compared to the kinetic models. The results showed that the adsorption process had better conformation with pseudo-second order model. The adsorption equilibrium data was investigated by Langmuir, Freundlich, Tempkin and Dubinin-Radushkevich isotherm models and the data were well fitted by Langmuir model with maximum adsorption capacity of 633.4 and 500.2mgg -1 for AB92 and DR80 dyes, respectively. APTES@ZIF-8 was regenerated and found to be reusable after four successive cycles without considerable loss in

  11. Optimization of Ultrasound-Assisted Extraction, Preliminary Characterization and In Vitro Antioxidant Activity of Polysaccharides from Green Pea Pods

    OpenAIRE

    Jalili Safaryan, Maryam; Ganjloo, Ali; Bimakr, Mandana; Zarringhalami, Soheila

    2016-01-01

    In this study, ultrasound-assisted extraction of green pea pod polysaccharide (GPPP) was investigated and optimized using a central composite response surface design coupled with a numerical optimization technique. The effects of ultrasonic power (50–150 W), sonication time (20–80 min), ratio of water to raw material (20:1–40:1 mL/g) and extraction temperature (40–80 °C) on polysaccharide extraction yield were studied. The maximum extraction yield was obtained with a sonication power of 135.3...

  12. Kinetics of Ultrasound-Assisted Flavonoid Extraction from Agri-Food Solid Wastes Using Water/Glycerol Mixtures

    Directory of Open Access Journals (Sweden)

    Dimitris P. Makris

    2016-01-01

    Full Text Available Red grape pomace (RGP and onion solid wastes (OSW were used as raw material to produce flavonoid-enriched extracts, using ultrasound-assisted solid-liquid extraction. The extraction medium used was composed of water and glycerol and under the conditions used the extraction of flavonoids from both materials was shown to obey first-order kinetics. Maximum diffusivities (De values were 4.01 × 10−11 and 2.35 × 10−11 m2·s−1, for RGP and OSW extraction, respectively, while the corresponding activation energies (Ea were 14.00 and 15.23 kJ·mol−1.

  13. Optimization of Ultrasound-Assisted Extraction of Natural Antioxidants from the Flower of Jatropha integerrima by Response Surface Methodology.

    Science.gov (United States)

    Xu, Dong-Ping; Zhou, Yue; Zheng, Jie; Li, Sha; Li, An-Na; Li, Hua-Bin

    2015-12-24

    An ultrasound-assisted extraction (UAE) method was developed for the efficient extraction of natural antioxidants from the flowers of Jatropha integerrima. Four independent variables, including ethanol concentration, solvent/material ratio, ultrasound irradiation time and temperature were studied by single factor experiments. Then, the central composite rotatable design and response surface methodology were employed to investigate the effect of three key parameters (ethanol concentration, solvent/material ratio, and ultrasound irradiation time) on the antioxidant activities of the flower extracts. The optimal extraction conditions were an ethanol concentration of 59.6%, solvent/material ratio of 50:1, ultrasound irradiation time of 7 min, and ultrasound irradiation temperature of 40 °C. Under these conditions, the optimized experimental value was 1103.38 ± 16.11 µmol Trolox/g dry weight (DW), which was in accordance with the predicted value (1105.49 µmol Trolox/g DW). Furthermore, the antioxidant activities of flower extracts obtained by UAE were compared with those produced by the traditional maceration and Soxhlet extraction methods, and UAE resulted in higher antioxidant activities after a shorter time at a lower temperature. The results obtained are helpful for the full utilization of Jatropha integerrima, and also indicate that ultrasound-assisted extraction is an efficient method for the extraction of natural antioxidants from plant materials.

  14. Optimization of Ultrasound-Assisted Extraction of Natural Antioxidants from the Flower of Jatropha integerrima by Response Surface Methodology

    Directory of Open Access Journals (Sweden)

    Dong-Ping Xu

    2015-12-01

    Full Text Available An ultrasound-assisted extraction (UAE method was developed for the efficient extraction of natural antioxidants from the flowers of Jatropha integerrima. Four independent variables, including ethanol concentration, solvent/material ratio, ultrasound irradiation time and temperature were studied by single factor experiments. Then, the central composite rotatable design and response surface methodology were employed to investigate the effect of three key parameters (ethanol concentration, solvent/material ratio, and ultrasound irradiation time on the antioxidant activities of the flower extracts. The optimal extraction conditions were an ethanol concentration of 59.6%, solvent/material ratio of 50:1, ultrasound irradiation time of 7 min, and ultrasound irradiation temperature of 40 °C. Under these conditions, the optimized experimental value was 1103.38 ± 16.11 µmol Trolox/g dry weight (DW, which was in accordance with the predicted value (1105.49 µmol Trolox/g DW. Furthermore, the antioxidant activities of flower extracts obtained by UAE were compared with those produced by the traditional maceration and Soxhlet extraction methods, and UAE resulted in higher antioxidant activities after a shorter time at a lower temperature. The results obtained are helpful for the full utilization of Jatropha integerrima, and also indicate that ultrasound-assisted extraction is an efficient method for the extraction of natural antioxidants from plant materials.

  15. Ultrasound-assisted extraction of natural antioxidants from the flower of Limonium sinuatum: Optimization and comparison with conventional methods.

    Science.gov (United States)

    Xu, Dong-Ping; Zheng, Jie; Zhou, Yue; Li, Ya; Li, Sha; Li, Hua-Bin

    2017-02-15

    Natural antioxidants are widely used as dietary supplements or food additives. An optimized method of ultrasound-assisted extraction (UAE) was proposed for the effective extraction of antioxidants from the flowers of Limonium sinuatum and evaluated by response surface methodology. In this study, ethanol concentration, ratio of solvent to solid, ultrasonication time and temperature were investigated and optimized using a central composite rotatable design. The optimum extraction conditions were as follows: ethanol concentration, 60%; ratio of solvent to solid, 56.9:1mL/g; ultrasonication time, 9.8min; and temperature, 40°C. Under the optimal UAE conditions, the experimental values (483.01±15.39μmolTrolox/gDW) matched with those predicted (494.13μmolTrolox/gDW) within a 95% confidence level. In addition, the antioxidant activities of UAE were compared with those of conventional maceration and Soxhlet extraction methods, and the ultrasound-assisted extraction could give higher yield of antioxidants and markedly reduce the extraction time. Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. Ecofriendly laccase-hydrogen peroxide/ultrasound-assisted bleaching of linen fabrics and its influence on dyeing efficiency.

    Science.gov (United States)

    Abou-Okeil, A; El-Shafie, A; El Zawahry, M M

    2010-02-01

    This study evaluates the bleaching efficiency of enzymatically scoured linen fabrics using a combined laccase-hydrogen peroxide bleaching process with and without ultrasonic energy, with the goal of obtaining fabrics with high whiteness levels, well preserved tensile strength and higher dye uptake. The effect of the laccase enzyme and the combined laccase-hydrogen peroxide bleaching process with and without ultrasound has been investigated with regard to whiteness value, tensile strength, dyeing efficiency and dyeing kinetics using both reactive and cationic dyes. The bleached linen fabrics were characterized using X-ray diffraction and by measuring tensile strength and lightness. The dyeing efficiency and kinetics were characterized by measuring dye uptake and colour fastness. The results indicated that ultrasound was an effective technique in the combined laccase-hydrogen peroxide bleaching process of linen fabrics. The whiteness values expressed as lightness of linen fabrics is enhanced by using ultrasonic energy. The measured colour strength values were found to be slightly better for combined laccase-hydrogen peroxide/ultrasound-assisted bleached fabrics than for combined laccase-hydrogen peroxide for both reactive and cationic dyes. The fastness properties of the fabrics dyed with reactive dye were better than those obtained when using cationic dye. The time/dye uptake isotherms were also enhanced when using combined laccase-hydrogen peroxide/ultrasound-assisted bleached fabric, which confirms the efficiency of ultrasound in the combined oxidative bleaching process. The dyeing rate constant, half-time of dyeing and dyeing efficiency have been calculated and discussed.

  17. Nano-coating of beta-galactosidase onto the surface of lactose by using an ultrasound-assisted technique

    DEFF Research Database (Denmark)

    Genina, Natalja; Räikkönen, Heikki; Heinämäki, Jyrki

    2010-01-01

    We nano-coated powdered lactose particles with the enzyme beta-galactosidase using an ultrasound-assisted technique. Atomization of the enzyme solution did not change its activity. The amount of surface-attached beta-galactosidase was measured through its enzymatic reaction product D-galactose us......We nano-coated powdered lactose particles with the enzyme beta-galactosidase using an ultrasound-assisted technique. Atomization of the enzyme solution did not change its activity. The amount of surface-attached beta-galactosidase was measured through its enzymatic reaction product D......-galactose using a standardized method. A near-linear increase was obtained in the thickness of the enzyme coat as the treatment proceeded. Interestingly, lactose, which is a substrate for beta-galactosidase, did not undergo enzymatic degradation during processing and remained unchanged for at least 1 month....... Stability of protein-coated lactose was due to the absence of water within the powder, as it was dry after the treatment procedure. In conclusion, we were able to attach the polypeptide to the core particles and determine precisely the coating efficiency of the surface-treated powder using a simple approach....

  18. Optimization and Comparison of Ultrasound-Assisted Extraction of Estragole from Tarragon Leaves with Hydro-Distillation Method

    Directory of Open Access Journals (Sweden)

    Mohammad Bagher Gholivand

    2014-12-01

    Full Text Available A comparative study of ultrasound-assisted extraction (UAE and hydro-distillation was performed for fast extraction of estragole from tarragon (Artemisia dracunculus L. dried leaves. Several influential parameters of the UAE procedure in the extraction of estragole (type of solvent, extraction cycles, solvent to material ratio, irradiation time and particle size were investigated and optimized. It was found that UAE offers a more rapid extraction of estragole than hydrodistillation. The optimum parameters were solvent to material ratio of 8:1 v/m, 96% (w/w ethanol in water as extraction solvent, particle size of 1.18 mm, irradiation time of 5 min, output power of 63 W, 9 pulses, and ultrasonic frequency of 20 kHz. The recovery of estragole by UAE under optimal conditions was 44.4% based on dry extract. The benefit of ultrasound was to decrease the extraction time (5 min relative to the classical hydrodistillation method (3 h. The experimental results also indicated that ultrasound-assisted extraction is a simple, rapid and effective method for extraction of the volatile oil components of tarragon.

  19. Green ultrasound-assisted extraction of anthocyanin and phenolic compounds from purple sweet potato using response surface methodology

    Science.gov (United States)

    Zhu, Zhenzhou; Guan, Qingyan; Guo, Ying; He, Jingren; Liu, Gang; Li, Shuyi; Barba, Francisco J.; Jaffrin, Michel Y.

    2016-01-01

    Response surface methodology was used to optimize experimental conditions for ultrasound-assisted extraction of valuable components (anthocyanins and phenolics) from purple sweet potatoes using water as a solvent. The Box-Behnken design was used for optimizing extraction responses of anthocyanin extraction yield, phenolic extraction yield, and specific energy consumption. Conditions to obtain maximal anthocyanin extraction yield, maximal phenolic extraction yield, and minimal specific energy consumption were different; an overall desirability function was used to search for overall optimal conditions: extraction temperature of 68ºC, ultrasonic treatment time of 52 min, and a liquid/solid ratio of 20. The optimized anthocyanin extraction yield, phenolic extraction yield, and specific energy consumption were 4.91 mg 100 g-1 fresh weight, 3.24 mg g-1 fresh weight, and 2.07 kWh g-1, respectively, with a desirability of 0.99. This study indicates that ultrasound-assisted extraction should contribute to a green process for valorization of purple sweet potatoes.

  20. Sequential Combination of Microwave- and Ultrasound-Assisted Extraction of Total Flavonoids from Osmanthus fragrans Lour. Flowers

    Directory of Open Access Journals (Sweden)

    Jianfeng Yu

    2017-12-01

    Full Text Available Microwave-assisted and ultrasound-assisted extraction assays were used to isolate total flavonoids (TF from Osmanthus fragrans flowers. The effects of the solid-liquid ratio, ethanol concentration, microwave power, microwave extraction time, ultrasonic power and ultrasonic extraction time on the yield of TF were studied. A sequential combination of microwave- and ultrasound-assisted extraction (SC-MUAE methods was developed, which was subsequently optimized by Box-Behnken design-response surface methodology (BBD-RSM. The interaction effects of the ethanol concentration (40–60%, microwave extraction time (5–7 min, ultrasonic extraction time (8–12 min and ultrasonic power (210–430 W on the yield of TF were investigated. The optimum operating parameters for the extraction of TF were determined to be as follows: ethanol concentration (48.15%, microwave extraction time (6.43 min, ultrasonic extraction time (10.09 min and ultrasonic power (370.9 W. Under these conditions, the extraction yield of TF was 7.86 mg/g.

  1. Optimization of deep eutectic solvent-based ultrasound-assisted extraction of polysaccharides from Dioscorea opposita Thunb.

    Science.gov (United States)

    Zhang, Lijin; Wang, Maoshan

    2017-02-01

    In this study, deep eutectic solvents were proposed for the ultrasound-assisted extraction of polysaccharides from Dioscorea opposita Thunb. Several deep eutectic solvents were prepared for the extraction of polysaccharides, among which the deep eutectic solvent composed of choline chloride and 1,4-butanediol was proved to be suitable for the extraction. Based on the screening of single-factor experiment design and orthogonal experiment design, three experimental factors were optimized for the Box-Behnken experimental design combined with response surface methodology, which gave the optimal extraction conditions: water content of 32.89%(v/v), extraction temperature of 94.00°C, and the extraction time of 44.74min. The optimal extraction conditions could supply higher extraction yield than those of hot water extraction and water-based ultrasound-assisted extraction. Therefore, deep eutectic solvents were an excellent extraction solvent alternative to the extraction of polysaccharides from sample matrices. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. RSM and ANN modeling-based optimization approach for the development of ultrasound-assisted liposome encapsulation of piceid.

    Science.gov (United States)

    Huang, Shang-Ming; Kuo, Chia-Hung; Chen, Chun-An; Liu, Yung-Chuan; Shieh, Chwen-Jen

    2017-05-01

    Piceid, a naturally occurring derivative of resveratrol found in many plants, has recently been considered as a potential nutraceutical. However, its poorly water-soluble property could cause a coupled problem of biological activities concerning drug dispersion and absorption in human body, which is still unsolved now. Liposome, a well-known aqueous carrier for water-insoluble ingredients, is commonly applied in drug delivery systems. In this study, a feasible approach for solving the problem is that the targeted piceid was encapsulated into a liposomal formula as aqueous substrate to overcome its poor water-solubility. The encapsulation process was assisted by ultrasound, with investigation of lipid content, ultrasound power and ultrasound time, for controlling encapsulation efficiency (E.E%), absolute loading (A.L%) and particle size (PS). Moreover, both RSM and ANN methodologies were further applied to optimize the ultrasound-assisted encapsulation process. The data indicated that the most important effects on the encapsulation performance were found to be of lipid content followed by ultrasound time and ultrasound power. The maximum E.E% (75.82%) and A.L% (2.37%) were exhibited by ultrasound assistance with the parameters of 160mg lipid content, ultrasound time for 24min and ultrasound power of 90W. By methodological aspects of processing, the predicted E.E% and A.L% were respectively in good agreement with the experimental results for both RSM and ANN. Moreover, RMSE, R 2 and AAD statistics were further used to compare the prediction abilities of RSM and ANN based on the validation data set. The results indicated that the prediction accuracy of ANN was better than that of RSM. In conclusion, ultrasound-assisted liposome encapsulation can be an efficient strategy for producing well-soluble/dispersed piceid, which could be further applied to promote human health by increased efficiency of biological absorption, and the process of ultrasound-mediated liposome

  3. Simultaneous derivatization and ultrasound-assisted dispersive liquid-liquid microextraction of chloropropanols in soy milk and other aqueous matrices combined with gas-chromatography-mass spectrometry.

    Science.gov (United States)

    Carro, A M; González, P; Lorenzo, R A

    2013-12-06

    A novel approach involving ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and derivatization combined with gas chromatography-mass spectrometry was developed for the determination of chloropropanols in water and beverages. UA-DLLME was optimized as less solvent-consuming and cost-effective extraction method for water, fruit juice, milk and soy milk samples. The effect of parameters such as the type and volume of extraction solvent, the type and volume of dispersive solvent, amount of derivatization agent, temperature, pH of sample and ionic strength was investigated and optimized for each specimen, using experimental designs. By adding acetonitrile as dispersive solvent, N-heptafluorobutyrylimizadole (HFBI) as derivatization agent and chloroform as extraction solvent, the extraction-derivatization and preconcentration were simultaneously performed. The analytical concentration range was investigated in detail for each analyte in the different samples, obtaining linearity with R(2) ranging between 0.9990 and 0.9999. The method detection limits were in the range of 0.2-1.8μgL(-1) (water), 0.5-15μgL(-1) (fruit juices) and 0.9-3.6μgkg(-1) (milk) and 0.1-1.0μgkg(-1) (soy milk). The method was applied to the analysis of a variety of specimens, with recoveries of 98-101% from water, 97-102% from juices, 99-103% from milk and 97-105% from soy beverage. The relative standard deviation (precision, n=6) varied between 1.3 and 4.9%RSD in water, 2.3 and 5.8%RSD in juices, 1.0 and 5.7%RSD in milk and 3.9 and 9.3%RSD in soy milk. The proposed method was applied to analysis of twenty-eight samples. 1,3-Dichloro-2-propanol was found in an influent water sample from urban wastewater treatment plant (WWTP) (2.1±0.04mgL(-1)) but no chloropropanols were found in the corresponding effluent water sample. This result suggests that the purification system used in the WWTP has been effective for this compound. Moreover, the results revealed the presence of 3

  4. Optimization of ultrasound-assisted dispersive solid-phase microextraction based on nanoparticles followed by spectrophotometry for the simultaneous determination of dyes using experimental design.

    Science.gov (United States)

    Asfaram, Arash; Ghaedi, Mehrorang; Goudarzi, Alireza

    2016-09-01

    A simple, low cost and ultrasensitive method for the simultaneous preconcentration and determination of trace amount of auramine-O and malachite green in aqueous media following accumulation on novel and lower toxicity nanomaterials by ultrasound-assisted dispersive solid phase micro-extraction (UA-DSPME) procedure combined with spectrophotometric has been described. The Mn doped ZnS nanoparticles loaded on activated carbon were characterized by Field emission scanning electron microscopy (FE-SEM), particle size distribution, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) analyses and subsequently were used as green and efficient material for dyes accumulation. Contribution of experimental variables such as ultrasonic time, ultrasonic temperature, adsorbent mass, vortex time, ionic strength, pH and elution volume were optimized through experimental design, and while the preconcentrated analytes were efficiently eluted by acetone. Preliminary Plackett-Burman design was applied for selection of most significant factors and giving useful information about their main and interaction part of significant variables like ultrasonic time, adsorbent mass, elution volume and pH were obtained by central composite design combined with response surface analysis and optimum experimental conditions was set at pH of 8.0, 1.2mg of adsorbent, 150μL eluent and 3.7min sonication. Under optimized conditions, the average recoveries (five replicates) for two dyes (spiked at 500.0ngmL(-1)) changes in the range of 92.80-97.70% with acceptable RSD% less than 4.0% over a linear range of 3.0-5000.0ngmL(-1) for the AO and MG in water samples with regression coefficients (R(2)) of 0.9975 and 0.9977, respectively. Acceptable limits of detection of 0.91 and 0.61ngmL(-1) for AO and MG, respectively and high accuracy and repeatability are unique advantages of present method to improve the figures of merit for their accurate determination at trace level in complicated

  5. Plastic deformation and wave formation on the interface of metals welded by ultrasound-assisted explosive welding

    Science.gov (United States)

    Kuz’min, E. V.; Kuz’min, S. V.; Lysak, V. I.; Lata, A. N.

    2017-10-01

    This paper presents the influence of the effect of ultrasound on the wave formation and plastic deformation in the metals welded by ultrasound-assisted explosive welding. It has been established that the influence of high-frequency acoustic waves on the metal leads to a reduction of the dynamic yield stress, which in turn leads to changes in the properties of the surface layers of metal and in the conditions of bonding between the collided plates upon explosive welding. It has been shown that the changes in the length and amplitude of waves that arise in the weld joint upon the explosive welding with the simultaneous action of ultrasonic vibrations is connected with a decrease in the magnitude of the deforming pulse and time of action of the compressive stresses that exceed the dynamic yield stress behind the point of contact.

  6. Optimization of ultrasound-assisted extraction of flavonoids compounds from Chenopodium hybridum L. stem with response surface methodology

    Science.gov (United States)

    Wu, Y.; Hu, H. B.; Wang, C. L.; Ma, S. R.; Zhang, L. L.

    2016-08-01

    Ultrasound-assisted extraction (UAE) of flavonoids compounds (FC) from the stem of Chenopodium hybridum L.(C.hybridum L.) was investigated in this paper. Significant technological parameters were screened and optimized by using Plackett-Burman (PB) design, Steepest ascent method and Box-Behnken (BB) design, respectively. A mathematical model with high correlation coefficient (R2=0.9896) was developed and showed good consistency between the experimental and predicted values. The optimum conditions for UAE were obtained by res- ponse surface methodology (RSM) as follows: volumn fraction of ethanol 76.62 %, extractive temperature 78.69°C, and liquid to solid ratio 58.43 for 30 min. Under these conditions, total flavo- noid content (TFC) of 9.4701 mg RE/100g were gained and it was closely related with predi- cted value (9.4640 mg RE/100g) and indicated the suitability of the developed model.

  7. Ultrasound assisted arthroscopic approach for removal of basilar sesamoid fragments of the proximal sesamoid bones in horses.

    Science.gov (United States)

    Barrett, Elizabeth J; Rodgerson, Dwayne H

    2014-08-01

    To describe an ultrasound assisted arthroscopic approach for removal of non-articular basilar sesamoid fragments in Thoroughbred yearlings. Thoroughbred yearlings (n = 7). Basilar sesamoid fragments identified during pre-sale radiographic examination were removed using a palmar/plantar arthroscopic approach to the fetlock joint and ultrasonographic guidance. Complete fragment removal was confirmed by ultrasonography and radiography. Basilar sesamoid fracture fragments were localized and removed successfully using rongeurs and a radiofrequency probe for soft tissue dissection of the fragment. Complete fragment removal was confirmed by ultrasonography and radiography. No intra- or postoperative complications occurred. At 6-8 months follow-up, no fragments or bony proliferation at the base of the sesamoid was observed. Ultrasonographic guidance can be used to facilitate localization, dissection, and confirmation of removal of basilar fragments of the proximal sesamoid bone. © Copyright 2014 by The American College of Veterinary Surgeons.

  8. Development and validation of ultrasound-assisted solid-liquid extraction of phenolic compounds from waste spent coffee grounds.

    Science.gov (United States)

    Al-Dhabi, Naif Abdullah; Ponmurugan, Karuppiah; Maran Jeganathan, Prakash

    2017-01-01

    In this current work, Box-Behnken statistical experimental design (BBD) was adopted to evaluate and optimize USLE (ultrasound-assisted solid-liquid extraction) of phytochemicals from spent coffee grounds. Factors employed in this study are ultrasonic power, temperature, time and solid-liquid (SL) ratio. Individual and interactive effect of independent variables over the extraction yield was depicted through mathematical models, which are generated from the experimental data. Determined optimum process conditions are 244W of ultrasonic power, 40°C of temperature, 34min of time and 1:17g/ml of SL ratio. The predicted values were in correlation with experimental values with 95% confidence level, under the determined optimal conditions. This indicates the significance of selected method for USLE of phytochemicals from SCG. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Ultrasound-assisted extraction of bioactive compounds from palm pressed fiber with high antioxidant and photoprotective activities.

    Science.gov (United States)

    Dal Prá, Valéria; Lunelli, Felipe C; Vendruscolo, Raquel Guidetti; Martins, Rafael; Wagner, Roger; Lazzaretti, Ayres P; Freire, Denise M Guimarães; Alexandri, Maria; Koutinas, Apostolis; Mazutti, Marcio A; da Rosa, Marcelo Barcellos

    2017-05-01

    This work is focused on the optimization of the ultrasound-assisted extraction of antioxidant compounds with photoprotective effect from palm pressed fiber. The influence of ultrasound intensity and pulse cycle was investigated by means of a central composite rotational design. The optimized condition was ultrasound intensity of 120W.cm -2 and pulse factor of 0.4, yielding 3.24wt%. Compounds such as fatty acids, β-sitosterol, α-tocopherol, squalene, total phenolics and carotene were identified. The extract presented antioxidant activity towards synthetic (2,2-diphenyl-1-picrylhydrazyl - DPPH, 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) - ABTS) and biological radicals (Hydroxyl - OH), besides a sun protection factor of 15.01. Polar extracts from palm pressed fiber are promising candidates for use in cosmetic and pharmaceutical formulation since they present high antioxidant activity towards different radicals, combined with the high sun protection factor. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Influencing factors and kinetics analysis on the leaching of iron from boron carbide waste-scrap with ultrasound-assisted method.

    Science.gov (United States)

    Li, Xin; Xing, Pengfei; Du, Xinghong; Gao, Shuaibo; Chen, Chen

    2017-09-01

    In this paper, the ultrasound-assisted leaching of iron from boron carbide waste-scrap was investigated and the optimization of different influencing factors had also been performed. The factors investigated were acid concentration, liquid-solid ratio, leaching temperature, ultrasonic power and frequency. The leaching of iron with conventional method at various temperatures was also performed. The results show the maximum iron leaching ratios are 87.4%, 94.5% for 80min-leaching with conventional method and 50min-leaching with ultrasound assistance, respectively. The leaching of waste-scrap with conventional method fits the chemical reaction-controlled model. The leaching with ultrasound assistance fits chemical reaction-controlled model, diffusion-controlled model for the first stage and second stage, respectively. The assistance of ultrasound can greatly improve the iron leaching ratio, accelerate the leaching rate, shorten leaching time and lower the residual iron, comparing with conventional method. The advantages of ultrasound-assisted leaching were also confirmed by the SEM-EDS analysis and elemental analysis of the raw material and leached solid samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. An ultrasound-assisted digestion method for the determination of toxic element concentrations in ash samples by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Ilander, Aki; Vaeisaenen, Ari

    2007-01-01

    A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of toxic element concentrations (arsenic, barium, cobalt, copper, lead, nickel, strontium, vanadium and zinc) in ash samples was developed. All the measurements were performed in robust plasma conditions which were tested by measuring the Mg(II) 280.270 nm/Mg(I) 285.213 nm line intensity ratios. The highest line intensity ratios were observed when a nebulizer gas flow of 0.6 L min -1 , auxiliary gas flow of 0.2 L min -1 and plasma power of 1400 W were used for radially viewed plasma. The analysis of SRM 1633b showed that the ultrasound-assisted method developed is highly comparable with the microwave digestion method standardized by the United States Environmental Protection Agency (EPA-3052). The ultrasound-assisted digestion with a digestion solution of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 81%. One exception is arsenic which resulted in recoveries of about 60% only; however, it could be digested with good recovery (>90%) using a digestion solution of 5 mL of water and 5 mL of aqua regia. The major advantage of the ultrasound-assisted digestion over microwave digestion is the high treatment rate (30 samples simultaneously with a sonication time of 18 min)

  12. Mechanistic study on ultrasound assisted pretreatment of sugarcane bagasse using metal salt with hydrogen peroxide for bioethanol production.

    Science.gov (United States)

    Ramadoss, Govindarajan; Muthukumar, Karuppan

    2016-01-01

    This study presents the ultrasound assisted pretreatment of sugarcane bagasse (SCB) using metal salt with hydrogen peroxide for bioethanol production. Among the different metal salts used, maximum holocellulose recovery and delignification were achieved with ultrasound assisted titanium dioxide (TiO2) pretreatment (UATP) system. At optimum conditions (1% H2O2, 4 g SCB dosage, 60 min sonication time, 2:100 M ratio of metal salt and H2O2, 75°C, 50% ultrasound amplitude and 70% ultrasound duty cycle), 94.98 ± 1.11% holocellulose recovery and 78.72 ± 0.86% delignification were observed. The pretreated SCB was subjected to dilute acid hydrolysis using 0.25% H2SO4 and maximum xylose, glucose and arabinose concentration obtained were 10.94 ± 0.35 g/L, 14.86 ± 0.12 g/L and 2.52 ± 0.27 g/L, respectively. The inhibitors production was found to be very less (0.93 ± 0.11 g/L furfural and 0.76 ± 0.62 g/L acetic acid) and the maximum theoretical yield of glucose and hemicellulose conversion attained were 85.8% and 77%, respectively. The fermentation was carried out using Saccharomyces cerevisiae and at the end of 72 h, 0.468 g bioethanol/g holocellulose was achieved. Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) analysis of pretreated SCB was made and its morphology was studied using scanning electron microscopy (SEM). The compounds formed during the pretreatment were identified using gas chromatography-mass spectrometry (GC-MS) analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Optimization of Ultrasound-Assisted Extraction, Preliminary Characterization and In Vitro Antioxidant Activity of Polysaccharides from Green Pea Pods

    Science.gov (United States)

    Jalili Safaryan, Maryam; Ganjloo, Ali; Bimakr, Mandana; Zarringhalami, Soheila

    2016-01-01

    In this study, ultrasound-assisted extraction of green pea pod polysaccharide (GPPP) was investigated and optimized using a central composite response surface design coupled with a numerical optimization technique. The effects of ultrasonic power (50–150 W), sonication time (20–80 min), ratio of water to raw material (20:1–40:1 mL/g) and extraction temperature (40–80 °C) on polysaccharide extraction yield were studied. The maximum extraction yield was obtained with a sonication power of 135.34 W, extraction time of 48.61 min, ratio of water to raw material of 33.6:1 mL/g and extraction temperature of 68.25 °C. Under these conditions, the experimental yield was 7.37% ± 0.13%, which was in close agreement with the predicted value (7.20%). The GPPP has been analyzed in order to identify a variety of chemical properties. The FT-IR spectrum demonstrated obvious characteristic peaks of polysaccharides. Furthermore, antioxidant activity of GPPP was evaluated by various antioxidant assays in vitro. The results revealed that GPPP possessed considerable DPPH free radical scavenging activity (91.03%), reducing power (0.63) and ferric reducing antioxidant power (0.34 mmol/L) at a total amount of 0.9 mg/mL. These findings indicated that GPPP extracted using an ultrasound-assisted extraction technique has potential as a novel source of natural antioxidant agent for future applications. PMID:28231174

  14. Optimization of Ultrasound-Assisted Extraction, Preliminary Characterization and In Vitro Antioxidant Activity of Polysaccharides from Green Pea Pods

    Directory of Open Access Journals (Sweden)

    Maryam Jalili Safaryan

    2016-11-01

    Full Text Available In this study, ultrasound-assisted extraction of green pea pod polysaccharide (GPPP was investigated and optimized using a central composite response surface design coupled with a numerical optimization technique. The effects of ultrasonic power (50–150 W, sonication time (20–80 min, ratio of water to raw material (20:1–40:1 mL/g and extraction temperature (40–80 °C on polysaccharide extraction yield were studied. The maximum extraction yield was obtained with a sonication power of 135.34 W, extraction time of 48.61 min, ratio of water to raw material of 33.6:1 mL/g and extraction temperature of 68.25 °C. Under these conditions, the experimental yield was 7.37% ± 0.13%, which was in close agreement with the predicted value (7.20%. The GPPP has been analyzed in order to identify a variety of chemical properties. The FT-IR spectrum demonstrated obvious characteristic peaks of polysaccharides. Furthermore, antioxidant activity of GPPP was evaluated by various antioxidant assays in vitro. The results revealed that GPPP possessed considerable DPPH free radical scavenging activity (91.03%, reducing power (0.63 and ferric reducing antioxidant power (0.34 mmol/L at a total amount of 0.9 mg/mL. These findings indicated that GPPP extracted using an ultrasound-assisted extraction technique has potential as a novel source of natural antioxidant agent for future applications.

  15. Analytical evaluation of a cup-horn sonoreactor used for ultrasound-assisted extraction of trace metals from troublesome matrices

    Science.gov (United States)

    De La Calle, Inmaculada; Cabaleiro, Noelia; Lavilla, Isela; Bendicho, Carlos

    2009-09-01

    In this work, a sample preparation method based on ultrasound-assisted extraction of trace metals from a variety of biological and environmental matrices using a cup-horn sonoreactor is described. Diluted acids (HNO 3, HCl and HF) and oxidants (H 2O 2) were tried for extraction, the extracts being directly analyzed by electrothermal-atomic absorption spectrometry. The cup-horn sonoreactor combines the advantages of probe and bath sonicators, allowing a variety of conditions to be used for metal extraction from troublesome matrices. This system facilitates the use of HF to destroy the silicate lattice, application of simultaneous treatments of up to six samples and short treatment times. Quantitative metal recoveries are achieved from different matrices (animal and vegetal tissues, soil, sediment, fly ash, sewage sludge) under a set of extraction conditions ranging from the use of 3 min sonication time and 3% volume/volume HNO 3 for some animal tissues to 40 min sonication time along with 5% volume/volume HNO 3 + 20% volume/volume HF for sediment. Vegetal matter required the use of 5% volume/volume HNO 3 + 5% volume/volume HF for extraction of some elements. Ultrasound-assisted extraction of Cd, Mn, Pb, Ni and Cr from 16 certified reference materials representing a variety of biological and environmental matrices using the cup-horn sonoreactor is evaluated. Cd, Pb and Mn are more easily extracted from most certified reference materials (CRMs) than Cr and Ni and less stringent conditions can be chosen for the former metals. Metal extractability follows the order of difficulty: animal tissue fly ash, sewage sludge < sediment.

  16. Analytical evaluation of a cup-horn sonoreactor used for ultrasound-assisted extraction of trace metals from troublesome matrices

    International Nuclear Information System (INIS)

    De La Calle, Inmaculada; Cabaleiro, Noelia; Lavilla, Isela; Bendicho, Carlos

    2009-01-01

    In this work, a sample preparation method based on ultrasound-assisted extraction of trace metals from a variety of biological and environmental matrices using a cup-horn sonoreactor is described. Diluted acids (HNO 3 , HCl and HF) and oxidants (H 2 O 2 ) were tried for extraction, the extracts being directly analyzed by electrothermal-atomic absorption spectrometry. The cup-horn sonoreactor combines the advantages of probe and bath sonicators, allowing a variety of conditions to be used for metal extraction from troublesome matrices. This system facilitates the use of HF to destroy the silicate lattice, application of simultaneous treatments of up to six samples and short treatment times. Quantitative metal recoveries are achieved from different matrices (animal and vegetal tissues, soil, sediment, fly ash, sewage sludge) under a set of extraction conditions ranging from the use of 3 min sonication time and 3% volume/volume HNO 3 for some animal tissues to 40 min sonication time along with 5% volume/volume HNO 3 + 20% volume/volume HF for sediment. Vegetal matter required the use of 5% volume/volume HNO 3 + 5% volume/volume HF for extraction of some elements. Ultrasound-assisted extraction of Cd, Mn, Pb, Ni and Cr from 16 certified reference materials representing a variety of biological and environmental matrices using the cup-horn sonoreactor is evaluated. Cd, Pb and Mn are more easily extracted from most certified reference materials (CRMs) than Cr and Ni and less stringent conditions can be chosen for the former metals. Metal extractability follows the order of difficulty: animal tissue < vegetal tissue < soil, fly ash, sewage sludge < sediment.

  17. Ultrasound assisted synthesis of ZnO/reduced graphene oxide composites with enhanced photocatalytic activity and anti-photocorrosion

    International Nuclear Information System (INIS)

    Peng, Yonggang; Ji, Junling; Chen, Dajun

    2015-01-01

    Graphical abstract: - Highlights: • ZnO/reduced graphene oxide composites were prepared by in situ growth with ultrasound assisted method. • A plausible formation mechanism of ZnO/rGO composites was deduced. • After hybridization with rGO, the photocatalytic activity of ZnO was improved and its photocorrosion was inhibited obviously. - Abstract: A method to improve the photocatalytic activity and suppress the photocorrosion of ZnO was developed by depositing ZnO nanoparticles onto the surface of reduced graphene oxide (rGO) via in situ growth with ultrasound assisted synthesis. The optimum synergetic effect of ZnO/rGO composite was found at a weight ratio of 2% (rGO/ZnO). Compared with ZnO, the photocatalytic activities of ZnO/rGO composite for the degradation of methylene blue (MB) and C.I. acid red 249 (AR249) aqueous solutions under UV light irradiation were increased by 8.6% and 14.7%, respectively. The improved photocatalytic activity was originated from the rapid separation of photogenerated electrons and holes on the interface of rGO and ZnO. The photocorrosion of ZnO was inhibited obviously after hybridization with rGO. Even after six successive cycles under UV irradiation, the photocatalytic activities of ZnO/rGO composite for MB and AR249 still retained 92.9% and 94.8% of that for the first cycling run, while that of ZnO obviously decreased due to serious photocorrosion. The photocorrosion inhibition of ZnO by rGO was attributed to the reduced activation of surface oxygen atom on the surface of ZnO.

  18. Ultrasound-assisted synthesis and characterization of magnetite nanoparticles and poly(methyl methacrylate)/magnetite nanocomposites.

    Science.gov (United States)

    Poddar, Maneesh Kumar; Arjmand, Mohammad; Sundararaj, Uttandaraman; Moholkar, Vijayanand S

    2018-05-01

    Poly(methyl methacrylate)/magnetite (PMMA/Fe 3 O 4 ) nanocomposites were prepared with a two-step technique involving sonication. Fe 3 O 4 nanoparticles were synthesized by ultrasound-assisted co-precipitation, and then PMMA/Fe 3 O 4 (1-5 wt%) nanocomposites were synthesized via ultrasound-assisted in-situ emulsion polymerization. Best physical properties of the nanocomposites for different Fe 3 O 4 loadings were: tensile strength (2 wt%) = 40.28 MPa, Young's modulus (2 wt%) = 2.4 GPa, percentage elongation (2 wt%) = 2.24%, glass transition temperature (2 wt%) = 122.5 °C, thermal inflection point (2 wt%) = 383 °C, electrical conductivity (5 wt%) = 2.0 × 10 -13  S/cm, coercivity = 59.85 Oe (2 wt%), magnetic saturation (5 wt%) = 5.12 emu/g, magnetic remanence (5 wt%) = 0.56 emu/g, and electromagnetic interference shielding effectiveness (5 wt%) = 1.45 dB. This unique combination of physical properties at relatively low Fe 3 O 4 loading is attributed to ultrasound-mediated uniform dispersion of the nanofiller in the polymer matrix. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. An efficient and green sonochemical synthesis of some new eco-friendly functionalized ionic liquids

    Directory of Open Access Journals (Sweden)

    Mouslim Messali

    2014-01-01

    Full Text Available Considerable stress to replace a lot of volatile organic compounds which were used as solvents in synthetic organic chemistry has been done for many chemical industries. A suitable solution for these problems is found by using the ionic liquids as a clean medium of working and avoiding the solvent effect. The present work describes a facile and green ultrasound-assisted procedure as an environmentally friendly alternative to traditional methods for the preparation of a series of 26 new functionalized imidazolium-based ionic liquids. Their structures were characterized by FT-IR, 1H, 13C, 11B, 19F, 31P NMR and mass spectra.

  20. Ultrasound-assisted extraction of lipids from Chlorella vulgaris using [Bmim][MeSO4

    International Nuclear Information System (INIS)

    Kim, Young-Hoo; Park, Saerom; Kim, Min Hoo; Choi, Yong-Keun; Yang, Yung-Hun; Kim, Hyung Joo; Kim, Hyungsup; Kim, Han-Soo; Song, Kyung-Guen; Lee, Sang Hyun

    2013-01-01

    Lipids from Chlorella vulgaris were successfully extracted using an ionic liquid, [Bmim][MeSO 4 ]. [Bmim][MeSO 4 ] dissolved C. vulgaris, leaving the lipids insoluble. The undissolved lipids could easily be recovered due to the lower density of the lipid phase. Furthermore, ultrasound irradiation highly enhanced the extraction rate and yield with [Bmim][MeSO 4 ]. The total amounts of lipid extracted from C. vulgaris by the Soxhlet method and the Bligh and Dyer's method were 21 and 29 mg/g dry cell weight (DCW), respectively, whereas it was 47 mg/g DCW with [Bmim][MeSO 4 ]. Additionally, the amount of lipid extracted using [Bmim][MeSO 4 ] was 1.6 times greater with ultrasound irradiation. The rate of extraction of lipids from C. vulgaris with [Bmim][MeSO 4 ] was also 2.7 times greater with ultrasound irradiation. The fatty acid profiles of the lipids extracted using [Bmim][MeSO 4 ] were very similar to those of the lipids obtained by Bligh and Dyer's method. -- Highlights: •[Bmim][MeSO 4 ] efficiently extracted lipids from algae without pretreatment. •Ultrasound irradiation highly enhanced the extraction rate and yield of the extraction system using IL. •Fatty acid profiles of lipids extracted using [Bmim][MeSO 4 ] were similar to those of the lipids obtained by conventional methods

  1. Ultrasound-assisted lipase-catalyzed synthesis of D-isoascorbyl palmitate: process optimization and Kinetic evaluation

    Science.gov (United States)

    2013-01-01

    Background D-isoascorbic acid is a food antioxidant additive and used in accordance with Good Manufacturing Practice (GMP). High solubility in water (about 150 g/L at 25°C) reduces its effectiveness in stabilizing fats and oils. Our research group had successfully synthesized D-isoascorbyl palmitate using immobilized lipase Novozym 435 as a biocatalyst. Low production efficiency of D-isoascorbyl palmitate is still a problem for industrial production due to the long reaction time of over 24 h. In the present work, ultrasonic treatment was applied for accelerating the reaction process. The operation parameters were optimized to obtain the maximum D-isoascorbyl palmitate conversion rate by using a 5-level-4-factor Central Composite Design (CCD) and Response Surface Methdology (RSM). The reaction apparent kinetic parameters under the ultrasound treatment and mechanical shaking conditions were also determined and compared. Results Results showed that ultrasound treatment decreased the reaction time by over 50%. D-isoascorbyl palmitate yielded to 94.32 ± 0.17% and the productivity reached to 8.67 g L-1 h-1 under the optimized conditions as: 9% of enzyme load (w/w), 61°C of reaction temperature, 1:5 of D- isoascorbic-to-palmitic acid molar ratio, and 137 W of the ultrasound power. The immobilized lipase Novozym 435 could be reused for 7 times with 65% of the remained D-isoascorbyl palmitate conversion rate. The reaction kinetics showed that the maximum apparent reaction rate (vmax) of the ultrasound-assisted reaction was 2.85 times higher than that of the mechanical shaking, which proved that ultrasound treatment significantly enhanced the reaction efficiency. Conclusion A systematic study on ultrasound-assisted enzymatic esterification for D-isoascorbyl palmitate production is reported. The results show a promising perspective of the ultrasound technique to reduce the reaction time and improve the production efficiency. The commercial D-isoascorbyl palmitate

  2. Ultrasound-assisted polyol method for the preparation of SBA-15-supported ruthenium nanoparticles and the study of their catalytic activity on the partial oxidation of methane.

    Science.gov (United States)

    Li, Hongliang; Wang, Renzhang; Hong, Qi; Chen, Luwei; Zhong, Ziyi; Koltypin, Yuri; Calderon-Moreno, J; Gedanken, Aharon

    2004-09-14

    Metallic Ru nanoparticles have been successfully produced and incorporated into the pores of SBA-15 in situ employing a simple ultrasound-assisted polyol method. The product has been confirmed by X-ray diffraction, transmission electron microscopy, and X-ray photoelectron spectroscopy, where ultrasound provides both the energy for the reduction of the Ru(III) ion and the driving force for the loading of the Ru(0) nanoparticles into the SBA-15 pores. An ultrasound-assisted insertion mechanism has been proposed based on the microjets and shake-wave effect of the collapsed bubbles. The catalytic properties of the SBA-15-supported Ru nanoparticles have been tested by the partial oxidization of methane and show very high activity and high CO selectivity.

  3. A novel ultrasound-assisted approach to the synthesis of CdSe and CdS nanoparticles

    International Nuclear Information System (INIS)

    Li Hongliang; Zhu Yingchun; Chen Siguang; Palchik, Oleg; Xiong Jinping; Koltypin, Yuri; Gofer, Yosef; Gedanken, Aharon

    2003-01-01

    Hexagonal CdSe and hexagonal CdS nanoparticles have been prepared using Cd(Ac) 2 and less hazardous elemental Se or S as precursors, respectively, with the aid of ultrasound irradiation under an atmosphere of H 2 /Ar (5/95, V/V). The products consist of 7-10 nm nanocrystallites which aggregated in the form of polydispersive nanoclusters with sizes in the range 30-40 nm in the case of CdSe, and near monodispersive nanoclusters with a mean size of about 40 nm in the case of CdS. X-ray diffraction, high-resolution TEM and SAED patterns (selected area electron diffraction patterns) show that the as-prepared particles are well crystallized. X-ray photoelectron spectroscopy (XPS) measurements further confirm the formation of CdSe and CdS. Diffuse reflection spectra indicate that both the CdSe and the CdS nanocryslallites are direct band-gap semiconductors with band-gap values of about 1.83 and 2.62 eV, respectively. Control experiments demonstrate that the hydrogen is the reducing agent, and the extreme high temperature induced by the collapse of the bubble accelerates the reduction of elemental Se or S by hydrogen. An ultrasound assisted in situ reduction/combination mechanism is proposed

  4. Optimization of ultrasound-assisted extraction of phenolic compounds, antioxidants, and anthocyanins from grape (Vitis vinifera) seeds.

    Science.gov (United States)

    Ghafoor, Kashif; Choi, Yong Hee; Jeon, Ju Yeong; Jo, In Hee

    2009-06-10

    Important functional components from Campbell Early grape seed were extracted by ultrasound-assisted extraction (UAE) technology. The experiments were carried out according to a five level, three variable central composite rotatable design (CCRD). The best possible combinations of ethanol concentration, extraction temperature, and extraction time with the application of ultrasound were obtained for the maximum extraction of phenolic compounds, antioxidant activities, and anthocyanins from grape seed by using response surface methodology (RSM). Process variables had significant effect on the extraction of functional components with extraction time being highly significant for the extraction of phenolics and antioxidants. The optimal conditions obtained by RSM for UAE from grape seed include 53.15% ethanol, 56.03 degrees C temperature, and 29.03 min time for the maximum total phenolic compounds (5.44 mg GAE/100 mL); 53.06% ethanol, 60.65 degrees C temperature, and 30.58 min time for the maximum antioxidant activity (12.31 mg/mL); and 52.35% ethanol, 55.13 degrees C temperature, and 29.49 min time for the maximum total anthocyanins (2.28 mg/mL). Under the above-mentioned conditions, the experimental total phenolics were 5.41 mg GAE/100 mL, antioxidant activity was 12.28 mg/mL, and total anthocyanins were 2.29 mg/mL of the grape seed extract, which is well matched with the predicted values.

  5. Optimization of ultrasound-assisted extraction of phenolic compounds, antioxidants and rosmarinic acid from perilla leaves using response surface methodology

    Directory of Open Access Journals (Sweden)

    Hui-Zhen LI

    Full Text Available Abstract Response surface methodology (RSM was used to optimize ultrasound-assisted extraction (UAE of functional components from perilla leaves. The factors investigated were ethanol concentration, extraction temperature, and extraction time. The results revealed that ethanol concentration had significant effects on all extraction parameters. Based on the RSM results, the optimal conditions were an ethanol concentration of 56%, a UAE temperature of 54 °C, and a UAE time of 55 min. Under these conditions, the experimental TPC (total phenolic content, RA (rosmarinic acid, FRAP (ferric reducing antioxidant power and DPPH (1,1-diphenyl-2-picrylhydrazyl values were 48.85 mg GAE/g DW (mg gallic acid equivalent /g of dry weight, 31.02 mg/g DW, 85.55 μmol Fe2+/g DW and 73.35%, respectively. The experimental values were in agreement with those predicted by RSM models, confirming suitability of the model employed and the success of RSM for optimization of the extraction conditions.

  6. Optimization for ultrasound-assisted extraction of polysaccharides with chemical composition and antioxidant activity from the Artemisia sphaerocephala Krasch seeds.

    Science.gov (United States)

    Zheng, Quan; Ren, Daoyuan; Yang, Nana; Yang, Xingbin

    2016-10-01

    Artemisia sphaerocephala Krasch seeds polysaccharides have been reported to have a variety of important biological activities. However, effective extraction of Artemisia sphaerocephala Krasch seeds polysaccharides is still an unsolved issue. In this study, the orthogonal rotatable central composite design was employed to optimize ultrasound-assisted extraction conditions of Artemisia sphaerocephala Krasch seeds polysaccharides. Based on a single-factor analysis method, ultrasonic power, extraction time, solid-liquid ratio and extraction temperature were shown to significantly affect the yield of polysaccharides extracted from the A. sphaerocephala Krasch seeds. The optimal conditions for extraction of Artemisia sphaerocephala Krasch seeds polysaccharides were determined as following: ultrasonic power 243W, extraction time 125min, solid-liquid ratio 64:1 and extraction temperature 64°C, where the experimental yield was 14.78%, which was well matched with the predicted value of 14.81%. Furthermore, ASKP was identified as a typical heteropolysaccharide with d-galacturonic acid (38.8%) d-galactose (20.2%) and d-xylose (15.5%) being the main constitutive monosaccharides. Moreover, Artemisia sphaerocephala Krasch seeds polysaccharides exhibited high total reducing power and considerable scavenging activities on DPPH, hydroxyl and superoxide radicals, in a concentration-dependent manner in vitro. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Optimization of Ultrasound-Assisted Extraction of Natural Antioxidants from Sugar Apple (Annona squamosa L.) Peel Using Response Surface Methodology.

    Science.gov (United States)

    Deng, Gui-Fang; Xu, Dong-Ping; Li, Sha; Li, Hua-Bin

    2015-11-17

    Sugar apple (Annona squamosa L.) is a popular tropical fruit and its peel is a municipal waste. An ultrasound-assisted extraction method was developed for the recovery of natural antioxidants from sugar apple peel. Central composite design was used to optimize solvent concentration (13.2%-46.8%), ultrasonic time (33.2-66.8 min), and temperature (43.2-76.8 °C) for the recovery of natural antioxidants from sugar apple peel. The second-order polynomial models demonstrated a good fit of the quadratic models with the experimental results in respect to total phenolic content (TPC, R²=0.9524, pextraction conditions were 20:1 (mL/g) of solvent-to-solid ratio, 32.68% acetone, and 67.23 °C for 42.54 min under ultrasonic irradiation. Under these conditions, the maximal yield of total phenolic content was 26.81 (mg GA/g FW). The experimental results obtained under optimal conditions agreed well with the predicted results. The application of ultrasound markedly decreased extraction time and improved the extraction efficiency, compared with the conventional methods.

  8. Extraction Optimization, Characterization, and Bioactivities of Polysaccharides from Pinelliae Rhizoma Praeparatum Cum Alumine Employing Ultrasound-Assisted Extraction.

    Science.gov (United States)

    Liu, Yu-Jie; Mo, Xue-Lin; Tang, Xiao-Zhang; Li, Jiang-Hua; Hu, Mei-Bian; Yan, Dan; Peng, Wei; Wu, Chun-Jie

    2017-06-09

    In this study, the ultrasound-assisted extraction of polysaccharides (PSA) from Pinelliae Rhizoma Praeparatum Cum Alumine (PRPCA) was optimized by response surface methodology (RSM). The structural characteristics of PSA were analyzed by UV-vis spectroscopy, infrared spectroscopy, scanning electron microscopy, high performance gel permeation chromatography and high performance liquid chromatography, respectively. In addition, antioxidant and antimicrobial activities of PSA were studied by different in vitro assays. Results indicated that the optimal extraction conditions were as follows: the ratio of water to raw of 30 mL/g, extraction time of 46.50 min, ultrasonic temperature of 72.00 °C, and ultrasonic power of 230 W. Under these conditions, the obtained PSA yield (13.21 ± 0.37%) was closely agreed with the predicted yield by the model. The average molecular weights of the PSA were estimated to be 5.34 × 10³ and 6.27 × 10⁵ Da. Monosaccharide composition analysis indicated that PSA consisted of mannose, galactose uronic acid, glucose, galactose, arabinose with a molar ratio of 1.83:0.55:75.75:1.94:0.45. Furthermore, PSA exhibited moderate antioxidant and antibacterial activities in vitro. Collectively, this study provides a promising strategy to obtain bioactive polysaccharides from processed products of herbal medicines.

  9. Ultrasound-assisted extraction and preliminary purification of proanthocyanidins and chlorogenic acid from almond (Prunus dulcis) skin.

    Science.gov (United States)

    Ma, Xue; Zhou, Xin-Yu; Qiang, Qian-Qian; Zhang, Zhi-Qi

    2014-07-01

    An aqueous solution of polyethylene glycol (PEG) as a green solvent was employed for the first time to develop the ultrasound-assisted extraction of proanthocyanidins (PA) and chlorogenic acid (CA) from almond skin. The optimized extraction parameters were determined based on response surface methodology, and corresponded to an ultrasound power of 120 W, a liquid-to-solid ratio of 20:1 (mL/g), and a PEG concentration of 50% (v/v). Under these optimized conditions, the extraction yields of PAs and CA from almond skin were 32.68 ± 0.22 and 16.01 ± 0.19 mg/g, respectively. Compared with organic solvent extraction, PEG solution extraction produced higher yields. Different macroporous resins were compared for their performance in purifying PAs and CA from almond skin extract. Static adsorption/desorption experimental results demonstrated that AB-8 resin exhibits excellent purification performance at pH 4. Under the optimized dynamic adsorption/desorption conditions on the AB-8 column, the total recovery of purification for PAs and CA was 80.67%. The total content of PAs and CA in the preliminarily purified extract was 89.17% (with respective contents of 60.90 and 28.27%). © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Ultrasound assisted extraction of natural dye from jackfruit's wood (Artocarpus heterophyllus): The effect of ethanol concentration as a solvent

    Science.gov (United States)

    Febriana, Ike Dayi; Gala, Selfina; Mahfud, Mahfud

    2017-05-01

    Azo dye are synthetic organic dyes which has an azo group (- N = N -) as chromophore. Azo dye is resistand to decomposition process and harmfull for the environment and human being. Natural dye can be used as substitution of azo dye at textile industry. Natural dye are eco - friendly and can be applied for dyeing of fibrous material. Natural dye can be obtained from natural origin such as leaves, wood, or roots. The wood of jackfruit (Artocarpus heterophyllus) can used as natural source of natural dye. Ultrasound assisted extraction (UAE) is a new method that can be used to extract natural dye from jackfruit's wood. The aim of this research are to study about influence of ethanol concentration as solvent and extraction kinetic. Jackfruit's wood dust from sawmill used for the experimentation were sifted by sieve 35 mesh. Ethanol 96% used as solvent of this experiment and varied the concentration in volume to volume ratio (v/v). Experiment were carried out from 20 to 50 minutes. The result of this experiment shows that ethanol concentration influenced yield of extraction from jackfruit's wood. Concentration of ethanol will be affected polarity of solvent. The Peleg model was used to describe about kinetic model of natural dye extraction. Value of k1 and k2 constant are 0.003835 and 0.04186 respectively.

  11. Morphologic, magnetic, and Moessbauer spectral properties of Fe75Co25 nanoparticles prepared by ultrasound-assisted electrochemistry

    International Nuclear Information System (INIS)

    Mancier, Valerie; Delplancke, J.-L.; Delwiche, Jacques; Hubin-Franskin, M.-J.; Piquer, Cristina; Rebbouh, Leila; Grandjean, Fernande

    2004-01-01

    Nanopowders of Fe 75 Co 25 alloys have been prepared by ultrasound-assisted electrochemistry. Their composition, crystallographic structure, morphology, have been studied by X-ray diffraction, transmission electron microscopy, X-ray fluorescence, and high-energy electron diffraction. The nanopowders are found to present a composition well determined by the electrolyte bath composition, they show a bcc structure. The iron and cobalt atoms exhibit a very homogeneous distribution in the particles. The magnetic properties of the nanopowders have been measured between 5 and 295 K with a vibrating sample magnetometer and their Moessbauer spectra have been obtained at 295 K. The saturation magnetization is characteristic of FeCo alloys. The magnetic behavior and transmission electron microscopy observations of the particles indicate strongly interacting particles with a radius of ca. 2-4 nm, particles which may form agglomerates of larger size. The measured average hyperfine field is situated at the maximum of the Slater-Pauling curve for the FeCo alloys

  12. Microwave- and ultrasound-assisted extraction of vanillin and its quantification by high-performance liquid chromatography in Vanilla planifolia.

    Science.gov (United States)

    Sharma, Anuj; Verma, Subash Chandra; Saxena, Nisha; Chadda, Neetu; Singh, Narendra Pratap; Sinha, Arun Kumar

    2006-03-01

    Microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE) and conventional extraction of vanillin and its quantification by HPLC in pods of Vanilla planifolia is described. A range of nonpolar to polar solvents were used for the extraction of vanillin employing MAE, UAE and conventional methods. Various extraction parameters such as nature of the solvent, solvent volume, time of irradiation, microwave and ultrasound energy inputs were optimized. HPLC was performed on RP ODS column (4.6 mm ID x 250 mm, 5 microm, Waters), a photodiode array detector (Waters 2996) using gradient solvent system of ACN and ortho-phosphoric acid in water (0.001:99.999 v/v) at 25 degrees C. Regression equation revealed a linear relationship (r2 > 0.9998) between the mass of vanillin injected and the peak areas. The detection limit (S/N = 3) and limit of quantification (S/N = 10) were 0.65 and 1.2 microg/g, respectively. Recovery was achieved in the range 98.5-99.6% for vanillin. Maximum yield of vanilla extract (29.81, 29.068 and 14.31% by conventional extraction, MAE and UAE, respectively) was found in a mixture of ethanol/water (40:60 v/v). Dehydrated ethanolic extract showed the highest amount of vanillin (1.8, 1.25 and 0.99% by MAE, conventional extraction and UAE, respectively).

  13. Ultrasound-assisted HCl-NaCl leaching of lead-rich and antimony-rich oxidizing slag.

    Science.gov (United States)

    Zhang, Rong Liang; Zhang, Xiao Fei; Tang, Shu Zhen; Huang, Ai Dong

    2015-11-01

    Lead-rich and antimony-rich oxidizing slag was subjected to regular HCl-NaCl leaching, with the experimental conditions optimized under which ultrasound was introduced. After only 15 min of ultrasound-assisted leaching, the leaching rate of Sb resembled that after 45 min of regular leaching. Ultrasonic treatment considerably elevated the leaching rates of Sb and Pb, and shortened the leaching time. With the decrease of particle size, the leaching rate of Sb and Pb increased gradually. Especially, as the particle size of the slag was greater than 0.217 mm, the ultrasonic leaching effects of Sb and Pb were significantly higher than that of regular leaching effects. The temperature exhibited great effect on ultrasonic leaching performance. As the temperature increased, the leaching rates of Sb and Pb increased step by step. In case the temperature was higher than 85°C, the increasing speed of the leaching rates for Sb and Pb tended to be slow. Increasing ultrasonic power could augment the leaching rate or accelerate the procedure till the same leaching rate. However, since ultrasound failed to energize the formation of new reaction pathways, the maximum leaching rates of Sb and Pb were determined by their phase compositions rather than by ultrasonic field. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Optimization of ultrasound-assisted extraction of grape seed oil to enhance process yield and minimize free radical formation.

    Science.gov (United States)

    Böger, Bruna R; Salviato, Aroldo; Valezi, Daniel F; Di Mauro, Eduardo; Georgetti, Sandra R; Kurozawa, Louise E

    2018-03-30

    Grape seeds are a relatively abundant source of oil and bioactive compounds. In order to use this by-product, the current work aimed to optimize the ultrasound-assisted extraction of grape seed oil to obtain greater process yield and minimize free radicals formation in the oil. The optimal condition was 15°C and amplitude of ultrasonic wave of 42 μm, leading to a process yield of 82.9% and content of free radicals of 14.7×10 17 kg -1 and 3.4×10 18 kg -1 for samples stored for 7 and 30 days, respectively. No significant differences in fatty acid composition and acidity and iodine values were observed between samples. The oil obtained by ultrasound had greater phenolic compound content and antioxidant activity by ferric reduction than the control sample (without ultrasound application). However, higher content of free radicals and peroxide value was observed. Sonication improved extraction yield when compared to the process without ultrasound application. Moreover, UAE favored phenolic compounds extraction. Since the proposed condition extraction enhanced process yield with the minimum formation of free radicals, UAE is a promising oil extraction technology. This article is protected by copyright. All rights reserved.

  15. Extraction of indium-tin oxide from end-of-life LCD panels using ultrasound assisted acid leaching.

    Science.gov (United States)

    Souada, Malika; Louage, Christophe; Doisy, Jean-Yves; Meunier, Ludivine; Benderrag, Abdelkader; Ouddane, Baghdad; Bellayer, Séverine; Nuns, Nicolas; Traisnel, Michel; Maschke, Ulrich

    2018-01-01

    In this report, indium-tin-oxide (ITO)-layer extraction from end-of-life (EOL) Liquid Crystal Displays (LCDs) was discussed by sulfuric acid leaching with simultaneous application of ultrasonication on the ITO-side of glass/ITO panels, exhibiting various dimensions. Applying this technique presents several advantages compared to the traditional leaching process such as fast and controllable kinetics, high extraction yield of indium and tin, selective recovery of these two metals possible, and the opportunity to recycle the neat glass separately avoiding additional separation processes. ITO-dissolution kinetics from EOL LCD panels were investigated as function of leaching time and acidity of sulfuric acid. At a temperature of 60°C, a nearly quantitative indium yield was obtained using an acid concentration of 18mol/L by simultaneous application of ultrasonication, whereas only 70% were recovered in the absence of ultrasound. Results from ICP-AES agreed well with SEM/BSE observations demonstrating the high efficiency of the ultrasound assisted process since only 3-4min were required to obtain maximum ITO recovery. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Ultrasound-assisted xanthation of cellulose from lignocellulosic biomass optimized by response surface methodology for Pb(II) sorption.

    Science.gov (United States)

    Wang, Chongqing; Wang, Hui; Gu, Guohua

    2018-02-15

    Alkali treatment of lignocellulosic biomass is conducted to remove hemi-cellulose and lignin, further increasing the reactivity and accessibility of cellulose. Ultrasound-assisted xanthation of alkali cellulose is optimized by response surface methodology (RSM) with a Box-Behnken design. A predicting mathematical model is obtained by fitting experimental data, and it is verified by analysis of variance. Response surface plots and the contour plots obtained from the model are applied to determine the interactions of experimental variables. The optimum conditions are NaOH concentration 1.3mol/L, ultrasonic time 71.6min and CS 2 dosage 1.5mL. FTIR, SEM and XPS characterizations confirm the synthesis and sorption mechanism of cellulose xanthate (CX). Biosorption of Pb (II) onto CX obeys pseudo-second order model and Langmuir model. The sorption mechanism is attributed to surface complexation or ion exchange. CX shows good reusability for Pb (II) sorption. The maximum sorption capacity of Pb(II) is 134.41mg/g, higher than that of other biosorbents. CX has great potential as an efficient and low-cost biosorbent for wastewater treatment. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Optimization of Ultrasound-Assisted Extraction of Natural Antioxidants from Sugar Apple (Annona squamosa L. Peel Using Response Surface Methodology

    Directory of Open Access Journals (Sweden)

    Gui-Fang Deng

    2015-11-01

    Full Text Available Sugar apple (Annona squamosa L. is a popular tropical fruit and its peel is a municipal waste. An ultrasound-assisted extraction method was developed for the recovery of natural antioxidants from sugar apple peel. Central composite design was used to optimize solvent concentration (13.2%–46.8%, ultrasonic time (33.2–66.8 min, and temperature (43.2–76.8 °C for the recovery of natural antioxidants from sugar apple peel. The second-order polynomial models demonstrated a good fit of the quadratic models with the experimental results in respect to total phenolic content (TPC, R2 = 0.9524, p < 0.0001, FRAP (R2 = 0.9743, p < 0.0001, and TEAC (R2 = 0.9610, p < 0.0001 values. The optimal extraction conditions were 20:1 (mL/g of solvent-to-solid ratio, 32.68% acetone, and 67.23 °C for 42.54 min under ultrasonic irradiation. Under these conditions, the maximal yield of total phenolic content was 26.81 (mg GA/g FW. The experimental results obtained under optimal conditions agreed well with the predicted results. The application of ultrasound markedly decreased extraction time and improved the extraction efficiency, compared with the conventional methods.

  18. Optimization of ultrasound-assisted extraction of antioxidant compounds from Tunisian Zizyphus lotus fruits using response surface methodology.

    Science.gov (United States)

    Hammi, Khaoula Mkadmini; Jdey, Ahmed; Abdelly, Chedly; Majdoub, Hatem; Ksouri, Riadh

    2015-10-01

    The optimization of antioxidant extraction conditions from a ripe edible fruits of Zizyphus lotus (L.) with an ultrasound-assisted system was achieved by response surface methodology. The central composite rotatable design was employed for optimization of extraction parameters in terms of total phenolic content and antioxidant activities using 2,2-diphenyl-1-picrylhydrazyl radical scavenging activity and phosphomolybdenum assay. The optimum operating conditions for extraction were as follows: ethanol concentration, 50%; extraction time, 25 min; extraction temperature, 63°C and ratio of solvent to solid, 67 mL/g. Under these conditions, the obtained extract exhibited a high content of phenolic compounds (40.782 mg gallic acid equivalents/g dry matter) with significant antioxidant properties (the total antioxidant activity was 75.981 mg gallic acid equivalents/g dry matter and the 2,2-diphenyl-1-picrylhydrazyl radical scavenging activity was 0.289 mg/mL). Copyright © 2015 Elsevier Ltd. All rights reserved.

  19. Multivariate optimization of an ultrasound-assisted extraction procedure for Cu, Mn, Ni and Zn determination in ration to chickens

    Directory of Open Access Journals (Sweden)

    JOELIA M. BARROS

    2013-09-01

    Full Text Available In this work, multivariate optimization techniques were used to develop a method based on the ultrasound-assisted extraction for copper, manganese, nickel and zinc determination from rations for chicken nutrition using flame atomic absorption spectrometry. The proportions of extracting components (2.0 mol.L–1 nitric, hydrochloric and acetic acid solutions were optimized using centroid-simplex mixture design. The optimum proportions of this mixture taken as percentage of each component were respectively 20%, 37% and 43%. Variables of method (sample mass, sonication time and final acid concentration were optimized using Doehlert design. The optimum values found for these variables were respectively 0.24 g, 18s and 3.6 mol.L–1. The developed method allows copper, manganese, nickel and zinc determination with quantification limits of 2.82; 4.52; 10.7; e 9.69 µg.g–1, and precision expressed as relative standard deviation (%RSD, 25 µg.g–1, N = 5 of 5.30; 2.13; 0.88; and 0.83%, respectively. This method was applied in the analytes determination from chicken rations collected from specialized commerce in Jequié city (Bahia State/Brazil. Application of paired t-test at the obtained results, in a confidence level of 95%, does not show significant difference between the proposed method and the microwave-assisted digestion.

  20. Comparison of Ultrasound-Assisted and Regular Leaching of Vanadium and Chromium from Roasted High Chromium Vanadium Slag

    Science.gov (United States)

    Wen, Jing; Jiang, Tao; Gao, Huiyang; Liu, Yajing; Zheng, Xiaole; Xue, Xiangxin

    2018-02-01

    Ultrasound-assisted leaching (UAL) was used for vanadium and chromium leaching from roasted material obtained by the calcification roasting of high-chromium-vanadium slag. UAL was compared with regular leaching. The effect of the leaching time and temperature, acid concentration, and liquid-solid ratio on the vanadium and chromium leaching behaviors was investigated. The UAL mechanism was determined from particle-size-distribution and microstructure analyses. UAL decreased the reaction time and leaching temperature significantly. Furthermore, 96.67% vanadium and less than 1% chromium were leached at 60°C for 60 min with 20% H2SO4 at a liquid-solid ratio of 8, which was higher than the maximum vanadium leaching rate of 90.89% obtained using regular leaching at 80°C for 120 min. Ultrasonic waves broke and dispersed the solid sample because of ultrasonic cavitation, which increased the contact area of the roasted sample and the leaching medium, the solid-liquid mass transfer, and the vanadium leaching rate.

  1. Optimization of Ultrasound-Assisted Extraction of Antioxidants from Apium graveolens L. Seeds using Response Surface Methodology

    Directory of Open Access Journals (Sweden)

    Şule Dinç Zor

    2017-09-01

    Full Text Available In this study, optimum conditions for ultrasound-assisted extraction (UAE of antioxidants from Apium graveolens L. seeds were investigated by Response Surface Methodology (RSM. A Box-Behnken Design (BBD was used to evaluate the effect of sonication time (5, 10, 15 min, ultrasound power (60, 120, 180 W and the ratio of extraction solvent in terms of methanol (0, 50, 100% on antioxidant capacity. The optimal UAE conditions for the parameters investigated were 11 min of sonication time, ultrasound power of 131 W and 100% methanol as an extraction solvent. Under these conditions, UAE of antioxidants from the seeds achieved a maximum of 95.08% in respect to 1,1-diphenyl-2-picryl hydrazyl (DPPH radical scavenging activity. Additionally, the high value of the adjusted coefficient of determination (R2adj = 0.9192 and the non-significant difference between experimental and predicted values confirmed the validity of the quadratic polynomial model. Hence, UAE is a suitable, fast, economical and practical technique for the extraction of antioxidants from Apium graveolens L. seeds.

  2. Synthesis and application of magnetic deep eutectic solvents: Novel solvents for ultrasound assisted liquid-liquid microextraction of thiophene.

    Science.gov (United States)

    Khezeli, Tahere; Daneshfar, Ali

    2017-09-01

    Two novel magnetic deep eutectic solvents (MDESs), comprised of cheap and simple components named [choline chloride/phenol] [FeCl 4 ] and [choline chloride/ethylene glycol] [FeCl 4 ] were prepared and characterized by CHN elemental analysis, proton nuclear magnetic resonance ( 1 H NMR), vibrating sample magnetometery (VSM), Raman, Fourier transform-infrared (FT-IR) and UV-Vis spectrometery. The extraction efficiency of the prepared MDESs has been investigated in ultrasound assisted liquid-liquid microextraction based MDES (UALLME-MDES). Briefly, MDESs were added to n-heptan containing thiophene. Then, MDESs were dispersed in n-heptane by sonication. After that, microdroplets of MDESs were collected by a magnet and the remained concentration of thiophene in n-heptane phase was analyzed by GC-FID. The results indicated that [choline chloride/phenol] [FeCl 4 ] has higher extraction efficiency than [choline chloride/ethylene glycol] [FeCl 4 ]. This work opens a new way to the application of MDESs. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Influence of the degree of inulin polymerization on the ultrasound-assisted encapsulation of annatto seed oil.

    Science.gov (United States)

    Silva, Eric Keven; Meireles, M Angela A

    2015-11-20

    The effect of the degree of polymerization (DP) of inulin was evaluated on its encapsulant characteristics. We assessed the influence of the average inulin DP (DP ≥10 and DP ≥23) in the ultrasound-assisted encapsulation of annatto seed oil using the freeze-drying technique for particle formation. The intensification of the homogenization process with ultrasound did not improve the characteristics of the emulsions due to the physicochemical limitations of the inulin molecular chain (molecules do not exhibit surface activity). The particle morphology, oil entrapment efficiency, encapsulation efficiency, X-ray diffraction, thermogravimetric analysis and Rancimat analyses proved the effectiveness of inulin as a wall material. The properties influenced by the DP were the surface oil, encapsulation efficiency, water activity, particle size and oxidative stability of the encapsulated oil because the highest DP promoted the formation of microparticles with lower surface oil content, greater encapsulation efficiency, low water activity, larger size and greater protection against oil oxidation. Copyright © 2015 Elsevier Ltd. All rights reserved.

  4. Optimisation of ultrasound-assisted extraction of natural pigment from annatto seeds by response surface methodology (RSM).

    Science.gov (United States)

    Yolmeh, Mahmoud; Habibi Najafi, Mohammad B; Farhoosh, Reza

    2014-07-15

    The present study reports on the extraction of natural pigment from annatto seeds. Response surface methodology (RSM) was used to investigate the effect of process variables on the ultrasound-assisted extraction (UAE). Four independent variables including temperature (20-80°C), sonication time (2-10 min), duty cycle (0.2-0.8s) and the ratio of seeds to the solvent (5-20%) were studied. According to the results, the optimal UAE condition was obtained with a temperature of 72.7°C, extraction time of 7.25 min, the ratio of seed to solvent of 14% and duty cycle of 0.8s. At these conditions, extraction yield determined as 6.35% and the absorbance value as 0.865%. The experimental values under optimal condition were in good consistent with the predicted values, which suggested UAE is more efficient process as compared to conventional extraction. Copyright © 2014 Elsevier Ltd. All rights reserved.

  5. Ultrasound-assisted removal of Acid Red 17 using nanosized Fe3O4-loaded coffee waste hydrochar.

    Science.gov (United States)

    Khataee, Alireza; Kayan, Berkant; Kalderis, Dimitrios; Karimi, Atefeh; Akay, Sema; Konsolakis, Michalis

    2017-03-01

    The Fe 3 O 4 -loaded coffee waste hydrochar (Fe 3 O 4 -CHC) was synthesized using a simple precipitation method. The as-prepared adsorbent was characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) and Fourier transform infrared spectroscopy (FT-IR). The EDX analysis indicated the presence of Fe in the structure of Fe 3 O 4 -CHC. The specific surface area of hydrochar increased from 17.2 to 34.7m 2 /g after loading of Fe 3 O 4 nanoparticles onto it. The prepared Fe 3 O 4 -CHC was used for removal of Acid Red 17 (AR17) through ultrasound-assisted process. The decolorization efficiency decreased from 100 to 74% with the increase in initial dye concentration and from 100 to 91 and 85% in the presence of NaCl and Na 2 SO 4 , respectively. The synthesized Fe 3 O 4 -CHC exhibited good stability in the repeated adsorption-desorption cycles. The high correlation coefficient (R 2 =0.997) obtained from Langmuir model indicated that physical and monolayer adsorption of dye molecules occurred on the Fe 3 O 4 -CHC surface. Furthermore, the by-products generated through the degradation of AR17 was identified by gas chromatography-mass spectrometry analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Ultrasound-Assisted Emulsification Microextraction in an Online System for Determination of Cadmium in Water and Tea Samples.

    Science.gov (United States)

    Nunes, Leane Santos; Lemos, Valfredo Azevedo

    2018-03-23

    In this work, a method using ultrasound-assisted emulsification microextraction (USAEME) without the use of ligands in an online system for preconcentration and determination of cadmium was developed. The method was based on the preconcentration of cadmium by USAEME, employing trichloroethylene as the extraction solvent, and subsequent retention of the rich phase in a mini-column packed with silica gel. The extracted metal was determined by flame atomic absorption spectrometry. The parameters that affect the extraction of cadmium were optimized using the univariate method. Under optimized conditions, the method presented a limit of detection of 0.17 μg/L, a limit of quantification of 0.57 μg/L, an enrichment factor of 56, and a consumptive index of 0.18 mL/min. The accuracy of the method was tested by analyzing the certified reference material, National Institute of Standards and Technology (NIST) 1573 (tomato leaves). The determination of Cd in water (drinking water, bottled water, river water, and seawater) and tea (black and green tea) samples was also performed using the proposed method. The method is simple, efficient, and eco-friendly because it requires low consumption of an organic solvent.

  7. Continuous-flow ultrasound assisted oxidative desulfurization (UAOD) process: An efficient diesel treatment by injection of the aqueous phase.

    Science.gov (United States)

    Rahimi, Masoud; Shahhosseini, Shahrokh; Movahedirad, Salman

    2017-11-01

    A new continuous-flow ultrasound assisted oxidative desulfurization (UAOD) process was developed in order to decrease energy and aqueous phase consumption. In this process the aqueous phase is injected below the horn tip leading to enhanced mixing of the phases. Diesel fuel as the oil phase with sulfur content of 1550ppmw and an appropriate mixture of hydrogen peroxide and formic acid as the aqueous phase were used. At the first step, the optimized condition for the sulfur removal has been obtained in the batch mode operation. Hence, the effect of more important oxidation parameters; oxidant-to-sulfur molar ratio, acid-to-sulfur molar ratio and sonication time were investigated. Then the optimized conditions were obtained using Response Surface Methodology (RSM) technique. Afterwards, some experiments corresponding to the best batch condition and also with objective of minimizing the residence time and aqueous phase to fuel volume ratio have been conducted in a newly designed double-compartment reactor with injection of the aqueous phase to evaluate the process in a continuous flow operation. In addition, the effect of nozzle diameter has been examined. Significant improvement on the sulfur removal was observed specially in lower sonication time in the case of dispersion method in comparison with the conventional contact between two phases. Ultimately, the flow pattern induced by ultrasonic device, and also injection of the aqueous phase were analyzed quantitatively and qualitatively by capturing the sequential images. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Optimization and physicochemical properties of nutritional protein isolate from pork liver with ultrasound-assisted alkaline extraction.

    Science.gov (United States)

    Zou, Ye; Bian, Huan; Li, Pengpeng; Sun, Zhilan; Sun, Chong; Zhang, Muhan; Geng, Zhiming; Xu, Weimin; Wang, Daoying

    2018-02-01

    The aim of this study was to investigate the optimal conditions of ultrasound-assisted alkaline extraction (UAAE) on pork liver protein isolate (UPLPI) and its physico-chemical properties. Response surface methodology was used to determine the optimal conditions for UAAE, which were at ultrasonic power 265 W, ultrasonic time 42 min, NaOH concentration 0.80%, temperature 50°C, and solvent/raw material ratio 70. The extraction yield and efficiency of UPLPI were significantly improved over the conventional alkaline extraction (PLPI). The results of amino acid composition showed that UAAE could increase serine (36.5 g/kg), arginine (38.1 g/kg), alanine (37.5 g/kg), proline (48.7 g/kg), phenylalanine (55.6 g/kg) and lysine (47.2 g/kg) elution amount. The changes in fourier transform infrared spectra indicated unfolding and destruction of the protein structure in UPLPI. The differential scanning calorimetry analysis presented UPLPI with a slightly lower onset and peak denaturation temperature over PLPI. Surface hydrophobicity increased and the microstructures presented larger and more pores of UPLPI, therefore, it had better in vitro digestibility than PLPI. Therefore, UPLPI might have a potential application prospect in the food field due to its changes on molecular structure as well as on the microstructure of protein by UAAE. © 2017 Japanese Society of Animal Science.

  9. Properties of soluble dietary fiber-polysaccharide from papaya peel obtained through alkaline or ultrasound-assisted alkaline extraction.

    Science.gov (United States)

    Zhang, Weimin; Zeng, Guanglin; Pan, Yonggui; Chen, Wenxue; Huang, Wuyang; Chen, Haiming; Li, Yuansong

    2017-09-15

    Soluble dietary fiber (SDF) from the peel of papaya (Carica papaya Linn.) was recovered through alkaline extraction (alkaline-extracted SDF, a-SDF) and ultrasound-assisted alkaline extraction (ultrasound-treated SDF, u-SDF) processes, and the composition, structure and properties of the extracts were compared. The optimal parameters for obtaining the maximum extraction yield of u-SDF were evaluated through response surface methodology. Under optimal conditions, the maximum yield of u-SDF was 36.99%, and u-SDF had a lower total amino acid content but a higher essential amino acid (16.18%) than a-SDF. A monosaccharide analysis indicated that the primary sugars in a-SDF and u-SDF were neutral sugars and pectic saccharides, respectively. An X-ray diffraction analysis confirmed that u-SDF was less crystalline than a-SDF. Moreover, a thermal analysis indicated that u-SDF exhibited higher thermal stability. In addition, u-SDF exhibited higher water-holding, oil-holding and swelling capacities than a-SDF. These results indicate that papaya peel is a potential inexpensive source of natural dietary fiber and a potential functional food ingredient. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. A Method Based on Ultrasound-assisted Solidification of Floating Drop Microextraction Technique for the Spectrophotometric Determination of Curcumin in Turmeric Powder

    OpenAIRE

    Abbas Afkhami; Massoumeh Pirdadeh-Beiranvand; Tayyebeh Madrakian

    2017-01-01

    A method based on the ultrasound-assisted solidification of floating drop microextraction technique was developed for the spectrophotometric and spectrofluorimetric determination of curcumin in turmeric powder. In this work a small volume of an organic solvent was floated on the surface of an aqueous solution. After sonication the organic solvent is solidified and separated. The effect of extraction parameters such as type and the volume of organic solvent, temperature, salt addition and expo...

  11. Optimization of ultrasound-assisted extraction of pectinase enzyme from guava (Psidium guajava) peel: Enzyme recovery, specific activity, temperature, and storage stability.

    Science.gov (United States)

    Amid, Mehrnoush; Murshid, Fara Syazana; Manap, Mohd Yazid; Islam Sarker, Zaidul

    2016-01-01

    This study aimed to investigate the effects of the ultrasound-assisted extraction conditions on the yield, specific activity, temperature, and storage stability of the pectinase enzyme from guava peel. The ultrasound variables studied were sonication time (10-30 min), ultrasound temperature (30-50 °C), pH (2.0-8.0), and solvent-to-sample ratio (2:1 mL/g to 6:1 mL/g). The main goal was to optimize the ultrasound-assisted extraction conditions to maximize the recovery of pectinase from guava peel with the most desirable enzyme-specific activity and stability. Under the optimum conditions, a high yield (96.2%), good specific activity (18.2 U/mg), temperature stability (88.3%), and storage stability (90.3%) of the extracted enzyme were achieved. The optimal conditions were 20 min sonication time, 40 °C temperature, at pH 5.0, using a 4:1 mL/g solvent-to-sample ratio. The study demonstrated that optimization of ultrasound-assisted process conditions for the enzyme extraction could improve the enzymatic characteristics and yield of the enzyme.

  12. Synthesis of hexagonal wurtzite Cu{sub 2}ZnSnS{sub 4} prisms by an ultrasound-assisted microwave solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Long, Fei, E-mail: long.drf@gmail.com [Key Laboratory of New Processing Technology for Nonferrous Metals and Materials of Ministry of Education, Guilin University of Technology, Guilin 541004 (China); Chi, Shangsen [Key Laboratory of New Processing Technology for Nonferrous Metals and Materials of Ministry of Education, Guilin University of Technology, Guilin 541004 (China); Institute of Advanced Materials and Technology, University of Science and Technology Beijing, Beijing 100083 (China); He, Jinyun; Wang, Jilin; Wu, Xiaoli; Mo, Shuyi; Zou, Zhengguang [Key Laboratory of New Processing Technology for Nonferrous Metals and Materials of Ministry of Education, Guilin University of Technology, Guilin 541004 (China)

    2015-09-15

    Wurtzite Cu{sub 2}ZnSnS{sub 4} (CZTS) hexagonal prisms were synthesized by a simple ultrasound-microwave solvothermal method. The product was characterized by XRD, FESEM, EDS, TEM, Raman and UV–vis spectrometer. The hexagonal prisms were 0.5–2 μm wide and 5–12 μm long. The PVP played an important role in the formation of the CZTS hexagonal prisms. In addition, the ultrasound-assisted microwave process was helpful for synthesis of wurtzite rather than kesterite phase CZTS. A nucleation–dissolution–recrystallization mechanism was also proposed to explain the growth of the CZTS hexagonal prisms. - Graphical abstract: Wurtzite Cu{sub 2}ZnSnS{sub 4} hexagonal prisms were synthesized by ultrasound-microwave solvothermal method. The ultrasound-assisted microwave process and PVP were useful to the growth of CZTS. A nucleation–dissolution–recrystallization growth mechanism was also proposed. - Highlights: • Wurtzite Cu{sub 2}ZnSnS{sub 4} was prepared by ultrasound-assisted microwave solvothermal method. • The wurtzite CZTS hexagonal prisms are demonstrated a band gap of 1.49 eV. • Synergistic effect of ultrasound and microwave is helpful to prepare Wurtzite CZTS. • PVP plays an important role in the formation of the CZTS hexagonal prisms. • Nucleation–dissolution–recrystallization growth mechanism of the CZTS was proposed.

  13. Instant controlled pressure drop technology and ultrasound assisted extraction for sequential extraction of essential oil and antioxidants.

    Science.gov (United States)

    Allaf, Tamara; Tomao, Valérie; Ruiz, Karine; Chemat, Farid

    2013-01-01

    The instant controlled pressure drop (DIC) technology enabled both the extraction of essential oil and the expansion of the matrix itself which improved solvent extraction. The sequential use of DIC and Ultrasound Assisted Extraction (UAE) triggered complementary actions materialized by supplementary effects. We visualized these combination impacts by comparing them to standard techniques: Hydrodistillation (HD) and Solvent Extraction (SE). First, the extraction of orange peel Essential Oils (EO) was achieved by HD during 4h and DIC process (after optimization) during 2 min; EO yields was 1.97 mg/g dry material (dm) with HD compared to 16.57 mg/g d m with DIC. Second, the solid residue was recovered to extract antioxidant compounds (naringin and hesperidin) by SE and UAE. Scanning electron microscope showed that after HD the recovered solid shriveled as opposite to DIC treatment which expanded the product structure. HPLC analyses showed that the best kinetics and yields of naringin and hesperidin extraction was when DIC and UAE are combined. Indeed, after 1h of extraction, DIC treated orange peels with UAE were 0.825 ± 1.6 × 10(-2)g/g of dry material (dm) for hesperidin and 6.45 × 10(-2) ± 2.3 × 10(-4)g/g d m for naringin compared to 0.64 ± 2.7 × 10(-2)g/g of dry material (dm) and 5.7 × 10(-2) ± 1.6 × 10(-3)g/g d m, respectively with SE. By combining DIC to UAE, it was possible to enhance kinetics and yields of antioxidant extraction. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. Ultrasound-assisted non-viral gene transfer of AQP1 to the irradiated minipig parotid gland restores fluid secretion

    Science.gov (United States)

    Wang, Z; Zourelias, L; Wu, C; Edwards, PC; Trombetta, M; Passineau, MJ

    2015-01-01

    Rationale Xerostomia is a common side effect of ionizing radiation used to treat head and neck cancer. A groundbreaking Phase I human clinical trial utilizing Adenoviral gene transfer of Aquaporin-1 (AQP1) to a single salivary gland of individuals suffering from radiation-induced xerostomia has recently been reported. Unfortunately, the limitations of the Adenoviral vector system utilized in this pioneering trial preclude its advancement to a Phase II trial and we have thus undertaken to evaluate the therapeutic potential of ultrasound-assisted non-viral gene transfer (UAGT) as an alternative means of delivering AQP1 gene therapy to the salivary gland by comparing head-to-head with the canonical Adenoviral vector in a swine model. Findings Swine irradiated unilaterally with a 10Gy electron beam targeted at the parotid gland suffered from significant, sustained hyposalivation that was bilateral, despite irradiation being confined to the targeted gland. Unilateral AQP1 gene therapy with UAGT resulted in bilateral restoration of stimulated salivary flow at 48 hours and one week post-treatment (1.62+/−0.48ml, 1.87+/−0.45ml) to pre-injury levels (1.34+/−0.14ml) in a manner comparable to Adenoviral delivery (2.32+/−0.6ml, 1.33+/−0.97ml). Conclusions UAGT can replace the Adenoviral vector as a means of delivering AQP1 gene therapy in the irradiated swine model and is a candidate for advancement to a Phase I human clinical trial. PMID:25871828

  15. Ultrasound-assisted synthesis of poly(MMA-co-BA)/ZnO nanocomposites with enhanced physical properties.

    Science.gov (United States)

    Poddar, Maneesh Kumar; Sharma, Sachin; Pattipaka, Srinivas; Pamu, D; Moholkar, Vijayanand S

    2017-11-01

    The present study reports synthesis and characterization of poly(MMA-co-BA)/ZnO nanocomposites using ultrasound-assisted in-situ emulsion polymerization. Methyl methacrylate (MMA) was copolymerized with butyl acrylate (BA), for enhanced ductility of copolymer matrix, in presence of nanoscale ZnO particles. Ultrasound generated strong micro-turbulence in reaction mixture, which resulted in higher encapsulation and uniform dispersion of ZnO (in native form - without surface modification) in polymer matrix, as compared to mechanical stirring. The nanocomposites were characterized for physical properties and structural morphology using standard techniques such as XRD, FTIR, particle size analysis, UV-Visible spectroscopy, electrical conductivity, TGA, DSC, FE-SEM and TEM. Copolymerization of MMA and BA (in presence of ZnO) followed second order kinetics. Thermal stability (T 10% =324.9°C) and glass transition temperature (T g =67.8°C) of poly(MMA-co-BA)/ZnO nanocomposites showed significant enhancement (35.1°C for 1wt% ZnO and 15.7°C for 4wt% ZnO, respectively), as compared to pristine poly(MMA-co-BA). poly(MMA-co-BA)/ZnO (5wt%) nanocomposites possessed the highest electrical conductivity of 0.192μS/cm and peak UV absorptivity of 0.55 at 372nm. Solution rheological study of nanocomposites revealed enhancement in viscosity with increasing ZnO loading. Maximum viscosity of 0.01Pa-s was obtained for 5wt% ZnO loading. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Assessment and optimization of an ultrasound-assisted washing process using organic solvents for polychlorinated biphenyl-contaminated soil.

    Science.gov (United States)

    Bezama, Alberto; Flores, Alejandra; Araneda, Alberto; Barra, Ricardo; Pereira, Eduardo; Hernández, Víctor; Moya, Heriberto; Konrad, Odorico; Quiroz, Roberto

    2013-10-01

    The goal of this work was to evaluate a washing process that uses organic solutions for polychlorinated biphenyl (PCB)-contaminated soil, and includes an ultrasound pre-treatment step to reduce operational times and organic solvent losses. In a preliminary trial, the suitability of 10 washing solutions of different polarities were tested, from which three n-hexane-based solutions were selected for further evaluation. A second set of experiments was designed using a three-level Taguchi L27 orthogonal array to model the desorption processes of seven different PCB congeners in terms of the variability of their PCB concentration levels, polarity of the washing solution, sonication time, the ratio washing solution/soil, number of extraction steps and total washing time. Linear models were developed for the desorption processes of all congeners. These models provide a good fit with the results obtained. Moreover, statistically significant outcomes were achieved from the analysis of variance tests carried out. It was determined that sonication time and ratio of washing solution/soil were the most influential process parameters. For this reason they were studied in a third set of experiments, constructed as a full factorial design. The process was eventually optimized, achieving desorption rates of more than 90% for all congeners, thus obtaining concentrations lower than 5 ppb in all cases. The use of an ultrasound-assisted soil washing process for PCB-contaminated soils that uses organic solvents seems therefore to be a viable option, especially with the incorporation of an extra step in the sonication process relating to temperature control, which is intended to prevent the loss of the lighter congeners.

  17. Employing Response Surface Methodology for the Optimization of Ultrasound Assisted Extraction of Lutein and β-Carotene from Spinach

    Directory of Open Access Journals (Sweden)

    Ammar Altemimi

    2015-04-01

    Full Text Available The extraction of lutein and β-carotene from spinach (Spinacia oleracea L. leaves is important to the dietary supplement industry. A Box-Behnken design and response surface methodology (RSM were used to investigate the effect of process variables on the ultrasound-assisted extraction (UAE of lutein and β-carotene from spinach. Three independent variables, extraction temperature (°C, extraction power (% and extraction time (min were studied. Thin-layer chromatography (TLC followed by UV visualization and densitometry was used as a simple and rapid method for both identification and quantification of lutein and β-carotene during UAE. Methanol extracts of leaves from spinach and authentic standards of lutein and β-carotene were separated by normal-phase TLC with ethyl acetate-acetone (5:4 (v/v as the mobile phase. In this study, the combination of TLC, densitometry, and Box–Behnken with RSM methods were effective for the quantitative analysis of lutein and β-carotene from spinach extracts. The resulting quadratic polynomial models for optimizing lutein and β-carotene from spinach had high coefficients of determination of 0.96 and 0.94, respectively. The optimal UAE settings for output of lutein and β-carotene simultaneously from spinach extracts were an extraction temperature of 40 °C, extraction power of 40% (28 W/cm3 and extraction time of 16 min. The identity and purity of each TLC spot was measured using time-of-flight mass spectrometry. Therefore, UAE assisted extraction of carotenes from spinach can provide a source of lutein and β-carotene for the dietary supplement industry.

  18. Optimized Ultrasound-Assisted Oxidative Desulfurization Process of Simulated Fuels over Activated Carbon-Supported Phosphotungstic Acid

    Directory of Open Access Journals (Sweden)

    Peniel Jean Gildo

    2018-01-01

    Full Text Available Recent technological advancements respond to the call to minimize/eliminate emissions to the atmosphere. However, on the average, fuel oils which is one of the major raw materials, is found to increase in sulfur concentration due to a phenomenon called thermal maturation. As such, a deeper desulfurization process is needed to obtain low/ultra-low sulfur fuel oils. In the present study, the ultrasound assisted oxidative desulfurization (UAOD processes using the H2O2 and HPW-AC oxidizing system applied to simulated fuel (~2800 ppm sulfur in the form of dibenzothiophene, benzothiophene, and thiophene dissolved in toluene, were optimized. After the pre-saturation of the HPW-AC with the simulated fuel, H2O2 was added just before the reaction was commenced under ultrasonic irradiation. After the application of both 2k-factorial design of experiment for screening and Face-Centered Design of Experiment for optimization, it was found that 25.52 wt% of H2O2 concentration, 983.9 mg of catalyst dose, 9.52 mL aqueous phase per 10 mL of the organic phase and 76.36 minutes of ultrasonication time would render 94.74% oxidation of the sulfur compounds in the simulated fuel. After the application of the optimized parameters to kerosene and employing a 4-cycle extraction using acetonitrile, 99% of the original sulfur content were removed from the kerosene using the UAOD optimized parameters. The desulfurization process resulted in a low-sulfur kerosene which retained its basic fuel properties such as density, viscosity and calorific value.

  19. Ultrasound assisted green synthesis of cerium oxide nanoparticles using Prosopis juliflora leaf extract and their structural, optical and antibacterial properties

    Directory of Open Access Journals (Sweden)

    Arunachalam Thirunavukkarasu

    2018-03-01

    Full Text Available Cerium oxide nanoparticles (CONPs were prepared using ultrasound assisted leaf extract of Prosopis juliflora acting as a reducing as well as stabilizing agent. The synthesized CONPs were characterized by ultraviolet-visible absorption spectroscopy (UV-Vis, particle size analyzer (PSA, Fourier transform infrared spectroscopy (FT-IR, Raman spectroscopy, X-ray diffraction (XRD, X-ray photoelectron spectroscopy (XPS and high-resolution transmission electron microscopy (HRTEM. From the UV-Vis analysis, the optical band gap of the prepared CONPs (Eg = 3.62 eV was slightly increased as compared to the bulk ceria (Eg = 3.19 eV. The phytochemicals in the extract reduced the particle size to 3.7 nm ± 0.3 nm, as it is evident from the PSA. FT-IR results confirmed the Ce-O stretching bands by showing the peaks at 452 cm-1. The Raman spectrumshowed a characteristic peak shift for CONPs at 461.2 cm-1. XRD analysis revealed the cubic fluorite structure of the synthesizednanoparticles with the lattice constant, a of 5.415 Å and unit cell volume, V of 158.813 Å3. XPS signals were used to determine the concentration of Ce3+ and Ce4+ in the prepared CONPs and it was found that major amount of cerium exist in the Ce4+ state. HRTEM images showed spherical shaped particles with an average size of 15 nm. Furthermore, the antibacterial activity of the prepared CONPs was evaluated and their efficacies were compared with the conventional antibiotics using disc diffusion assay against a set of Gram positive (G+ bacteria (Staphylococcus aureus, Streptococcus pneumonia and Gram negative (G- bacteria (Pseudomonas aeruginosa, Proteus vulgaris. The results suggested that CONPs showed antibacterial activity with significant variations due to the differences in the membrane structure and cell wall composition among the two groups tested.

  20. Production of graphene quantum dots by ultrasound-assisted exfoliation in supercritical CO2/H2O medium.

    Science.gov (United States)

    Gao, Hanyang; Xue, Chen; Hu, Guoxin; Zhu, Kunxu

    2017-07-01

    In this research, three kinds of graphene quantum dots (GQDs)-pristine graphene quantum dots (PGQDs), expanded graphene quantum dots (EGQDs) and graphene oxide quantum dots (GOQDs)-were produced from natural graphite, expanded graphite, and oxide graphite respectively in an ultrasound-assisted supercritical CO 2 (scCO 2 )/H 2 O system. The effects of aqueous solution content ratio, system pressure, and ultrasonic power on the yields of different kinds of GQDs were investigated. According to these experiment results, the combination of the intense knocking force generated from high-pressure acoustic cavitation in a scCO 2 /H 2 O system and the superior penetration ability of scCO 2 was considered to be the key to the successful exfoliation of such tiny pieces from bulk graphite. An interesting result was found that, contrary to common experience, the yield of PGQDs from natural graphite was much higher than that of GOQDs from graphite oxide. Based on the experimental analysis, the larger interlayer resistance of natural graphite, which hindered the insertion of scCO 2 molecules, and the hydrophobic property of natural graphite surface, which made the planar more susceptible to the attack of ultrasonic collapsing bubbles, were deduced to be the two main reasons for this result. The differences in characteristics among the three kinds of GQDs were also studied and compared in this research. In our opinion, this low-cost and time-saving method may provide an alternative green route for the production of various kinds of GQDs, especially PGQDs. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Gas chromatography-flame ionization determination of benzaldehyde in non-steroidal anti-inflammatory drug injectable formulations using new ultrasound-assisted dispersive liquid-liquid micro extraction

    International Nuclear Information System (INIS)

    Mashayekhi, H.A.; Pourshamsian, K.

    2012-01-01

    Summary: In this study, simple and efficient ultrasound-assisted dispersive liquid-liquid micro extraction combined with gas chromatography (GC) was developed for the preconcentration and determination of benzaldehyde in injectable formulations of the non-steroidal anti-inflammatory drugs, diclofenac, Vitamin B-complex and Voltaren injection solutions. Fourteen microliters of toluene was injected slowly into 10 mL home-designed centrifuge glass vial containing an aqueous sample without salt addition that was located inside the ultrasonic water bath. The formed emulsion was centrifuged and 2 macro L of separated toluene was injected into a gas chromatographic system equipped with a flame ionization detector (GC-FID) for analysis. Several factors influencing the extraction efficiency as the nature and volume of organic solvent, extraction temperature, ionic strength and centrifugation time were investigated and optimized. Using optimum extraction conditions a detection limit of 0.3 macro g L/sup -1/ and a good linearity in a calibration range of 2.0-1000 macro g L/sup -1/ were achieved for analyte. This proposed method was successfully applied to the analysis of benzaldehyde in three injection formulations and relative standard deviation (RSD) of analysis (n=3), before spiking with standard benzaldehyde were 3.3, 2.0 and 1.3% for Na-diclofenac, vitamin B-complex and voltaren, respectively and after spiking of standard benzaldehyde (0.3 mg L/sup -1/), the RSD were 6.5, 3.6 and 2.8% for Na-diclofenac, vitamin B-complex and voltaren, respectively. (author)

  2. Determination of organophosphorus pesticides and metabolites in cereal-based baby foods and wheat flour by means of ultrasound-assisted extraction and hollow-fiber liquid-phase microextraction prior to gas chromatography with nitrogen phosphorus detection.

    Science.gov (United States)

    González-Curbelo, Miguel Ángel; Hernández-Borges, Javier; Borges-Miquel, Teresa María; Rodríguez-Delgado, Miguel Ángel

    2013-10-25

    A new method based on hollow-fiber liquid-phase microextraction (HF-LPME) has been developed for the determination of a group of organophosphorus pesticides, including some of their metabolites, in two commercial cereal-based baby foods and one wheat flour prior to gas chromatography-nitrogen phosphorus detection. Samples were first extracted by ultrasound-assisted extraction with acetonitrile (ACN) containing 1.25% (v/v) of formic acid. After evaporation and reconstitution in Milli-Q water, the HF-LPME procedure, using 1-octanol as extraction solvent, was applied followed by a desorption step in ACN, which clearly improved the performance of the technique. The effects of sample pH, ionic strength, stirring rate, extraction temperature and time as well as the desorption procedure were investigated. Under the optimum conditions that involved the extraction of the analytes from 10 mL of the water reconstituted extract at pH 7.0 containing 5% (w/v) of NaCl for 45 min at 960 rpm, the method was validated in terms of linearity, precision and accuracy. The limits of detection (LODs) were between 0.29 and 3.20 μg/kg. The extraction of Milli-Q water, as an example of the applicability of the procedure to aqueous samples, allowed achieving LODs in the range 0.01-0.04 μg/L. Such values, together with the ones achieved for the rest of the samples, are below or equal to the maximum residue limits specified by the European Union. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Ligandless, ion pair-based and ultrasound assisted emulsification solidified floating organic drop microextraction for simultaneous preconcentration of ultra-trace amounts of gold and thallium and determination by GFAAS.

    Science.gov (United States)

    Fazelirad, Hamid; Taher, Mohammad Ali

    2013-01-15

    In the present work, a new, simple and efficient method for simultaneous preconcentration of ultra-trace amounts of gold and thallium is developed using an ion pair based-ultrasound assisted emulsification-solidified floating organic drop microextraction procedure before graphite furnace atomic absorption spectrometry determination. This methodology was used to preconcentrate the ion pairs formed between AuCl(4)(-) and TlCl(4)(-) and [C(23)H(42)]N(+) in a microliter-range volume of 1-undecanol. Several factors affecting the microextraction efficiency, such as HCl volume, type and volume of extraction solvent, sonication time, sample volume, temperature, ionic strength and [C(23)H(42)]NCl volume were investigated and optimized. Under the optimized conditions, the enrichment factor of 441 and 443 and calibration graphs of 2.2-89 and 22.2-667 ng L(-1) for gold and thallium were obtained, respectively. The intra- and inter-day precision of ± 4.4 and ± 4.9% for Au and ± 4.8 and ± 5.4% for Tl were obtained. The detection limit was 0.66 ng L(-1) for Au and 4.67 ng L(-1) for Tl. The results show that the liquid-liquid pretreatment using ion pair forming, is sensitive, rapid, simple and safe method for the simultaneous preconcentration of gold and thallium. The method was successfully applied for determination of gold and thallium in natural water and hair samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. Ultrasound Assisted Optical Imaging

    National Research Council Canada - National Science Library

    Chen, Nan

    2002-01-01

    .... A novel image reconstruction algorithm has been proposed and implemented. It reconstructs lower orders moments of targets from limited information from a diffusive system, and is more robust than conventional iterative algorithms...

  5. Ultrasound assisted enhancement in natural dye extraction from beetroot for industrial applications and natural dyeing of leather.

    Science.gov (United States)

    Sivakumar, Venkatasubramanian; Anna, J Lakshmi; Vijayeeswarri, J; Swaminathan, G

    2009-08-01

    There is a growing demand for eco-friendly/non-toxic colorants, specifically for health sensitive applications such as coloration of food and dyeing of child textile/leather garments. Recently, dyes derived from natural sources for these applications have emerged as an important alternative to potentially harmful synthetic dyes and pose need for suitable effective extraction methodologies. The present paper focus on the influence of process parameters for ultrasound assisted leaching of coloring matter from plant materials. In the present work, extraction of natural dye from beetroot using ultrasound has been studied and compared with static/magnetic stirring as a control process at 45 degrees C. The influence of process parameters on the extraction efficiency such as ultrasonic output power, time, pulse mode, effect of solvent system and amount of beetroot has been studied. The use of ultrasound is found to have significant improvement in the extraction efficiency of colorant obtained from beetroot. Based on the experiments it has been found that a mixture of 1:1 ethanol-water with 80W ultrasonic power for 3h contact time provided better yield and extraction efficiency. Pulse mode operation may be useful in reducing electrical energy consumption in the extraction process. The effect of the amount of beetroot used in relation to extraction efficiency has also been studied. Two-stage extraction has been studied and found to be beneficial for improving the yield for higher amounts of beetroot. Significant 8% enhancement in % yield of colorant has been achieved with ultrasound, 80W as compared to MS process both using 1:1 ethanol-water. The coloring ability of extracted beet dye has been tested on substrates such as leather and paper and found to be suitable for dyeing. Ultrasound is also found to be beneficial in natural dyeing of leather with improved rate of exhaustion. Both the dyed substrates have better color values for ultrasonic beet extract as inferred from

  6. Learning Ionic

    CERN Document Server

    Ravulavaru, Arvind

    2015-01-01

    This book is intended for those who want to learn how to build hybrid mobile applications using Ionic. It is also ideal for people who want to explore theming for Ionic apps. Prior knowledge of AngularJS is essential to complete this book successfully.

  7. Ultrasound assisted synthesis of PANI/ZnMoO4 nanocomposite for simultaneous improvement in anticorrosion, physico-chemical properties and its application in gas sensing.

    Science.gov (United States)

    Bhanvase, B A; Darda, N S; Veerkar, N C; Shende, A S; Satpute, S R; Sonawane, S H

    2015-05-01

    Ultrasound assisted in-situ semi-batch emulsion polymerization has been used for the preparation of polyaniline (PANI) and PANI/ZnMoO4 nanocomposite with different loading of ZnMoO4 (ZM) nanoparticles. ZM nanoparticles were functionalized using Myristic acid (MA) for better compatibility with PANI. The cavitational effects induced due to ultrasonic irradiations have been shown significant enhancement in the dispersion of functionalized ZM nanoparticles into the PANI during ultrasound assisted in-situ emulsion polymerization process. TEM images of PANI/ZM nanocomposite particles give the direct evidence of fine dispersion and encapsulation of MA treated ZM nanoparticles in PANI matrix. The presence of ZM nanoparticles in PANI/ZM nanocomposite shows significant improvement in the mechanical (cross-cut adhesion), thermal, anticorrosion and sensing properties of PANI/ZM nanocomposite/alkyd coatings over PANI/alkyd and neat alkyd resin coating. Fine and uniform dispersion of ZM nanoparticles in PANI matrix using this novel synthesis method (PANI (p-type)/ZM (n-type) hetero-junction) improves LPG sensing ability and minimizes response time to sense LPG significantly compared with neat PANI. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Optimization of ultrasound-assisted extraction to obtain mycosterols from Agaricus bisporus L. by response surface methodology and comparison with conventional Soxhlet extraction.

    Science.gov (United States)

    Heleno, Sandrina A; Diz, Patrícia; Prieto, M A; Barros, Lillian; Rodrigues, Alírio; Barreiro, Maria Filomena; Ferreira, Isabel C F R

    2016-04-15

    Ergosterol, a molecule with high commercial value, is the most abundant mycosterol in Agaricus bisporus L. To replace common conventional extraction techniques (e.g. Soxhlet), the present study reports the optimal ultrasound-assisted extraction conditions for ergosterol. After preliminary tests, the results showed that solvents, time and ultrasound power altered the extraction efficiency. Using response surface methodology, models were developed to investigate the favourable experimental conditions that maximize the extraction efficiency. All statistical criteria demonstrated the validity of the proposed models. Overall, ultrasound-assisted extraction with ethanol at 375 W during 15 min proved to be as efficient as the Soxhlet extraction, yielding 671.5 ± 0.5mg ergosterol/100 g dw. However, with n-hexane extracts with higher purity (mg ergosterol/g extract) were obtained. Finally, it was proposed for the removal of the saponification step, which simplifies the extraction process and makes it more feasible for its industrial transference. Copyright © 2015 Elsevier Ltd. All rights reserved.

  9. Simple method for the determination of personal care product ingredients in lettuce by ultrasound-assisted extraction combined with solid-phase microextraction followed by GC-MS.

    Science.gov (United States)

    Cabrera-Peralta, Jerónimo; Peña-Alvarez, Araceli

    2018-02-19

    A simple method for the simultaneous determination of personal care product ingredients: galaxolide, tonalide, oxybenzone, 4-methylbenzyliden camphor, padimate-o, 2-ethylhexyl methoxycinnamate, octocrylene, triclosan, and methyl triclosan in lettuce by ultrasound-assisted extraction combined with solid-phase microextraction followed by gas chromatography with mass spectrometry was developed. Lettuce was directly extracted by ultrasound-assisted extraction with methanol, this extract was combined with water, extracted by solid-phase microextraction in immersion mode, and analyzed by gas chromatography with mass spectrometry. Good linear relationships (25-250 ng/g, R 2  > 0.9702) and low detection limits (1.0-25 ng/g) were obtained for analytes along with acceptable precision for almost all analytes (RSDs < 20%). The validated method was applied for the determination of personal care product ingredients in commercial lettuce and lettuces grown in soil and irrigated with the analytes, identifying the target analytes in leaves and roots of the latter. This procedure is a miniaturized and environmentally friendly proposal which can be a useful tool for quality analysis in lettuce. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Metamaterial Behavior of Polymer Nanocomposites Based on Polypropylene/Multi-Walled Carbon Nanotubes Fabricated by Means of Ultrasound-Assisted Extrusion

    Science.gov (United States)

    Pérez-Medina, Juan C.; Waldo-Mendoza, Miguel A.; Cruz-Delgado, Víctor J.; Quiñones-Jurado, Zoe V.; González-Morones, Pablo; Ziolo, Ronald F.; Martínez-Colunga, Juan G.; Soriano-Corral, Florentino; Avila-Orta, Carlos A.

    2016-01-01

    Metamaterial behavior of polymer nanocomposites (NCs) based on isotactic polypropylene (iPP) and multi-walled carbon nanotubes (MWCNTs) was investigated based on the observation of a negative dielectric constant (ε′). It is demonstrated that as the dielectric constant switches from negative to positive, the plasma frequency (ωp) depends strongly on the ultrasound-assisted fabrication method, as well as on the melt flow index of the iPP. NCs were fabricated using ultrasound-assisted extrusion methods with 10 wt % loadings of MWCNTs in iPPs with different melt flow indices (MFI). AC electrical conductivity (σ(AC)) as a function of frequency was determined to complement the electrical classification of the NCs, which were previously designated as insulating (I), static-dissipative (SD), and conductive (C) materials. It was found that the SD and C materials can also be classified as metamaterials (M). This type of behavior emerges from the negative dielectric constant observed at low frequencies although, at certain frequencies, the dielectric constant becomes positive. Our method of fabrication allows for the preparation of metamaterials with tunable ωp. iPP pure samples show only positive dielectric constants. Electrical conductivity increases in all cases with the addition of MWCNTs with the largest increases observed for samples with the highest MFI. A relationship between MFI and the fabrication method, with respect to electrical properties, is reported. PMID:28774042

  11. Metamaterial Behavior of Polymer Nanocomposites Based on Polypropylene/Multi-Walled Carbon Nanotubes Fabricated by Means of Ultrasound-Assisted Extrusion

    Directory of Open Access Journals (Sweden)

    Juan C. Pérez-Medina

    2016-11-01

    Full Text Available Metamaterial behavior of polymer nanocomposites (NCs based on isotactic polypropylene (iPP and multi-walled carbon nanotubes (MWCNTs was investigated based on the observation of a negative dielectric constant (ε′. It is demonstrated that as the dielectric constant switches from negative to positive, the plasma frequency (ωp depends strongly on the ultrasound-assisted fabrication method, as well as on the melt flow index of the iPP. NCs were fabricated using ultrasound-assisted extrusion methods with 10 wt % loadings of MWCNTs in iPPs with different melt flow indices (MFI. AC electrical conductivity (σ(AC as a function of frequency was determined to complement the electrical classification of the NCs, which were previously designated as insulating (I, static-dissipative (SD, and conductive (C materials. It was found that the SD and C materials can also be classified as metamaterials (M. This type of behavior emerges from the negative dielectric constant observed at low frequencies although, at certain frequencies, the dielectric constant becomes positive. Our method of fabrication allows for the preparation of metamaterials with tunable ωp. iPP pure samples show only positive dielectric constants. Electrical conductivity increases in all cases with the addition of MWCNTs with the largest increases observed for samples with the highest MFI. A relationship between MFI and the fabrication method, with respect to electrical properties, is reported.

  12. Thioimidazolium Ionic Liquids as Tunable Alkylating Agents.

    Science.gov (United States)

    Guterman, Ryan; Miao, Han; Antonietti, Markus

    2018-01-19

    Alkylating ionic liquids based on the thioimidazolium structure combine the conventional properties of ionic liquids, including low melting point and nonvolatility, with the alkylating function. Alkyl transfer occurs exclusively from the S-alkyl position, thus allowing for easy derivatization of the structure without compromising specificity. We apply this feature to tune the electrophilicty of the cation to profoundly affect the reactivity of these alkylating ionic liquids, with a caffeine-derived compound possessing the highest reactivity. Anion choice was found to affect reaction rates, with iodide anions assisting in the alkylation reaction through a "shuttling" process. The ability to tune the properties of the alkylating agent using the toolbox of ionic liquid chemistry highlights the modular nature of these compounds as a platform for alkylating agent design and integration in to future systems.

  13. Optimization of ultrasound-assisted extraction of crude oil from winter melon (Benincasa hispida) seed using response surface methodology and evaluation of its antioxidant activity, total phenolic content and fatty acid composition.

    Science.gov (United States)

    Bimakr, Mandana; Rahman, Russly Abdul; Taip, Farah Saleena; Adzahan, Noranizan Mohd; Sarker, Md Zaidul Islam; Ganjloo, Ali

    2012-10-08

    In the present study, ultrasound-assisted extraction of crude oil from winter melon seeds was investigated through response surface methodology (RSM). Process variables were power level (25-75%), temperature (45-55 °C) and sonication time (20-40 min). It was found that all process variables have significant (p oil obtained by the Soxhlet method. It was found that crude extract yield (CEY) of ultrasound-assisted extraction was lower than that of the Soxhlet method, whereas antioxidant activity and total phenolic content of the extract obtained by ultrasound-assisted extraction were clearly higher than those of the Soxhlet extract. Furthermore, both extracts were rich in unsaturated fatty acids. The major fatty acids of the both extracts were linoleic acid and oleic acid.

  14. Ionic Liquid Fuels for Chemical Propulsion

    Science.gov (United States)

    2016-10-31

    supplied the drawings, specifications, or other data does not license the holder or any other person or corporation; or convey any rights or...PROPELLANTS 10/2012- 9/2015 BERMAN USAF-AFRL Brand NASA Providing advanced monopropellant based on AFOSR material for spacecraft...demonstration Spacecraft Monopropulsion L,I O Pd IONIC LIQUID- BASED PROPELLANTS 6/2012- 12/2014 BERMAN USAF-AFRL Brand Aerojet Providing advanced

  15. Microwave-assisted extraction of coumarin and related compounds from Melilotus officinalis (L.) Pallas as an alternative to Soxhlet and ultrasound-assisted extraction.

    Science.gov (United States)

    Martino, Emanuela; Ramaiola, Ilaria; Urbano, Mariangela; Bracco, Francesco; Collina, Simona

    2006-09-01

    Soxhlet extraction, ultrasound-assisted extraction (USAE) and microwaves-assisted extraction (MAE) in closed system have been investigated to determine the content of coumarin, o-coumaric and melilotic acids in flowering tops of Melilotus officinalis. The extracts were analyzed with an appropriate HPLC procedure. The reproducibility of extraction and of chromatographic analysis was proved. Taking into account the extraction yield, the cost and the time, we studied the effects of extraction variables on the yield of the above-mentioned compounds. Better results were obtained with MAE (50% v/v aqueous ethanol, two heating cycles of 5 min, 50 degrees C). On the basis of the ratio extraction yield/extraction time, we therefore propose MAE as the most efficient method.

  16. Comparison of soxhlet, ultrasound-assisted and pressurized liquid extraction of terpenes, fatty acids and Vitamin E from Piper gaudichaudianum Kunth.

    Science.gov (United States)

    Péres, Valéria Flores; Saffi, Jenifer; Melecchi, Maria Inês S; Abad, Fernanda C; de Assis Jacques, Rosângela; Martinez, Migdalia M; Oliveira, Eniz Conceição; Caramão, Elina B

    2006-02-10

    This paper describes a comparative study of extraction methods of terpenes (terpenic alcohols and phytosterols), fatty acids and Vitamin E from leaves of Piper gaudichaudianum Kunth. The analysis of extracts was done by gas chromatography with mass spectrometric detection. The identification and quantification was made by co-injections of the extract with certified standards. The use of pressurized liquid extraction (PLE; Dionex trade name: ASE, for accelerated solvent extraction) decrease significantly the total time of extraction, the amount of solvent and the manipulation of sample and solvents in comparison with soxhlet (SE) and ultrasound-assisted (USE). In addition, PLE was more effective for the extractions of terpenes (terpenic alcohols and phytosterols), fatty acids and Vitamin E.

  17. Bio-guided optimization of the ultrasound-assisted extraction of compounds from Annona glabra L. leaves using the etiolated wheat coleoptile bioassay.

    Science.gov (United States)

    Matsumoto, Sadao; Varela, Rosa M; Palma, Miguel; Molinillo, José M G; Lima, Inês S; Barroso, Carmelo G; Macías, Francisco A

    2014-07-01

    A bio-guided optimization of the extraction of bioactive components from Annona glabra leaves has been developed using the etiolated wheat coleoptile bioassay as the control method. The optimization of an ultrasound-assisted extraction of bioactive compounds using allelopathy results as target values has been carried out for the first time. A two-level fractional factorial experimental design was applied to optimize the ultrasound-assisted extraction. The solvent was the extraction variable that had the most marked effect on the resulting bioactivity of the extracts in the etiolated wheat coleoptile bioassay. Extraction time, extraction temperature and the size of the ultrasonic probe also influenced the bioactivity of the extracts. A larger scale extraction was carried out in the next step in the allelopathic study, i.e., the isolation of compounds from the bioactive extract and chemical characterization by spectroscopic techniques, including NMR. Eight compounds were isolated and identified from the active extracts, namely two steroids (β-sistosterol and stigmasterol), five diterpenes with the kaurane skeleton (ent-kaur-16-en-19-oic acid, ent-19-methoxy-19-oxokauran-17-oic acid, annoglabasin B, ent-17-hydroxykaur-15-en-19-oic acid and ent-15β,16β-epoxy-17-hydroxy-kauran-19-oic acid) and the acetogenin asimicin. The most active compound was annoglabasin B, which showed inhibition with values of -95% at 10(-3) M, -87% at 5×10(-4) M and greater than -70% at 10(-4) M in the etiolated wheat coleoptile bioassay. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Optimization of ultrasound-assisted aqueous two-phase system extraction of polyphenolic compounds from Aronia melanocarpa pomace by response surface methodology.

    Science.gov (United States)

    Xu, Yan-Yang; Qiu, Yang; Ren, Hui; Ju, Dong-Hu; Jia, Hong-Lei

    2017-03-16

    Aronia melanocarpa berries are abundant in polyphenolic compounds. After juice production, the pomace of pressed berries still contains a substantial amount of polyphenolic compounds. For efficient utilization of A. melanocarpa berries and the enhancement of polyphenolic compound yields in Aronia melanocarpa pomace (AMP), total phenolics (TP) and total flavonoids (TF) from AMP were extracted, using ultrasound-assisted aqueous two-phase system (UAE-ATPS) extraction method. First, the influences of ammonium sulfate concentration, ethanol-water ratio, ultrasonic time, and ultrasonic power on TP and TF yields were investigated. On this basis, process variables such as ammonium sulfate concentration (0.30-0.35 g mL -1 ), ethanol-water ratio (0.6-0.8), ultrasonic time (40-60 min), and ultrasonic power (175-225 W) were further optimized by implementing Box-Benhnken design with response surface methodology. The experimental results showed that optimal extraction conditions of TP from AMP were as follows: ammonium sulfate concentration of 0.324 g mL -1 , ethanol-water ratio of 0.69, ultrasonic time of 52 min, and ultrasonic power of 200 W. Meanwhile, ammonium sulfate concentration of 0.320 g mL -1 , ethanol-water ratio of 0.71, ultrasonic time of 50 min, and ultrasonic power of 200 W were determined as optimum extraction conditions of TF in AMP. Experimental validation was performed, where TP and TF yields reached 68.15 ± 1.04 and 11.67 ± 0.63 mg g -1 , respectively. Close agreement was found between experimental and predicted values. Overall, the present results demonstrated that ultrasound-assisted aqueous two-phase system extraction method was successfully used to extract total phenolics and flavonoids in A. melanocarpa pomace.

  19. Fe(II)–Al(III) layered double hydroxides prepared by ultrasound-assisted co-precipitation method for the reduction of bromate

    International Nuclear Information System (INIS)

    Zhong, Yu; Yang, Qi; Luo, Kun; Wu, Xiuqiong; Li, Xiaoming; Liu, Yang; Tang, Wangwang; Zeng, Guangming; Peng, Bo

    2013-01-01

    Highlights: ► Fe(II)–Al(III) LDHs were synthesized by ultrasound-assisted co-precipitation method. ► The Fe–Al (30 min) exhibited highly reduction reactivity on bromate. ► Pseudo-first-order model described the experimental data well. ► The mechanisms of bromate removal were proposed. -- Abstract: Bromate is recognized as an oxyhalide disinfection byproduct in drinking water. In this paper, Fe(II)–Al(III) layered double hydroxides (Fe–Al LDHs) prepared by the ultrasound-assisted co-precipitation method were used for the reduction of bromate in solution. The Fe–Al LDHs particles were characterized by X-ray diffractometer, scanning electron microscopy and thermogravimetry–differential scanning calorimetry. It was found that ultrasound irradiation assistance promoted the formation of the hydrotalcite-like phase and then improved the removal efficiency of bromate. In addition, the effects of solid-to-solution ratio, contact time, initial bromate concentration, initial pH, coexisting anions on the bromate removal were investigated. The results showed the bromate with an initial concentration of 1.56 μmol/L could be completely removed from solution by Fe–Al LDHs within 120 min. When the initial bromate concentration was 7.81 μmol/L, the Fe–Al LDHs with irradiation time of 30 min exhibited the optimum removal efficiency and the bromate removal capacity (q e ) was 6.80 μmol/g. In addition, the appearance of sulfate and production of bromide were observed simultaneously in this process, which suggested that ion-exchange between sulfate and bromate, and the reduction of bromate to bromide by Fe 2+ were the main mechanisms responsible for the bromate removal by Fe–Al LDHs

  20. Biocompatibility assessment of graphene oxide-hydroxyapatite coating applied on TiO2 nanotubes by ultrasound-assisted pulse electrodeposition.

    Science.gov (United States)

    Fathyunes, Leila; Khalil-Allafi, Jafar; Sheykholeslami, Seyed Omid Reza; Moosavifar, Maryam

    2018-06-01

    In this study, the ultrasound-assisted pulse electrodeposition was introduced to fabricate the graphene oxide (GO)-hydroxyapatite (HA) coating on TiO 2 nanotubes. The results of the X-ray diffraction (XRD), Fourier Transform Infrared spectroscope (FTIR), Transmission Electron Microscope (TEM) and micro-Raman spectroscopy showed the successful synthesis of GO. The Scanning Electron Microscope (SEM) images revealed that in the presence of ultrasonic waves and GO sheets a more compact HA-based coating with refined microstructure could be formed on the pretreated titanium. The results of micro-Raman analysis confirmed the successful incorporation of the reinforcement filler of GO into the coating electrodeposited by the ultrasound-assisted method. The FTIR analysis showed that the GO-HA coating was consisted predominantly of the B-type carbonated HA (CHA) phase. The pretreatment of the substrate and incorporation of the GO sheets into the HA coating had a significant effect on improving the bonding strength at the coating-substrate interface. Moreover, the results of the fibroblast cell culture and 3‑(4,5‑dimethylthiazolyl‑2)‑2, 5‑diphenyltetrazolium bromide (MTT) assay after 2 days demonstrated a higher percentage of cell activity for the GO-HA coated sample. Finally, the 7-day exposure to simulated body fluid (SBF) showed a faster rate of apatite precipitation on the GO-HA coating, as compared to the HA coating and pretreated titanium. Copyright © 2018 Elsevier B.V. All rights reserved.

  1. Comparison of bioconcentration of ionic silver and silver nanoparticles in zebrafish eleutheroembryos.

    Science.gov (United States)

    López-Serrano, A; Muñoz-Olivas, R; Sanz-Landaluze, J; Olasagasti, M; Rainieri, S; Cámara, C

    2014-08-01

    The production of silver nanoparticles has reached nowadays high levels. Bioconcentration studies, information on persistence and toxicity are fundamental to assess their global risk and thus necessary to establish legislations regarding their use. Previous studies on silver nanoparticle toxicity have determined a clear correlation between their chemical stability and toxicity. In this work, experimental conditions able to assure silver nanoparticles stability have been optimized. Then, zebrafish (Danio rerio) eleutheroembryos were exposed to ionic silver and to Ag NPs for comparison purposes. A protocol alternative to the OECD 305 technical guideline was used. To determine silver concentration in both the eleutheroembryos and the exposure media, an analytical method consisting in ultrasound assisted extraction, followed by inductively coupled plasma mass spectrometry and graphite furnace atomic absorption spectrometry, was developed. Then, bioconcentration factors were calculated. The results revealed that ionic silver was more accumulative for zebrafish eleutheroembryos than nanoparticles at the levels tested. Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. METODE EKSTRAKSI PELARUT BERBANTUAN ULTRASONIK UNTUK RECOVERY MINYAK DARI LIMBAH CAIR PABRIK KELAPA SAWIT Application of Ultrasound-assisted Solvent Extraction for Recovery of Oil from Palm Oil Mill Effluent

    Directory of Open Access Journals (Sweden)

    Muhammad Dani Supardan

    2012-05-01

    Full Text Available In this study, application of ultrasound-assisted solvent extraction for recovery of oil from palm oil mill effluent (POMEwas studied. Extraction conditions such as volume ratio of POME to solvent, extraction time and type of solvent were investigated. Extraction was carried out at room temperature with total volume (POME and solvent of 300 ml. The experimental results showed that ultrasound-assisted extraction provided higher yield than without ultrasound using mechanical stirring. The highest oil yield of 0.265 % obtained at ultrasound-assisted extraction condition of volume ratio of POME to solvent 5:1, extraction time of 60 minutes using n-hexane as solvent. The highest oil yield and carotene concentration were obtained by n-hexane. Meanwhile, there was no significant differenece of carotene concentration obtained from ultrasound-assisted and without ultrasound-assisted extraction. ABSTRAK Penelitian ini bertujuan mempelajari metode ekstraksi pelarut berbantuan ultrasonik untuk recovery minyak dari limbahcair pabrik kelapa sawit. Ekstraksi dilakukan pada temperatur kamar dengan menggunakan volum total campuran (limbah dan pelarut sebanyak 300 ml. Variabel penelitian yang digunakan adalah rasio volum limbah terhadap pelarut (1:1; 2:1; 4:1; dan 5:1, waktu ekstraksi (30, 60, 90 dan 120 menit, dan jenis pelarut (n-heksan dan petroleum eter. Hasil penelitian menunjukkan bahwa ekstraksi berbantuan ultrasonik menghasilkan rendemen minyak yang lebih besar dibandingkan ekstraksi tanpa bantuan ultrasonik dengan menggunakan pengadukan mekanik. Rendemen minyak tertinggi sebesar 0,265 % diperoleh pada proses ekstraksi berbantuan ultrasonik dengan rasio volum limbah terhadap pelarut 5:1, waktu ekstraksi 90 menit dengan menggunakan pelarut n-heksan. Rendemen minyak dan konsentrasi karoten yang lebih tinggi diperoleh pada ekstraksi menggunakan pelarut n-heksan. Metode ekstraksi pelarut berbantuan ultrasonik dan tanpa bantuan ultrasonik memberikan perbedaan

  3. Modified Ionic Liquid-Based High-Performance Lubricants for Robotic Operations Project

    Data.gov (United States)

    National Aeronautics and Space Administration — NASA requires a highly efficient lubrication system for robotic operations, which will withstand very low temperatures (20 K) and other rigors of outer space and...

  4. Ionic-Liquid-Based Acidic Aqueous Biphasic Systems for Simultaneous Leaching and Extraction of Metallic Ions.

    Science.gov (United States)

    Gras, Matthieu; Papaiconomou, Nicolas; Schaeffer, Nicolas; Chainet, Eric; Tedjar, Farouk; Coutinho, Joao A P; Billard, Isabelle

    2018-02-05

    The first instance of an acidic aqueous biphasic system (AcABS) based on tributyltetradecyl phosphonium chloride ([P 44414 ][Cl]) and an acid is here reported. This AcABS exhibits pronounced thermomorphic behavior and is shown to be applicable to the extraction of metal ions from concentrated acidic solutions. Metal ions such as cobalt(II), iron(III), platinum(IV) and nickel(II) are found to partition preferentially to one of the phases of the acidic aqueous biphasic system and it is here shown that it successfully allows the difficult separation of Co II from Ni II , here studied at 24 and 50 °C. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Modified Ionic Liquid-Based High-Performance Lubricants for Robotic Operations, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — NASA requires a highly efficient lubrication system for robotic operations, which will withstand very low temperatures (20 K) and other rigors of outer space and...

  6. Modified Ionic Liquid-Based Phase Change Materials as Effective Heat Exchangers, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Future manned spacecraft venturing into deep space will require sophisticated thermal control systems to protect against extreme environments ranging from direct...

  7. Modified Ionic Liquid-Based Phase Change Materials as Effective Heat Exchangers, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — Future manned mission venturing into deep space will require sophisticated thermal control systems to protect against extreme environments ranging from direct...

  8. Modified Ionic Liquid-Based High-Performance Lubricants for Robotic Operations, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — NASA needs an advanced lubrication solution for its future robotic systems and planetary surface assets. The required lubrication technology must offer...

  9. Synthesis, Characterization, Thermal Analyses, and Spectroscopic Properties of Novel Naphthyl-Functionalized Imidazolium Ionic Liquids

    Science.gov (United States)

    Yao, Meihuan; Li, Qing; Xia, Yanqiu; Liang, Yongmin

    2018-03-01

    A series of novel ionic liquids based on naphthyl-functionalized imidazolium cation have been prepared. Their structure was characterized by NMR. The thermal stabilities of the prepared liquids were studied by thermal gravimetric analysis. The new ionic liquids containing NTf- 2 anion display significantly higher thermal stabilities (>400°C). Anion exchange to PF- 6, BF- 4, and Br- decreases the thermal stabilities of such ionic liquids. Fluorescence and UV-Vis absorption spectroscopy were used to study the spectroscopic properties of the ionic liquids. Compared with common ionic liquids, the described ionic liquids provide robust fluorescence properties and remarkably increased UV-Vis absorption. This research may enrich the field of functionalized ionic liquids and provide a platform for extension of ionic liquid applications.

  10. Battery electrolytes based on saturated ring ionic liquids: Physical and electrochemical properties

    International Nuclear Information System (INIS)

    Di Leo, Roberta A.; Marschilok, Amy C.; Takeuchi, Kenneth J.; Takeuchi, Esther S.

    2013-01-01

    Physical and electrochemical properties of mixtures of ionic liquids based on saturated ring systems with carbonate based solvents were investigated. The conductivity and electrochemical stability of two series of ionic liquids based on piperidinium and pyrrolidinium cations with tetrafluoroborate and bis(trifluorosulfonylimide) anions were evaluated. The effects of the ionic liquid cation, substituent chain length of the cation function group, and the anion type on conductivity and electrochemical stability as determined by cyclic voltammetry were studied. The conductivity was influenced by the substituent chain length of the ionic liquid cation and the solvent carbonate type, where higher conductivities were observed with shorter substituent chains and EC versus PC. The saturated ring ionic liquid–carbonate mixtures may show particular promise for implementation as battery electrolytes due to notable high voltage stabilities, where stability >5.5 V was maintained in the presence of lithium salt. This study should promote development of future safe, high voltage lithium ion battery systems

  11. Ultrasound assisted dispersion of different amount of Ni over ZSM-5 used as nanostructured catalyst for hydrogen production via CO2 reforming of methane

    International Nuclear Information System (INIS)

    Vafaeian, Yaser; Haghighi, Mohammad; Aghamohammadi, Sogand

    2013-01-01

    Graphical abstract: A series of Ni/ZSM-5 nanocatalysts with different amount of Ni were prepared via ultrasound assisted method and characterized with XRD, FESEM, TEM, BET and FTIR techniques. The research deals with catalyst development for dry reforming of methane with the aim of reaching the most stable catalyst specifically over nano-sized catalysts. About more than 99% of Ni particles size is less than 100 nm for the sample prepared with 8% Ni, which is essential to the relative suppression of the carbon formation on catalysts. Catalyst prepared with 8% Ni content showed superior activity in process expected due to its better catalytic properties. - Highlights: • Using ZSM-5 zeolite in dry reforming of methane. • Employing ultrasound energy in synthesis of Ni/ZSM-5 nanocatalyst. • Enhancement of Ni particles size to meet desired catalyst at lower amount of Ni loading. • Dry reforming of methane over Ni/ZSM-5 nanocatalyst with different Ni-loading. • Superior activity of Ni/ZSM-5 nanocatalyst synthesized with 8% Ni content. - Abstract: Carbon dioxide reforming of methane is an interesting route for synthesis gas production especially over nanostructured catalysts. The present research deals with nanocatalyst development by sonochemical method for dry reforming of methane with the aim of reaching the most efficient nanocatalyst. Effect of Ni metal content, one of the most significant variables, on the properties of the ZSM-5 supported nanocatalysts was taken into account. The Ni/ZSM-5 nanocatalysts were prepared via assisted traditional impregnation method via ultrasound irradiation and characterized with XRD, FESEM, TEM, BET and FTIR techniques. Comparison of XRD patterns implies that the peaks related to NiO become sharper by increasing metal content over the support. In the case of nanocatalysts with lower metal content (3% and 8%), the beneficial influence of ultrasound assisted procedure become more pronounced and the observed reduction in

  12. Ionic liquid and nanoparticle hybrid systems: Emerging applications.

    Science.gov (United States)

    He, Zhiqi; Alexandridis, Paschalis

    2017-06-01

    Having novel electronic and optical properties that emanate from their nano-scale dimensions, nanoparticles are central to numerous applications. Ionic liquids can confer to nanoparticle chemical protection and physicochemical property enhancement through intermolecular interactions and can consequently improve the stability and reusability of nanoparticle for various operations. With an aim to combine the novel properties of nanoparticles and ionic liquids, different structures have been generated, based on a balance of several intermolecular interactions. Such ionic liquid and nanoparticle hybrids are showing great potential in diverse applications. In this review, we first introduce various types of ionic liquid and nanoparticle hybrids, including nanoparticle colloidal dispersions in ionic liquids, ionic liquid-grafted nanoparticles, and nanoparticle-stabilized ionic liquid-based emulsions. Such hybrid materials exhibit interesting synergisms. We then highlight representative applications of ionic liquid and nanoparticle hybrids in the catalysis, electrochemistry and separations fields. Such hybrids can attain better stability and higher efficiency under a broad range of conditions. Novel and enhanced performance can be achieved in these applications by combining desired properties of ionic liquids and of nanoparticles within an appropriate hybrid nanostructure. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Extraction of Natural Antioxidants from the Thelephora ganbajun Mushroom by an Ultrasound-Assisted Extraction Technique and Evaluation of Antiproliferative Activity of the Extract against Human Cancer Cells.

    Science.gov (United States)

    Xu, Dong-Ping; Zheng, Jie; Zhou, Yue; Li, Ya; Li, Sha; Li, Hua-Bin

    2016-10-01

    The Thelephora ganbajun mushroom has been found to be a potential rich source of natural antioxidants. In this study, an ultrasound-assisted extraction (UAE) technique together with GRAS (generally recognized as safe) solvents (ethanol and water) was used to maximize the extraction of antioxidants from Thelephora ganbajun . Five extraction parameters (ethanol concentration, solvent to solid ratio, extraction time, temperature and ultrasound power) were investigated by single-factor experiments, and then a central composite rotatable design was employed to study interaction of three key extraction parameters. The optimum conditions were as follows: 57.38% ethanol, 70.15 mL/g solvent to solid ratio, 10.58 min extraction time, 40 °C extraction temperature and 500 W ultrasound power. Under the optimum conditions, the antioxidant activity obtained was 346.98 ± 12.19 µmol Trolox/g DW, in accordance with the predicted value of 344.67 µmol Trolox/g DW. Comparison of UAE with conventional maceration and Soxhlet extraction, the UAE method showed stronger extract efficiency in a shorter extraction time. These results showed that UAE was an effective technique to extract antioxidants from Thelephora ganbajun . Furthermore, the extracts obtained under the optimized conditions exhibited antiproliferative activities toward human lung (A549), breast (MCF-7), liver (HepG2) and colon (HT-29) cancer cells, especially for liver and lung cancer cells. In addition, rutin, 2-hydrocinnamic acid and epicatechin were identified in the extract, which might contribute to antioxidant and antiproliferative activities.

  14. Ultrasound-assisted leaching of rare earths from the weathered crust elution-deposited ore using magnesium sulfate without ammonia-nitrogen pollution.

    Science.gov (United States)

    Yin, Shaohua; Pei, Jiannan; Jiang, Feng; Li, Shiwei; Peng, Jinhui; Zhang, Libo; Ju, Shaohua; Srinivasakannan, Chandrasekar

    2018-03-01

    The in situ leaching process of China's unique ion-adsorption rare earth ores has caused severe environmental damages due to the use of (NH 4 ) 2 SO 4 solution. This study reports that magnesium sulfate (MgSO 4 ) as a leaching agent would replace (NH 4 ) 2 SO 4 by ultrasonically assisted leaching to deal with the ammonia-nitrogen pollution problem and enhance leaching process. At leaching conditions of 3wt% MgSO 4 concentration, 3:1L/S ratio and 30min, the total rare earth leaching efficiency reaches 75.5%. Ultrasound-assisted leaching experiments show that the leaching efficiency of rare earths is substantially increased by introducing ultrasound, and nearly completely leached out after two stage leaching process. Thus, ultrasonic-assisted leaching process with MgSO 4 is not only effective but also environmentally friendly, and beneficial to leach rare earths at laboratory scale. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Continuous ultrasound-assisted extraction of cadmium from legumes and dried fruit samples coupled with on-line preconcentration-flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yebra, M.C.; Cancela, S. [University of Santiago de Compostela, Department of Analytical Chemistry, Nutrition and Bromatology, Santiago de Compostela (Spain)

    2005-06-01

    Cadmium was continuously extracted with diluted nitric acid from legumes and dried fruit samples using a simple, rapid and continuous ultrasound-assisted extraction system. A minicolumn packed with a chelating resin (Chelite P, with aminomethylphosphoric acid groups) was placed between the extraction unit and the detector for cadmium preconcentration. The cadmium content in the acid extract was retained into the minicolumn, and elution was carried out with hydrochloric acid, with this trace metal continuously monitored by flame atomic absorption spectrometry. An experimental design (Plackett-Burman 2{sup 6} x 3/16) was used to optimize the continuous leaching procedure and the preconcentration step. The method allowed a total sampling frequency of 10 and 14 samples per hour for legumes and dried fruit, respectively. The procedure displayed good precision (2.0 and 2.5%, respectively, expressed as relative standard deviations) for samples containing 0.202{+-}0.005 {mu}g g{sup -1} Cd (broad bean) and 0.239{+-}0.004 {mu}g g{sup -1} Cd (peanut). Detection limits of 0.014 {mu}g g{sup -1} Cd for 60 mg of legume samples and 0.011 {mu}g g{sup -1} Cd for 80 mg of dried fruit samples were obtained. The method was successfully applied to the determination of trace amounts of cadmium in legumes and dried fruit samples. (orig.)

  16. Ultrasound-assisted extraction technique for establishing selenium contents in breast cancer biopsies by Zeeman-electrothermal atomic absorption spectrometry using multi-injection

    International Nuclear Information System (INIS)

    Lavilla, I.; Mosquera, A.; Millos, J.; Cameselle, J.; Bendicho, C.

    2006-01-01

    A solid-liquid extraction method is developed to establish the contents of selenium in breast cancer biopsies. The method is based on the ultrasound-assisted extraction of selenium from pretreated biopsies prior to Se determination by atomic absorption spectrometry with longitudinal-Zeeman background correction. Fifty-one breast biopsies were collected from the Cies Hospital (Vigo, Spain), 32 of which correspond to tumor tissue and 19 to normal tissue (parenchyma). Difficulties arising from the samples analyzed, i.e. small samples mass (50-100 mg), extremely low Se contents and sample texture modification including tissue hardening due to formaldehyde preservation are addressed and overcome. High intensity sonication using a probe together with addition of hydrogen peroxide succeeded in completely extracting Se from biopsies. The multiple injection technique was useful to tackle the low Se contents present in some biopsies. The detection limit was 25 ng g -1 of Se and the precision, expressed as relative standard deviation, was less than 10%. Se contents ranged from 0.08 to 0.4 μg g -1 for parenchyma samples and from 0.09 to 0.8 μg g -1 for tumor samples. In general, Se levels in tumor biopsies were higher as compared with the adjacent normal tissue in 19 patients by a factor of up to 6. Analytical data confirmed Se accumulation in the breast tumors

  17. Ultrasound-assisted surfactant-enhanced emulsification microextraction for the determination of carbamates in wines by ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Moreno-González, David; Huertas-Pérez, José F; García-Campaña, Ana M; Bosque-Sendra, Juan M; Gámiz-Gracia, Laura

    2013-11-08

    A new sensitive multiresidue method based on ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) has been developed for the detection, confirmation and quantification of twenty five carbamates in wine samples. The separation was achieved in 5.5 min, using a Zorbax Eclipse plus RRHD C18 column (50 mm×2.1 mm, 1.8 μm), with a mobile phase of water and methanol, both of them with 0.01% formic acid. The analytes were detected in positive mode with multiple reaction monitoring mode. Ultrasound-assisted surfactant-enhanced emulsification microextraction (UASEME), using a low-density extraction solvent has been optimized for the satisfactory extraction of carbamates and clean-up of extracts. The matrix effect was studied, showing that the proposed procedure provides very clean extracts. Under optimum conditions, recoveries for fortified wine samples ranged from 74 to 102%, with relative standard deviations lower than 6%. Limits of quantification ranged from 0.15 to 0.92 μgl(-1), showing the high sensitivity of this fast and simple method and its compliance with current requirements. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Determination of Pb in river water samples by inductively coupled plasma optical emission spectrometry after ultrasound-assisted co-precipitation with manganese dioxide

    International Nuclear Information System (INIS)

    Sousa Bispo, Marcia; Santos da Boa Morte, Elane; Korn das Gracas Andrade, Maria; Sena Gomes Teixeira, Leonardo; Korn, Mauro; Costa, Antonio Celso Spinola

    2005-01-01

    A simple and efficient procedure for separation and pre-concentration using ultrasound-assisted co-precipitation with manganese dioxide was developed for Pb determination by inductively coupled plasma optical emission spectrometry (ICP OES). The optimization process was carried out using a two-level factorial design and a Doehlert matrix. Three variables (i.e. concentration of oxidizing solution-KMnO 4 , concentration of MnSO 4 solution and time of ultrasonic irradiation) were used as factors in the optimization. The recoveries, based on the analysis of spiked samples, were between 90% and 105%, and the precision was ≤ 5%. The detection limit and quantification limit for Pb determination were 3.2 and 10.7 μg L -1 , respectively. The proposed method was applied for the determination of Pb in water samples from a river heavily polluted by industrial effluents. The recovery measured by analyte addition technique showed that the proposed pre-concentration method had good accuracy

  19. A phase separation method for analyses of fluoroquinones in meats based on ultrasound-assisted salt-induced liquid-liquid microextraction and a new integrated device.

    Science.gov (United States)

    Wang, Huili; Gao, Ming; Xu, Youqu; Wang, Wenwei; Zheng, Lian; Dahlgren, Randy A; Wang, Xuedong

    2015-08-01

    Herein, we developed a novel integrated device to perform phase separation based on ultrasound-assisted, salt-induced, liquid-liquid microextraction for determination of five fluoroquinones in meats by HPLC analysis. The novel integrated device consisted of three simple HDPE (high density polyethylene) parts that were used to separate the solvent from the aqueous solution prior to retrieving the extractant. The extraction parameters were optimized using the response surface method based on central composite design: 589μL of acetone solvent, pH2.1, 4.1min extraction time and 3.5g of Na2SO4. The limits of detection were 0.056-0.64 μgkg(-1) and recoveries were 87.2-110.6% for the five fluoroquinones in muscle tissue from fish, chicken, pork and beef. This method is easily constructed from inexpensive materials, extraction efficiency is high, and the approach is compatible with HPLC analysis. Thus, it has excellent prospects for sample pre-treatment and analysis of fluoroquinones in meat samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

  20. Ultrasound-assisted extraction of fructans from agave (Agave tequilana Weber var. azul at different ultrasound powers and solid-liquid ratios

    Directory of Open Access Journals (Sweden)

    Miguel Ángel SÁNCHEZ-MADRIGAL

    Full Text Available Abstract The effects of ultrasound-assisted extraction (UAE at different ultrasound power densities (UPDs; 40, 80, and 120 mW/mL and solid:liquid (S:L ratio (1:2, 1:3, and 1:6 on the extraction of carbohydrates from Agave tequilana plant of different ages were evaluated. Extracts obtained (6- and 7-year-old plant were analyzed in the yield of carbohydrates (YC, fructan (FRU content, simple sugars, fructan profile and the average degree of polymerization (DPn. UPD, S:L ratio, and plant age all affected YC, FRU, and DPn. Maximum YC and FRU were obtained from the older agave with UPD and S:L ratio of 120 mW/mL and 1:6, respectively; while glucose, fructose, and sucrose were highly released from the younger plant. Agave of 7-year-old presented the highest DPn. Fructan degradation occurred at high UPD, increasing the simple sugars and decreasing the DPn. Thermal-traditional extraction without sonication caused more fructan degradation; and overall, ultrasound enhanced fructan extraction and minimized fructan damage, representing a technological alternative for fructan extraction from agave.

  1. Design and optimization of ultrasound assisted extraction of curcumin as an effective alternative for conventional solid liquid extraction of natural products.

    Science.gov (United States)

    Mandal, Vivekananda; Dewanjee, Saikat; Sahu, Ranabir; Mandal, Subhash C

    2009-01-01

    The first step in the qualitative and quantitative analysis of medicinal plant constituents is the extraction step. Ideally, an extraction procedure should be exhaustive with respect to the constituents to be analyzed, rapid, simple, and for routine analysis amenable to automation. Usually, the traditional techniques require long extraction times, with more consumption of energy resources and organic solvent, have low efficiency and are often unsafe for thermolabile botanicals. The Taguchi based optimization technique was adapted for the process optimization of ultrasound assisted extraction (UAE) of Curcuma longa to identify the effect of four major factors namely, extraction time, solvent viscosity, grinding degree and solvent volume on the percentage extraction of curcumin. The reproducibility and recovery of the method was also investigated. The efficiency of the new extraction method was then compared with conventional solid liquid extraction procedures. Using this novel method, long hours of conventional Soxhlet extraction were cut down to 70 minutes of UAE with greater reproducibility and recovery. The study clearly shows that this method can be effectively utilized for cutting down long extraction time of botanicals to just a few minutes without the aid of heat.

  2. Ultrasound assisted production of fatty acid methyl esters from transesterification of triglycerides with methanol in the presence of KOH catalyst: optimization, mechanism and kinetics.

    Science.gov (United States)

    Thanh, Le Tu; Okitsu, Kenji; Maeda, Yasuaki; Bandow, Hiroshi

    2014-03-01

    Ultrasound assisted transesterification of triglycerides (TG) with methanol in the presence of KOH catalyst was investigated, where the changes in the reactants and products (diglycerides (DG), monoglycerides (MG), fatty acid methyl esters (FAME) and glycerin (GL)) concentrations were discussed to understand the reaction mechanism and kinetics under ultrasound irradiation. The optimum reaction condition for the FAME production was the concentration of KOH 1.0 wt.%, molar ratio of TG to methanol of 1:6, and irradiation time of 25 min. The rate constants during the TG transesterification with methanol into GL and FAME were estimated by a curve fitting method with simulated curves to the obtained experimental results. The rate constants of [Formula: see text] were estimated to be 0.21, 0.008, 0.23, 0.005, 0.14 and 0.001 L mol(-1)min(-1), respectively. The rate determining step for the TG transesterification with methanol into GL and FAME was the reaction of MG with methanol into GL and FAME. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Postharvest Ultrasound-Assisted Freeze-Thaw Pretreatment Improves the Drying Efficiency, Physicochemical Properties, and Macamide Biosynthesis of Maca (Lepidium meyenii).

    Science.gov (United States)

    Chen, Jin-Jin; Gong, Peng-Fei; Liu, Yi-Lan; Liu, Bo-Yan; Eggert, Dawn; Guo, Yuan-Heng; Zhao, Ming-Xia; Zhao, Qing-Sheng; Zhao, Bing

    2018-04-01

    A novel technique of ultrasound-assisted freeze-thaw pretreatment (UFP) was developed to improve the drying efficiency of maca and bioactive amide synthesis in maca. The optimal UFP conditions are ultrasonic processing 90 min at 30 °C with 6 freeze-thaw cycles. Samples with freeze-thaw pretreatment (FP), ultrasound pretreatment (UP), and UFP were prepared for further comparative study. A no pretreatment (NP) sample was included as a control. The results showed that UFP improved the drying efficiency of maca slices, showing the highest effective moisture diffusivity (1.75 × 10 -9 m 2 /s). This result was further supported by low-field nuclear magnetic resonance (LF-NMR) analysis and scanning electron microscopy (SEM). The rehydration capacity and protein content of maca slices were improved by UFP. More importantly, contents of bioactive macamides and their biosynthetic precursors were increased in 2.5- and 10-fold, respectively. In conclusion, UFP is an efficient technique to improve drying efficiency, physicochemical properties, and bioactive macamides of maca, which can be applied in the industrial manufacture of maca products. © 2018 Institute of Food Technologists®.

  4. Optimization of Ultrasound-Assisted Extraction, HPLC and UHPLC-ESI-Q-TOF-MS/MS Analysis of Main Macamides and Macaenes from Maca (Cultivars of Lepidium meyenii Walp).

    Science.gov (United States)

    Chen, Shu-Xiao; Li, Ke-Ke; Pubu, Duoji; Jiang, Si-Ping; Chen, Bin; Chen, Li-Rong; Yang, Zhen; Ma, Chao; Gong, Xiao-Jie

    2017-12-10

    Ultrasound-assisted extraction (UAE), using petroleum ether as the solvent, was systematically applied to extract main macamides and macaenes from Maca hypocotyls. Extraction yield was related with four variables, including ratio of solution to solid, extraction temperature, extraction time, and extraction power. On the basis of response surface methodology (RSM), the optimal conditions were determined to be the ratio of solution to solid as 10:1 (mL/g), the extraction temperature of 40 °C, the extraction time of 30 min, and the extraction power of 200 W. Based on the optimal extraction method of UAE, the total contents of ten main macamides and two main macaenes of Maca cultivated in twenty different areas of Tibet were analyzed by HPLC and UHPLC-ESI-Q-TOF-MS/MS. This study indicated that UAE was able to effectively extract macamides alkaloids from Maca hypocotyls. Quantitative analysis showed that geographical origins, not ecotypes, played a more important role on the accumulation of active macamides in Maca.

  5. Influence of High Shear Dispersion on the Production of Cellulose Nanofibers by Ultrasound-Assisted TEMPO-Oxidation of Kraft Pulp.

    Science.gov (United States)

    Loranger, Eric; Piché, André-Olivier; Daneault, Claude

    2012-09-10

    Cellulose nanofibers can be produced using a combination of TEMPO, sodium bromide (NaBr) and sodium hypochlorite, and mechanical dispersion. Recently, this process has been the subject of intensive investigation. However, studies on the aspects of mechanical treatment of this process remain marginal. The main objective of this study is to evaluate the high shear dispersion parameters (e.g., consistency, stator-rotor gap, recirculation rate and pH) and determine their influences on nanocellulose production using ultrasound-assisted TEMPO-oxidation of Kraft pulp. All nanofiber gels produced in this study exhibited rheological behaviors known as shear thinning. From all the dispersion parameters, the following conditions were identified as optimal: 0.042 mm stator-rotor gap, 200 mL/min recycle rate, dispersion pH of 7 and a feed consistency of 2%. High quality cellulose gel could be produced under these conditions. This finding is surely of great interest for the pulp and paper industry.

  6. Simultaneous ultrasound-assisted water extraction and β-cyclodextrin encapsulation of polyphenols from Mangifera indica stem bark in counteracting TNFα-induced endothelial dysfunction.

    Science.gov (United States)

    Mura, Marzia; Palmieri, Daniela; Garella, Davide; Di Stilo, Antonella; Perego, Patrizia; Cravotto, Giancarlo; Palombo, Domenico

    2015-01-01

    This study proposes an alternative technique to prevent heat degradation induced by classic procedures of bioactive compound extraction, comparing classical maceration/decoction in hot water of polyphenols from Mango (Mangifera indica L.) (MI) with ultrasound-assisted extraction (UAE) in a water solution of β-cyclodextrin (β-CD) at room temperature and testing their biological activity on TNFα-induced endothelial dysfunction. Both extracts counteracted TNFα effects on EAhy926 cells, down-modulating interleukin-6, interleukin-8, cyclooxygenase-2 and intracellular adhesion molecule-1, while increasing endothelial nitric oxide synthase levels. β-CD extract showed higher efficacy in improving endothelial function. These effects were abolished after pre-treatment with the oestrogen receptor inhibitor ICI1182,780. Moreover, the β-CD extract induced Akt activation and completely abolished the TNFα-induced p38MAPK phosphorylation. UAE and β-CD encapsulation provide an efficient extraction protocol that increases polyphenol bioavailability. Polyphenols from MI play a protective role on endothelial cells and may be further considered as oestrogen-like molecules with vascular protective properties.

  7. Ultrasound-assisted single extraction tests for rapid assessment of metal extractability from soils by total reflection X-ray fluorescence.

    Science.gov (United States)

    De La Calle, I; Cabaleiro, N; Lavilla, I; Bendicho, C

    2013-09-15

    In this work, ultrasound-assisted extraction (UAE) was employed for acceleration of metal extraction from soil samples. After extraction, multielemental analysis (Cr, Mn, Fe, Ni, Cu, Zn and Pb) of EDTA and acetic acid extracts was performed by total reflection X-ray fluorescence spectrometry (TXRF). High-intensity ultrasonic processors, i.e. the ultrasonic probe (50W) and the cup-horn sonoreactor (200W) were applied. Both ultrasonic procedures were compared with a miniaturized version of the single extraction scheme proposed by the Standards, Measurements and Testing program (SM&T). The extraction time with EDTA was reduced from 1h (conventional procedure) to 2 min (ultrasonic probe) or to 10 min (cup-horn sonoreactor). The time required for acetic acid extraction was also reduced from 16 h (conventional procedure) to 6 min (ultrasonic probe) or to 30 min (cup-horn sonoreactor). In addition, the amount of sample and extractants was drastically reduced as a result of the miniaturization implemented in the developed approaches. The combination of UAE and TXRF allows assessing the potential metal mobility and bioavailability in a simple way. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Synthesis and characterization of ultrasound assisted "graphene oxide-magnetite" hybrid, and investigation of its adsorption properties for Sr(II) and Co(II) ions

    Science.gov (United States)

    Tayyebi, Ahmad; Outokesh, Mohammad; Moradi, Shahab; Doram, Amir

    2015-10-01

    Magnetite nanoparticles with a size distribution of 15-21 nm were synthesized and decorated onto surface of graphene oxide by ultrasound assisted precipitation. Size and size distribution of the obtained M-GO hybrid were appreciably finer than the hybrids prepared by stirring method. M-GO is a superparamagnetic material with saturation magnetization of 31 emu g-1. The Langevin equation was successfully applied for estimation of size of Fe3O4 nanoparticles in M-GO hybrid, with maximum error of 17.5%. The study put forward a formation mechanism for M-GO, based on instrumental analyses. Adsorption isotherms of Sr2+ and Co2+ ions, which were fitted by Langmuir monolayer model, displayed two-fold higher capacity for Co2+ ions, presumably due to its similarity to Fe2+ (of Fe3O4 component). Uptake of both Co2+ and Sr2+ ions were endothermic, and spontaneous, however the former proceeded through inner-shell complex formation, while the latter took place via ion exchange mechanism. Rate of adsorption of Co2+ was faster, but for both ions, chemical reaction was the rate determining step. Sorption of Sr2+ and Co2+ ions greatly increased at pHs above 5, where (1) surface zeta potential changed its sign, and (2) deprotonating reactions at the surface became complete.

  9. An optimized ultrasound-assisted extraction and simultaneous quantification of 26 characteristic components with four structure types in functional foods from ginkgo seeds.

    Science.gov (United States)

    Zhou, Guisheng; Yao, Xin; Tang, Yuping; Qian, Dawei; Su, Shulan; Zhang, Li; Jin, Chun; Qin, Yong; Duan, Jin-ao

    2014-09-01

    An optimized method of ultrasound-assisted extraction followed by ultra-high-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (UAE-UHPLC-TQ/MS(2)) was proposed for the simultaneous extraction and determination of 26 characteristic components covering four structure types (flavonoids, terpene lactones, ginkgolic acids and phenylpropanols) in ginkgo seeds (GSs). The UAE parameters (ultrasound power, time and solvent-to-material ratio) were optimized using a response surface methodology. This is the first report of the simultaneous analysis of 26 compounds in Ginkgo biloba using UHPLC-TQ/MS(2); this analysis afforded good linearity, precision, repeatability and accuracy. UAE-UHPLC-TQ/MS(2) was successfully applied to ginkgo seed samples, and the analysis showed that GSs are rich in terpene lactones and could be selected as a healthy food resource. The results suggest that UAE-UHPLC-TQ/MS(2) might be able to be utilized as a tool for the quality assessment of samples from GSs or other related products using flavonoids, terpene lactones, ginkgolic acids and phenylpropanols as markers. Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. Indirect determination of the flavor enhancer maltol in foods and beverages through flame atomic absorption spectrometry after ultrasound assisted-cloud point extraction.

    Science.gov (United States)

    Altunay, Nail; Gürkan, Ramazan; Orhan, Ulaş

    2017-11-15

    A simple ultrasound assisted-cloud point extraction (UA-CPE) method was developed and combined with flame atomic absorption spectrometry (FAAS) for pre-concentration and indirect determination of the flavor enhancer maltol in foods and beverages. The method is based on reduction of Cu(II) to Cu(I) by maltol at pH 6.5, and subsequent selective interaction of Cu(I) with bathocuproine (BCP) to form a ternary complex in presence of sodium dodecyl sulfate (SDS). Under the optimized conditions, pre-concentration of a 35mL sample solution allowed detection of 1.24µgL -1 maltol in a linear range of 4-230µgL -1 . The method was validated by intra- and inter-day precision studies ranging from 2.1 to 3.4%, and recoveries ranged from 93.3% to 104.4% using standard addition method. After pretreatment with two different sample preparation steps assisted by ultrasound energy, the proposed method was applied successfully for determination of maltol in selected foods and beverages. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Sensitive Detection of Organophosphorus Pesticides in Medicinal Plants Using Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction Combined with Sweeping Micellar Electrokinetic Chromatography.

    Science.gov (United States)

    Wei, Jin-Chao; Hu, Ji; Cao, Ji-Liang; Wan, Jian-Bo; He, Cheng-Wei; Hu, Yuan-Jia; Hu, Hao; Li, Peng

    2016-02-03

    A simple, rapid, and sensitive method using ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) combined with sweeping micellar electrokinetic chromatography (sweeping-MEKC) has been developed for the determination of nine organophosphorus pesticides (chlorfenvinphos, parathion, quinalphos, fenitrothion, azinphos-ethyl, parathion-methyl, fensulfothion, methidathion, and paraoxon). The important parameters that affect the UA-DLLME and sweeping efficiency were investigated. Under the optimized conditions, the proposed method provided 779.0-6203.5-fold enrichment of the nine pesticides compared to the normal MEKC method. The limits of detection ranged from 0.002 to 0.008 mg kg(-1). The relative standard deviations of the peak area ranged from 1.2 to 6.5%, indicating the good repeatability of the method. Finally, the developed UA-DLLME-sweeping-MEKC method has been successfully applied to the analysis of the investigated pesticides in several medicinal plants, including Lycium chinense, Dioscorea opposite, Codonopsis pilosula, and Panax ginseng, indicating that this method is suitable for the determination of trace pesticide residues in real samples with complex matrices.

  12. A Method Based on Ultrasound-assisted Solidification of Floating Drop Microextraction Technique for the Spectrophotometric Determination of Curcumin in Turmeric Powder

    Directory of Open Access Journals (Sweden)

    Abbas Afkhami

    2017-06-01

    Full Text Available A method based on the ultrasound-assisted solidification of floating drop microextraction technique was developed for the spectrophotometric and spectrofluorimetric determination of curcumin in turmeric powder. In this work a small volume of an organic solvent was floated on the surface of an aqueous solution. After sonication the organic solvent is solidified and separated. The effect of extraction parameters such as type and the volume of organic solvent, temperature, salt addition and exposure time, on the extraction recovery was investigated and optimized. Finally, the method droplet was used for the determination of analyte. Under the optimum extraction conditions, a linear range of 0.006–30 μg mL-1 and a relative standard deviation (RSD of 2.72% for curcumin wasachieved. Limits of detection of 7 and 2 ng mL-1 curcumin was obtained for the spectrophotometric and spectrofluometric methods, respectively. The obtained results show that the application of this method can be successful for the analysis of curcumin in turmeric powder samples.

  13. Optimisation of an ultrasound-assisted extraction followed by RP-HPLC separation for the simultaneous determination of oleanolic acid, ursolic acid and oridonin content in Rabdosia rubescens.

    Science.gov (United States)

    Yang, Yu-Chiao; Wei, Ming-Chi; Huang, Ting-Chia

    2012-01-01

    Rabdosia rubescens is a commonly used herb in traditional Chinese medicine and contains diterpenoids, triterpenoids and various other compounds. Among these components, oridonin, oleanolic acid and ursolic acid have gained considerable interest concerning anti-cancer activities. However, there is no suitable currently available method for the simultaneous evaluation of these three bioactive compounds in R. rubescens. To develop an optimised ultrasound-assisted extraction (UAE) method and an efficient HPLC method for the simultaneous evaluation of the three bioactive compounds in R. rubescens. Various parameters that can potentially affect the UAE process were investigated and optimised. HPLC operating conditions were also optimised, and the chromatographic separation was performed on a C(18) -column with an acetonitrile-water gradient as the mobile phase. Validation of the HPLC technique developed showed that the method has good linearity, sensitivity, precision and accuracy. The combined UAE-HPLC method was applied to quantitate the amount of oridonin, oleanolic acid and ursolic acid in the plant sample and exhibited good repeatability (RSD (%) 92.4). Furthermore, the combined UAE-HPLC method was applied successfully to the extraction and determination of oridonin, oleanolic acid and ursolic acid content in samples obtained from different geographical regions, which is the first time that this comparison has been investigated. The combined UAE-HPLC process is a fast, convenient and appropriate method for the quantitative analysis of these three compounds in R. rubescens. Copyright © 2012 John Wiley & Sons, Ltd.

  14. Development and validation of a modified ultrasound-assisted extraction method and a HPLC method for the quantitative determination of two triterpenic acids in Hedyotis diffusa.

    Science.gov (United States)

    Yang, Yu-Chiao; Wei, Ming-Chi; Chiu, Hui-Fen; Huang, Ting-Chia

    2013-12-01

    In the present study, the oleanolic acid (OA) and ursolic acid (UA) contents ofHedyotis diffusa and H. corymbosa were determined by a rapid, selective and accurate method combining modified ultrasound-assisted extraction (MUAE) and HPLC. Compared with traditional extraction methods, MUAE reduced the extraction time, the extraction temperature and the solvent consumption and maximized the extraction yields of OA and UA. Furthermore, the combined MUAE-HPLC method was applied to quantitate OA and UA in plant samples and exhibited good repeatability, reproducibility and stability. The mean recovery studies (one extraction cycle) for OA and UA were between 91.3 and 91.7% with RSD values less than 4.5%. The pioneer method was further applied to quantitate OA and UA in six samples of H. diffusa and five samples of H. corymbosa. The results showed that the OA and UA content in the samples from different sources were significantly different. This report is valuable for the application of H. diffusa and H. corymbosa obtained from different regions in clinical research and pharmacology.

  15. Optimization of Ultrasound-Assisted Extraction, HPLC and UHPLC-ESI-Q-TOF-MS/MS Analysis of Main Macamides and Macaenes from Maca (Cultivars of Lepidium meyenii Walp

    Directory of Open Access Journals (Sweden)

    Shu-Xiao Chen

    2017-12-01

    Full Text Available Ultrasound-assisted extraction (UAE, using petroleum ether as the solvent, was systematically applied to extract main macamides and macaenes from Maca hypocotyls. Extraction yield was related with four variables, including ratio of solution to solid, extraction temperature, extraction time, and extraction power. On the basis of response surface methodology (RSM, the optimal conditions were determined to be the ratio of solution to solid as 10:1 (mL/g, the extraction temperature of 40 °C, the extraction time of 30 min, and the extraction power of 200 W. Based on the optimal extraction method of UAE, the total contents of ten main macamides and two main macaenes of Maca cultivated in twenty different areas of Tibet were analyzed by HPLC and UHPLC-ESI-Q-TOF-MS/MS. This study indicated that UAE was able to effectively extract macamides alkaloids from Maca hypocotyls. Quantitative analysis showed that geographical origins, not ecotypes, played a more important role on the accumulation of active macamides in Maca.

  16. Influence of High Shear Dispersion on the Production of Cellulose Nanofibers by Ultrasound-Assisted TEMPO-Oxidation of Kraft Pulp

    Directory of Open Access Journals (Sweden)

    Claude Daneault

    2012-09-01

    Full Text Available Cellulose nanofibers can be produced using a combination of TEMPO, sodium bromide (NaBr and sodium hypochlorite, and mechanical dispersion. Recently, this process has been the subject of intensive investigation. However, studies on the aspects of mechanical treatment of this process remain marginal. The main objective of this study is to evaluate the high shear dispersion parameters (e.g., consistency, stator-rotor gap, recirculation rate and pH and determine their influences on nanocellulose production using ultrasound-assisted TEMPO-oxidation of Kraft pulp. All nanofiber gels produced in this study exhibited rheological behaviors known as shear thinning. From all the dispersion parameters, the following conditions were identified as optimal: 0.042 mm stator-rotor gap, 200 mL/min recycle rate, dispersion pH of 7 and a feed consistency of 2%. High quality cellulose gel could be produced under these conditions. This finding is surely of great interest for the pulp and paper industry.

  17. Optimization of Ultrasound-assisted extraction of polyphenols, tannins and epigallocatechin gallate from barks of Stryphnodendron adstringens (Mart.) Coville bark extracts.

    Science.gov (United States)

    Sousa, Jordana N; Pedroso, Nathália B; Borges, Leonardo L; Oliveira, Gerlon A R; Paula, José R; Conceição, Edemilson C

    2014-04-01

    Stryphnodendron adstringens (Mar.) Coville is a native plant from Brazil, rich in phenolic compounds and used on popular medicine as a wound healing agent, in the treatment of gastric lesions and as antimicrobial. Ultrassound-assisted extraction (UAE) was applied to extraction of epigallocatechin gallate (EGCG), total polyphenols (TP) and total tannins (TT) content from barks of Stryphnodendron adstringens (Mar.) Coville. Several operating parameters, namely extraction time (min), liquid to solid ratio (mg/mL), ethanolic strength (%, v/v), were optimized using response surface methodology (RSM) with a Box-Behnken design. By using the desirability function approach, the optimum UAE conditions to obtain desirable extraction yields for all these metabolites simultaneously were found at the extraction time of 30 min, solid to liquid ratio of 4 mg/mL and ethanolic strength of 65. Under these conditions, the epigallocatechin gallate, total polyphenols and total tannins content were 0.31; 22.95 and 11.95 % (w/w), respectively. The results indicated that knowledge gained from this study should be helpful to further exploit and apply this resource and also showed the feasibility of ultrasound-assisted extraction for obtaining GEGC, TP and TT from barks of S. adstrigens.

  18. Assessment of parabens and ultraviolet filters in human placenta tissue by ultrasound-assisted extraction and ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Vela-Soria, F; Gallardo-Torres, M E; Ballesteros, O; Díaz, C; Pérez, J; Navalón, A; Fernández, M F; Olea, N

    2017-03-03

    Increasing concerns have been raised over recent decades about human exposure to Endocrine Disrupting Chemicals (EDCs), especially about their possible effects on embryo, foetus, newborn, and child. Parabens (PBs) and ultraviolet filters (UV-filters) are prevalent EDCs widely used as additives in cosmetics and personal care products (PCPs). The objective of this study was to determine the presence of four PBs and ten UV-filters in placental tissue samples using a novel analytical method based on ultrasound-assisted extraction (UAE) and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Multivariate optimization strategies were used to accurately optimize extraction and clean-up parameters. Limits of quantification ranged from 0.15 to 0.5μgkg -1 , and inter-day variability (evaluated as relative standard deviation) ranged from 3.6% to 14%. The method was validated using matrix-matched standard calibration followed by a recovery assay with spiked samples. Recovery percents ranged from 94.5% to 112%. The method was satisfactorily applied for the determination of the target compounds in human placental tissue samples collected at delivery from 15 randomly selected women. This new analytical procedure can provide information on foetal exposure to compounds, which has been little studied. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Determination of personal care products and hormones in leachate and groundwater from Polish MSW landfills by ultrasound-assisted emulsification microextraction and GC-MS.

    Science.gov (United States)

    Kapelewska, Justyna; Kotowska, Urszula; Wiśniewska, Katarzyna

    2016-01-01

    Determination of the endocrine disrupting compounds (EDCs) in leachate and groundwater samples from the landfill sites is very important because of the proven harmful effects of these compounds on human and animal organisms. A method combining ultrasound-assisted emulsification microextraction (USAEME) and gas chromatography-mass spectrometry (GC-MS) was developed for simultaneous determination of seven personal care products (PCPs): methylparaben (MP), ethylparaben (EP), propylparaben (PP), buthylparaben (BP), benzophenone (BPh), 3-(4-methylbenzylidene)camphor (4-MBC), N,N-diethyltoluamide (DEET), and two hormones: estrone (E1) and β-estradiol (E2) in landfill leachate and groundwater samples. The limit of detection (LOD)/limit of quantification (LOQ) values in landfill leachate and groundwater samples were in the range of 0.003-0.083/0.009-0.277 μg L(-1) and 0.001-0.015/0.002-0.049 μg L(-1), respectively. Quantitative recoveries and satisfactory precision were obtained. All studied compounds were found in the landfill leachates from Polish municipal solid waste (MSW) landfills; the concentrations were between 0.66 and 202.42 μg L(-1). The concentration of pollutants in groundwater samples was generally below 0.1 μg L(-1).

  20. Determination of cadmium and lead in mussels by electrothermal atomic absorption spectrometry using an ultrasound-assisted extraction method optimized by factorial design

    Energy Technology Data Exchange (ETDEWEB)

    Lavilla, I.; Capelo, J.L.; Bendicho, C. [Departamento de Quimica Analitica y Alimentaria, Universidad de Vigo, Facultad de Ciencias (Quimicas), As Lagoas - Marcosende s/n. E-36200 Vigo (Spain)

    1999-02-01

    A simple and rapid method is described for the quantitative extraction and determination of Cd and Pb in mussel tissue (Mytilus edulis). The method is based on the quantitative ultrasound-assisted extraction (i.e. sample mass at mg level) of the two metals using diluted nitric acid as extractant. The extraction procedure is carried out in autosampler cups of the graphite furnace (typically, less than 20 mg). A two-level full factorial design (2{sup 4}) was applied to optimize the variables influencing the ultrasound extraction process. These variables were: extraction time, ultrasound amplitude, nitric acid concentration and particle size. Optimization results showed that acid concentration and particle size were the more significant variables. Determination of Cd and Pb in extracts obtained after ultrasound treatment was carried out by Electrothermal Atomic Absorption Spectrometry. The method was validated by statistically comparing the metal contents found with the certified ones corresponding to the BCR 278 mussel tissue. No significant differences were observed for P= 0.05. LODs for Cd and Pb in mussel tissue were 0.019 and 0.37 {mu}g g{sup -1}. RSDs values (corresponding to between-batch precision for n= 5) were 2.2 and 6.7% for Cd and Pb, respectively. The method was applied to measure the contents of Cd and Pb in mussels used as pollution bioindicators from the Galician coast (Ria de Vigo, Spain). (orig.) With 2 figs., 9 tabs., 6 refs.

  1. Ultrasound-assisted solid-phase extraction coupled with photodiode-array and fluorescence detection for chemotaxonomy of isoflavone phytoestrogens in Trifolium L. (Clover) species.

    Science.gov (United States)

    Zgórka, Grazyna

    2009-04-01

    Detailed chemotaxonomic studies were undertaken to establish the qualitative profile and real amounts of the pharmacologically active isoflavone aglycones genistein, daidzein, formononetin, and biochanin A in aerial parts of thirteen Trifolium L. (clover) species, native to Poland. A newly elaborated micropreparative technique--SPE--on BakerBond octadecyl, cyclohexyl, and phenyl cartridges was used in combination with ultrasound-assisted extraction for isolation of isoflavone aglycones from hydrolyzed samples. The effectiveness of all three SPE sorbents in the purification of plant extracts was compared and very high recoveries (>96%) were documented for four isoflavones. Classical photodiode-array and very sensitive fluorescence detection, coupled with reversed-phase high-performance liquid chromatography (RP-HPLC), were employed to obtain the most reliable qualitative and quantitative results. Chemotaxonomic differences combined with flower color variability were demonstrated within thirteen clover species. Concentration levels of particular isoflavones in ten Trifolium species possessing flowers with white, pink, or purple-red corolla ranged from approximately 3 to approximately 3300 microg/g dry weight, while in three yellow flowering clovers (T. aureum, T. dubium, and T. campestre) isoflavone compounds have not been detected at all. RSD values, determined for intra- and inter-day precision of the quantitative results, were not higher than 6.2% and 7.1%, respectively.

  2. Double spike isotope dilution GC-ICP-MS for evaluation of mercury species transformation in real fish samples using ultrasound-assisted extraction.

    Science.gov (United States)

    Esteban-Fernández, Diego; Mirat, Manuela; de la Hinojosa, M Ignacia Martín; Alonso, J Ignacio García

    2012-08-29

    Sample preparation continues being a key factor to obtain fast and reliable quantification of Hg species. Assisted procedures enhance the efficiency and reduce the extraction time; however, collateral species transformations have been observed. Moreover, differential interconversions have been observed even between similar matrixes, which introduce an important uncertainty for real sample analysis. Trying to minimize Hg species transformations, we have tested a soft ultrasound-assisted extraction procedure. Species quantification and transformations have been evaluated using double spike isotope dilution analysis (IDA) together with gas chromatography inductively coupled plasma mass spectrometry (GC-ICP-MS) for a CRM material (Tort-2) and shark and swordfish muscle samples. Optimum extraction solution and sonication time led to quantitative extraction and accurate determination of MeHg and IHg in a short time, although different behaviors regarding species preservation were observed depending on the sample. Negligible species transformations were observed in the analysis of the CRM, while a small but significant demethylation factor was observed in the case of real samples. In comparison with other extraction procedures, species transformations became smaller, and fewer differences between fish species were found. Similar results were obtained for fresh and lyophilized samples of both fish samples, which permit one to analyze the fresh sample directly and save time in the sample preparation step. The high grade of species preservation and the affordability of the extraction procedure allow one to obtain accurate determinations even for routine laboratories using quantification techniques, which do not estimate species transformations.

  3. Optimization of Ultrasound-Assisted Extraction of Crude Oil from Winter Melon (Benincasa hispida Seed Using Response Surface Methodology and Evaluation of Its Antioxidant Activity, Total Phenolic Content and Fatty Acid Composition

    Directory of Open Access Journals (Sweden)

    Md. Zaidul Islam Sarker

    2012-10-01

    Full Text Available In the present study, ultrasound-assisted extraction of crude oil from winter melon seeds was investigated through response surface methodology (RSM. Process variables were power level (25–75%, temperature (45–55 °C and sonication time (20–40 min. It was found that all process variables have significant (p < 0.05 effects on the response variable. A central composite design (CCD was used to determine the optimum process conditions. Optimal conditions were identified as 65% power level, 52 °C temperature and 36 min sonication time for maximum crude yield (108.62 mg-extract/g-dried matter. The antioxidant activity, total phenolic content and fatty acid composition of extract obtained under optimized conditions were determined and compared with those of oil obtained by the Soxhlet method. It was found that crude extract yield (CEY of ultrasound-assisted extraction was lower than that of the Soxhlet method, whereas antioxidant activity and total phenolic content of the extract obtained by ultrasound-assisted extraction were clearly higher than those of the Soxhlet extract. Furthermore, both extracts were rich in unsaturated fatty acids. The major fatty acids of the both extracts were linoleic acid and oleic acid.

  4. Effect of irradiation power and time on ultrasound assisted co-precipitation of nanostructured CuO–ZnO–Al2O3 over HZSM-5 used for direct conversion of syngas to DME as a green fuel

    International Nuclear Information System (INIS)

    Allahyari, Somaiyeh; Haghighi, Mohammad; Ebadi, Amanollah; Hosseinzadeh, Shahin

    2014-01-01

    Graphical abstract: Nanostructured CuO–ZnO–Al 2 O 3 /HZSM-5 catalyst has been prepared by an ultrasound-assisted co-precipitation hybrid method. Effect of power and irradiation time have been studied by changing the time (30–45–60 min) and power of sonication (50–100–150 W) during the synthesis which lead to different physiochemical properties of the catalyst. The XRD, FESEM, EDX, FTIR and BET analyses exhibited smaller particles with higher surface area and less population of particle aggregates at longer and highly irradiated catalysts. Study on the performance of investigated catalysts in direct synthesis of DME from syngas showed ultrasound-assisted co-precipitated synthesized catalysts have superior reactivity and stability compared with non-sonicated catalyst. Among sonicated catalysts, with increasing power and time of irradiation, the catalyst represents higher activity and DME selectivity. - Highlights: • Synthesis of CuO–ZnO–Al 2 O 3 /HZSM-5 by ultrasound assisted co-precipitation method. • Significant changes in morphology and surface area after ultrasound irradiations. • Smaller dispersed particle aggregates in longer and more intense irradiated catalysts. • Improvement in reactivity and stability of the longer and more intense ultrasound irradiated CZAZ catalyst. - Abstract: Nanostructured CuO–ZnO–Al 2 O 3 /HZSM-5 catalyst has been prepared by an ultrasound-assisted co-precipitation hybrid method. The effect of irradiation power and irradiation time have been studied by changing time (30, 45, 60 min) and power of the sonication (50, 100, 150 W) during the synthesis which led to different physiochemical properties of the nanocatalyst. The XRD, FESEM, EDX, FTIR and BET analyses exhibited smaller particles with higher surface area and less population of particle aggregates at longer and highly irradiated nanocatalysts. The nanocatalyst irradiated at 150 W for 60 min (the longest irradiation time and the most intense power

  5. Thermotropic Ionic Liquid Crystals

    Science.gov (United States)

    Axenov, Kirill V.; Laschat, Sabine

    2011-01-01

    The last five years’ achievements in the synthesis and investigation of thermotropic ionic liquid crystals are reviewed. The present review describes the mesomorphic properties displayed by organic, as well as metal-containing ionic mesogens. In addition, a short overview on the ionic polymer and self-assembled liquid crystals is given. Potential and actual applications of ionic mesogens are also discussed. PMID:28879986

  6. Thermotropic Ionic Liquid Crystals.

    Science.gov (United States)

    Axenov, Kirill V; Laschat, Sabine

    2011-01-14

    The last five years' achievements in the synthesis and investigation of thermotropic ionic liquid crystals are reviewed. The present review describes the mesomorphic properties displayed by organic, as well as metal-containing ionic mesogens. In addition, a short overview on the ionic polymer and self-assembled liquid crystals is given. Potential and actual applications of ionic mesogens are also discussed.

  7. Thermotropic Ionic Liquid Crystals

    OpenAIRE

    Axenov, Kirill V.; Laschat, Sabine

    2011-01-01

    The last five years’ achievements in the synthesis and investigation of thermotropic ionic liquid crystals are reviewed. The present review describes the mesomorphic properties displayed by organic, as well as metal-containing ionic mesogens. In addition, a short overview on the ionic polymer and self-assembled liquid crystals is given. Potential and actual applications of ionic mesogens are also discussed.

  8. Quality assessment of trace Cd and Pb contaminants in Thai herbal medicines using ultrasound-assisted digestion prior to flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Watsaka Siriangkhawut

    2017-10-01

    Full Text Available A simple, efficient, and reliable ultrasound-assisted digestion (UAD procedure was used for sample preparation prior to quantitative determination of trace Cd and Pb contaminants in herbal medicines using flame atomic absorption spectrometry. The parameters influencing UAD such as the solvent system, sample mass, presonication time, sonication time, and digestion temperature were evaluated. The efficiency of the proposed UAD procedure was evaluated by comparing with conventional acid digestion (CAD procedure. Under the optimum conditions, linear calibration graphs in a range of 2–250 μg/L for Cd, and 50–1000 μg/L for Pb were obtained with detection limits of 0.56 μg/L and 10.7 μg/L for Cd and Pb, respectively. The limit of quantification for Cd and Pb were 1.87 μg/L and 40.3 μg/L, respectively. The repeatability for analysis of 10 μg/L for Cd and 100 μg/L for Pb was 2.3% and 2.6%, respectively. The accuracy of the proposed method was evaluated by rice flour certified reference materials. The proposed method was successfully applied for analysis of trace Cd and Pb in samples of various types of medicinal plant and traditional medicine consumed in Thailand. Most herbal medicine samples were not contaminated with Cd or Pb. The contaminant levels for both metals were still lower than the maximum permissible levels of elements in medicinal plant materials and finished herbal products sets by the Ministry of Public Health of Thailand. The exception was the high level of Cd contamination found in two samples of processed medicinal plants.

  9. Extraction of Natural Antioxidants from the Thelephora ganbajun Mushroom by an Ultrasound-Assisted Extraction Technique and Evaluation of Antiproliferative Activity of the Extract against Human Cancer Cells

    Directory of Open Access Journals (Sweden)

    Dong-Ping Xu

    2016-10-01

    Full Text Available The Thelephora ganbajun mushroom has been found to be a potential rich source of natural antioxidants. In this study, an ultrasound-assisted extraction (UAE technique together with GRAS (generally recognized as safe solvents (ethanol and water was used to maximize the extraction of antioxidants from Thelephora ganbajun. Five extraction parameters (ethanol concentration, solvent to solid ratio, extraction time, temperature and ultrasound power were investigated by single-factor experiments, and then a central composite rotatable design was employed to study interaction of three key extraction parameters. The optimum conditions were as follows: 57.38% ethanol, 70.15 mL/g solvent to solid ratio, 10.58 min extraction time, 40 °C extraction temperature and 500 W ultrasound power. Under the optimum conditions, the antioxidant activity obtained was 346.98 ± 12.19 µmol Trolox/g DW, in accordance with the predicted value of 344.67 µmol Trolox/g DW. Comparison of UAE with conventional maceration and Soxhlet extraction, the UAE method showed stronger extract efficiency in a shorter extraction time. These results showed that UAE was an effective technique to extract antioxidants from Thelephora ganbajun. Furthermore, the extracts obtained under the optimized conditions exhibited antiproliferative activities toward human lung (A549, breast (MCF-7, liver (HepG2 and colon (HT-29 cancer cells, especially for liver and lung cancer cells. In addition, rutin, 2-hydrocinnamic acid and epicatechin were identified in the extract, which might contribute to antioxidant and antiproliferative activities.

  10. Determination of fragrance allergens in indoor air by active sampling followed by ultrasound-assisted solvent extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lamas, J Pablo; Sanchez-Prado, Lucia; Garcia-Jares, Carmen; Llompart, Maria

    2010-03-19

    Fragrances are ubiquitous pollutants in the environment, present in the most of household products, air fresheners, insecticides and cosmetics. Commercial perfumes may contain hundreds of individual fragrance chemicals. In addition to the widespread use and exposure to fragranced products, many of the raw fragrance materials have limited available health and safety data. Because of their nature as artificial fragrances, inhalation should be considered as an important exposure pathway, especially in indoor environments. In this work, a very simple, fast, and sensitive methodology for the analysis of 24 fragrance allergens in indoor air is presented. Considered compounds include those regulated by the EU Directive, excluding limonene; methyl eugenol was also included due to its toxicity. The proposed methodology is based on the use of a very low amount of adsorbent to retain the target compounds, and the rapid ultrasound-assisted solvent extraction (UAE) using a very low volume of solvent which avoids further extract concentration. Quantification was performed by gas chromatography coupled to mass spectrometry (GC-MS). The influence of main factors involved in the UAE step (type of adsorbent and solvent, solvent volume and extraction time) was studied using an experimental design approach to account for possible factor interactions. Using the optimized procedure, 0.2 m(-3) air are sampled, analytes are retained on 25 mg Florisil, from which they are extracted by UAE (5 min) with 2 mL ethyl acetate. Linearity was demonstrated in a wide concentration range. Efficiency of the total sampling-extraction process was studied at several concentration levels (1, 5 and 125 microg m(-3)), obtaining quantitative recoveries, and good precision (RSD<10%). Method detection limits were < or =0.6 microg m(-3). Finally, the proposed method was applied to real samples collected in indoor environments in which several of the target compounds were determined. Copyright 2010 Elsevier B

  11. Ultrasound-assisted enzymatic hydrolysis for iodinated amino acid extraction from edible seaweed before reversed-phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Romarís-Hortas, Vanessa; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

    2013-09-27

    The combination of reverse phase high performance liquid chromatography (RP-HPLC) with inductively coupled plasma mass spectrometry (ICP-MS) was used for the determination of monoiodotyrosine (MIT) and diiodotyrosine (DIT) in edible seaweed. A sample pre-treatment based on ultrasound assisted enzymatic hydrolysis was optimized for the extraction of these iodinated amino acids. Pancreatin was selected as the most adequate type of enzyme, and parameters affecting the extraction efficiency (pH, temperature, mass of enzyme and extraction time) were evaluated by univariate approaches. In addition, extractable inorganic iodine (iodide) was also quantified by anion exchange high performance liquid chromatography (AE-HPLC) coupled with ICP-MS. The proposed procedure offered limits of detection of 1.1 and 4.3ngg(-1) for MIT and DIT, respectively. Total iodine contents in seaweed, as well as total iodine in enzymatic digests were measured by ICP-MS after microwave assisted alkaline digestion with tetramethylamonium hydroxide (TMAH) for total iodine assessment, and also by treating the pancreatin extracts (extractable total iodine assessment). The optimized procedure was successfully applied to five different types of edible seaweed. The highest total iodine content, and also the highest iodide levels, was found in the brown seaweed Kombu (6646±45μgg(-1)). Regarding iodinated amino acids, Nori (a red seaweed) was by far the one with the highest amount of both species (42±3 and 0.41±0.024μgg(-1) for MIT and DIT, respectively). In general, MIT concentrations were much higher than the amounts of DIT, which suggests that iodine from iodinated proteins in seaweed is most likely bound in the form of MIT residues. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Circulating ultrasound-assisted extraction, countercurrent chromatography, and liquid chromatography for the simultaneous extraction, isolation, and analysis of the constituents of Uncaria tomentosa.

    Science.gov (United States)

    Zhang, Yuchi; Liu, Chunming; Qi, Yanjuan; Li, Sainan; Pan, Yan; Li, Yuchun

    2015-04-03

    A hyphenated automated technique for the online extraction, isolation, analysis, and identification of natural organic compounds was established. Circulating ultrasound-assisted extraction (CUAE) was coupled with countercurrent chromatography (CCC), high performance liquid chromatography (HPLC), and a diode array detector (DAD). This approach was applied to the fractionation and purification of alkaloids from Uncaria tomentosa. A biphasic solvent system of chloroform-methanol-water (6:4:5, v:v:v) was used for the CUAE and CCC separation of compounds from 500 g of U. tomentosa. Two CUAE/CCC/HPLC/DAD modes were established. Either the upper aqueous phase or the lower organic phase of the solvent system could be used as the extraction solvent. The target compounds were extracted by CUAE, and the extract was pumped into a sample loop before being directly injected into the CCC column, or pre-purified using a flash chromatography column before injection. The target compounds were eluted using either the organic or aqueous phase of the solvent system and the fractions were monitored using a UV detector. The target fractions were collected by a sample loop via a six-port valve, and analyzed by HPLC/DAD for purity and structural identification. This system isolated of 8.2mg, 7.4 mg, and 12.9 mg of rhynchophylline, corynoxine, and corynoxine B with HPLC purities of 96.15%, 95.34%, and 95.49%, respectively via the first mode; and isolated 26.6 mg, 24.6 mg, and 45.3mg of rhynchophylline, corynoxine, and corynoxine B with a HPLC purities of 98.22%, 97.18%, and 97.93% via the second mode. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

  13. Extraction of Natural Antioxidants from the Thelephora ganbajun Mushroom by an Ultrasound-Assisted Extraction Technique and Evaluation of Antiproliferative Activity of the Extract against Human Cancer Cells

    Science.gov (United States)

    Xu, Dong-Ping; Zheng, Jie; Zhou, Yue; Li, Ya; Li, Sha; Li, Hua-Bin

    2016-01-01

    The Thelephora ganbajun mushroom has been found to be a potential rich source of natural antioxidants. In this study, an ultrasound-assisted extraction (UAE) technique together with GRAS (generally recognized as safe) solvents (ethanol and water) was used to maximize the extraction of antioxidants from Thelephora ganbajun. Five extraction parameters (ethanol concentration, solvent to solid ratio, extraction time, temperature and ultrasound power) were investigated by single-factor experiments, and then a central composite rotatable design was employed to study interaction of three key extraction parameters. The optimum conditions were as follows: 57.38% ethanol, 70.15 mL/g solvent to solid ratio, 10.58 min extraction time, 40 °C extraction temperature and 500 W ultrasound power. Under the optimum conditions, the antioxidant activity obtained was 346.98 ± 12.19 µmol Trolox/g DW, in accordance with the predicted value of 344.67 µmol Trolox/g DW. Comparison of UAE with conventional maceration and Soxhlet extraction, the UAE method showed stronger extract efficiency in a shorter extraction time. These results showed that UAE was an effective technique to extract antioxidants from Thelephora ganbajun. Furthermore, the extracts obtained under the optimized conditions exhibited antiproliferative activities toward human lung (A549), breast (MCF-7), liver (HepG2) and colon (HT-29) cancer cells, especially for liver and lung cancer cells. In addition, rutin, 2-hydrocinnamic acid and epicatechin were identified in the extract, which might contribute to antioxidant and antiproliferative activities. PMID:27706082

  14. A Retrospective Comparison of Ultrasound-Assisted Catheter-Directed Thrombolysis and Catheter-Directed Thrombolysis Alone for Treatment of Proximal Deep Vein Thrombosis

    Energy Technology Data Exchange (ETDEWEB)

    Tichelaar, Vladimir Y. I. G., E-mail: ynse.i.tichelaar@uit.no; Brodin, Ellen E.; Vik, Anders; Isaksen, Trond [UiT – The Arctic University of Norway, K. G. Jebsen – Thrombosis Research and Expertise Centre (TREC), Department of Clinical Medicine (Norway); Skjeldestad, Finn Egil [UiT – The Arctic University of Norway, Research Group Epidemiology of Chronic Diseases, Department of Community Medicine (Norway); Kumar, Satish; Trasti, Nora C.; Singh, Kulbir [University Hospital of North Norway, Department of Radiology (Norway); Hansen, John-Bjarne [UiT – The Arctic University of Norway, K. G. Jebsen – Thrombosis Research and Expertise Centre (TREC), Department of Clinical Medicine (Norway)

    2016-08-15

    BackgroundRecent studies have suggested that catheter-directed thrombolysis (CDT) reduces development of post-thrombotic syndrome (PTS). Ultrasound-assisted CDT (USCDT) might enhance the efficiency of thrombolysis. We aimed to compare USCDT with CDT on efficacy, safety, development of PTS, and quality of life after long-term follow-up.MethodsWe describe a retrospective case series of 94 consecutive patients admitted with iliofemoral or more proximal deep vein thrombosis (DVT) to the University Hospital from 2002 to 2011, treated either with CDT or USCDT. Scheduled follow-up visits took place between April 2013 and January 2014. Venography measured the degree of residual luminal obstruction of the affected veins. Each patient completed the Short Form 36-item health survey assessment and the Venous Insufficiency Epidemiological and Economic Study-Quality of Life/Symptoms questionnaires. PTS was assessed using the Villalta scale.ResultsRisk factors of DVT were equally distributed between groups. In the USCDT group, we observed a significant decline in the duration of thrombolytic treatment (<48 h: 27 vs. 10 %), shortened hospital stay (median 6.0 days (IQR 5.0–9.0) vs. 8.0 (IQR 5.8–12.0)), and less implantation of (intravenous) stents (30 vs. 55 %). There was no difference in patency (76 vs. 79 % fully patent), prevalence of PTS (52 vs. 55 %), or quality of life between groups after long-term follow-up (median 65 months, range: 15–141).ConclusionsIn this observational study, USCDT was associated with shortened treatment duration, shorter hospital stay, and less intravenous stenting, compared to CDT alone without affecting the long-term prevalence of PTS or quality of life.

  15. Evaluation, prediction and optimization the ultrasound-assisted extraction method using response surface methodology: antioxidant and biological properties of Stachys parviflora L.

    Directory of Open Access Journals (Sweden)

    Davoud Salarbashi

    2016-05-01

    Full Text Available Objective(s:To optimize the extraction method using response surface methodology, extract the phenolic compounds, and identify the antioxidant and biological properties of Stachys parviflora L.  extracts. Materials and Methods: Maceration and ultrasound-assisted extraction (UAE (4, 7, 10 min treatment time, 40, 70, 100 % high-intensity and 60, 80, 100 % (v v-1 methanol purity were applied to obtain the extracts. SEM was conducted to provide the microstructure of the extracted plant. MICs (colorimetric assay, MFCs (colony diameter, total phenolic content, total flavonoid content, radical scavenging capacity and extraction efficiency were determined. HPLC analysis was applied to measure the existent phenolic compounds. Results: A quadratic model (4 min treatment time, 74.5 % high-intensity and 74.2 % solvent purity was suggested as the best (TPC: 20.89 mg GAE g-1 d.m., TFC: 6.22 mg QEs g-1 d.m., DPPH IC50: 21.86 µg ml-1 and EE: 113.65 mg g-1 d.m. UAE extraction model. The optimized UAE extract was generally more effective against Gram-positive microorganisms (MIC: 10-20; MBC: 10-40 (mg ml-1 than Gram-negative ones (MIC: 40; MBC: >40 (mg ml-1. Moreover, it (MGI: 2.32-100 % revealed more anti-mold activity than maceration (MGI: Conclusion: RSM optimization was successfully applied for UAE from S. parviflora. The considerable antioxidant and biological properties were attributed to the phenolic compounds.

  16. Simultaneous ultrasound-assisted ternary adsorption of dyes onto copper-doped zinc sulfide nanoparticles loaded on activated carbon: optimization by response surface methodology.

    Science.gov (United States)

    Asfaram, Arash; Ghaedi, Mehrorang; Hajati, Shaaker; Goudarzi, Alireza; Bazrafshan, Ali Akbar

    2015-06-15

    The simultaneous and competitive ultrasound-assisted removal of Auramine-O (AO), Erythrosine (Er) and Methylene Blue (MB) from aqueous solutions were rapidly performed onto copper-doped zinc sulfide nanoparticles loaded on activated carbon (ZnS:Cu-NP-AC). ZnS:Cu nanoparticles were studied by FESEM, XRD and TEM. First, the effect of pH was optimized in a one-at-a-time procedure. Then the dependency of dyes removal percentage in their ternary solution on the level and magnitude of variables such as sonication time, initial dyes concentrations and adsorbent dosage was fully investigated and optimized by central composite design (CCD) under response surface methodology (RSM) as well as by regarding desirability function (DF) as a good and general criterion. The good agreement found between experimental and predicted values supports and confirms the suitability of the present model to predict adsorption state. The applied ultrasound strongly enhanced mass transfer process and subsequently performance. Hence, a small amount of the adsorbent (0.04 g) was capable to remove high percentage of dyes, i.e. 100%, 99.6% and 100% for MB, AO and Er, respectively, in very short time (2.5 min). The experimental equilibrium data fitting to Langmuir, Freundlich, Temkin and Dubinin-Radushkevich models showed that the Langmuir model applies well for the evaluation and description of the actual behavior of adsorption. The small amount of proposed adsorbent (0.015 g) was applicable for successful removal of dyes (RE>99.0%) in short time (2.5 min) with high adsorption capacity in single component system (123.5 mg g(-1) for MB, 123 mg g(-1) for AO and 84.5 mg g(-1) for Er). Kinetics evaluation of experiments at various time intervals reveals that adsorption processes can be well predicated and fitted by pseudo-second-order and Elovich models. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Ultrasound assisted combined molecularly imprinted polymer for selective extraction of nicotinamide in human urine and milk samples: Spectrophotometric determination and optimization study.

    Science.gov (United States)

    Asfaram, Arash; Ghaedi, Mehrorang; Dashtian, Kheibar

    2017-01-01

    Ultrasound-assisted dispersive solid phase microextraction followed by UV-vis spectrophotometer (UA-DSPME-UV-vis) was designed for extraction and preconcentration of nicotinamide (vitamin B 3 ) by HKUST-1 metal organic framework (MOF) based molecularly imprinted polymer (MIP). This new material was characterized by FTIR and FE-SEM techniques. The preliminary Plackett-Burman design was used for screening and subsequently the central composite design justifies significant terms and possible construction of mathematical equation which give the individual and cooperative contribution of variables like HKUST-1-MOF-NA-MIP mass, sonication time, temperature, eluent volume, pH and vortex time. Accordingly the optimum condition was set as: 2.0mg HKUST-1-MOF-NA-MIP, 200μL eluent and 5.0min sonication time in center points other variables were determined as the best conditions to reach the maximum recovery of the analyte. The UA-DSPME-UV-vis method performances like excellent linearity (LR), limits of detection (LOD), limits of quantification of 10-5000μgL -1 with R 2 of 0.99, LOD (1.96ngmL -1 ), LOQ (6.53μgL -1 ), respectively show successful and accurate applicability of the present method for monitoring analytes with within- and between-day precision of 0.96-3.38%. The average absolute recoveries of the nicotinamide extracted from the urine, milk and water samples were 95.85-101.27%. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Almeida, Jorge S.; Anunciação, Taiana A.; Brandão, Geovani C.; Dantas, Alailson F.; Lemos, Valfredo A.; Teixeira, Leonardo S. G.

    2015-05-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO3 gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box-Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L- 1 HNO3 as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg- 1. Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method.

  19. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Jorge S.; Anunciação, Taiana A. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Brandão, Geovani C. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); INCT de Energia e Ambiente, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Dantas, Alailson F. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Lemos, Valfredo A. [Laboratório de Química Analítica (LQA), Universidade Estadual do Sudoeste da Bahia, Campus de Jequié, Jequié, Bahia 45506-191 (Brazil); and others

    2015-05-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO{sub 3} gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box–Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L{sup −1} HNO{sub 3} as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg{sup −1}. Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method. - Highlights: • The determination of cadmium in vegetable oils was developed using UA-SDME. • HR-CS ET-AAS was employed as a detection technique with direct drop sampling. • The procedure allowed for a reduction in the consumption of reagents and

  20. Enhancement of thermal and mechanical properties of poly(MMA-co-BA)/Cloisite 30B nanocomposites by ultrasound-assisted in-situ emulsion polymerization.

    Science.gov (United States)

    Sharma, Sachin; Kumar Poddar, Maneesh; Moholkar, Vijayanand S

    2017-05-01

    This study reports synthesis and characterization of poly(MMA-co-BA)/Cloisite 30B (organo-modified montmorillonite clay) nanocomposites by ultrasound-assisted in-situ emulsion polymerization. Copolymers have been synthesized with MMA:BA monomer ratio of 4:1, and varying clay loading (1-5wt% monomer). The poly(MMA-co-BA)/Cloisite 30B nanocomposites have been characterized for their thermal and mechanical properties. Ultrasonically synthesized nanocomposites have been revealed to possess higher thermal degradation resistance and mechanical strength than the nanocomposites synthesized using conventional techniques. These properties, however, show an optimum (or maxima) with clay loading. The maximum values of thermal and mechanical properties of the nanocomposites with optimum clay loading are as follows. Thermal degradation temperatures: T 10% =320°C (4wt%), T 50 =373°C (4wt%), maximum degradation temperature=384°C (4wt%); glass transition temperature=64.8°C (4wt%); tensile strength=20MPa (2wt%), Young's modulus=1.31GPa (2wt%), Percentage elongation=17.5% (1wt%). Enhanced properties of poly(MMA-co-BA)/Cloisite 30B nanocomposites are attributed to effective exfoliation and dispersion of clay nanoparticles in copolymer matrix due to intense micro-convection induced by ultrasound and cavitation. Clay platelets help in effective heat absorption with maximum surface interaction/adhesion that results in increased thermal resistivity of nanocomposites. Hindered motion of the copolymer chains due to clay platelets results in enhancement of tensile strength and Young's modulus of nanocomposite. Rheological (liquid) study of the nanocomposites reveals that nanocomposites have higher yield stress and infinite shear viscosity than neat copolymer. Nonetheless, nanocomposites still display shear thinning behavior - which is typical of the neat copolymer. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Comparison of Ultrasound-Assisted Headspace Solid-Phase Microextraction and Hydrodistillation for the Identification of Major Constituents in Two Species of Hypericum.

    Science.gov (United States)

    Ghiasvand, Alireza; Shadabi, Shahriar; Hajipour, Somayeh; Nasirian, Afagh; Borzouei, Mohammad; Hassani-Moghadam, Esfandyar; Hashemi, Payman

    2016-02-01

    Ultrasound-assisted headspace solid-phase microextraction (UA-HS-SPME) and hydrodistillation (HD) methods, coupled to gas chromatography-mass spectrometry (GC-MS), were used for the extraction and analysis of volatile compounds from Hypericum perforatum and Hypericum scabrum collected from two different sites in Iran. In the UA-HS-SPME method, various experimental parameters such as the type of fiber coating, sonication time, extraction time, extraction temperature and desorption time were investigated. The highest extraction efficiency was achieved by a 100-µm polydimethylsiloxane (PDMS) fiber. Consequently, 36 compounds were identified in H. perforatum and H. scabrum samples, using the UA-HS-SPME-GC-MS method, of which 14 were the same in both species. On the other hand, 57 compounds of these species were identified by the HD-GC-MS method, of which 21 were the same. The predominant constituents identified using the UA-HS-SPME method in H. perforatum included β-caryophyllene, α-pinene, γ-cadinene, α-selinene, germacrene-D, limonene and myrcene, and in H. scabrum were α-pinene, nonane, β-pinene and limonene. The common constituents identified by the HD-GC-MS method for H. perforatum involved germacrene-D, limonene, β-caryophyllene, α-pinene, β-pinene and germacrene-B, and for H. scabrum were α-pinene, β-pinene, germacrene-D, nonane, limonene and γ-cadinene. The results about the main constituents of the examined species correspond to the findings of other researchers. Additionally, comparing UA-HS-SPME-GC-MS and HD-GC-MS methods showed that the UA-HS-SPME-GC-MS method is much faster and simpler, and it requires much less sample size and lower temperature. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  2. Determination of parabens in human urine by optimal ultrasound-assisted emulsification microextraction and on-line acetylation gas chromatography-mass spectrometry.

    Science.gov (United States)

    Hui-Ting, Zhou; Ding, Erica M C; Ding, Wang-Hsien

    2017-07-15

    An effective and solvent-less method for the rapid determination of four commonly detected parabens (methyl-, ethyl-, propyl- and butyl-) in human urine samples is described. This method employed ultrasound-assisted emulsification microextraction (USAEME) before identification and quantitation of the parabens via on-line acetylation gas chromatography-mass spectrometry (GC-MS). Urine samples were enzymatically de-conjugated with β-glucuronidase and then extracted by an optimal USAEME procedure for the measurement of total concentrations of target analytes. The optimal USAEME parameters for one mL of urine sample (containing 0.1-g of sodium chloride), according to the Box-Behnken design method, are thus described: extractant of 200-μL of ethyl acetate, and ultrasonication for 1.0min and centrifugation at 7000rpm (3min). The supernatant was collected and evaporated until dry. Then the residue was re-dissolved in methanol (100-μL), and the extract was subjected to on-line acetylation GC-MS analysis. The limits of quantitation (LOQs) were less than 0.06ng/mL. Precisions for both intra- and inter-day analysis were calculated, and were less than 8%. Mean extraction recovery (known as trueness) was between 83 and 101% on three concentration levels. In human urine, the total concentrations of the four selected parabens, according to preliminary results, range from 0.3 to 124.5ng/mL for male, and from 27.2 to 246.3ng/mL for female. Female urine samples showed higher concentrations for the target parabens, which may indicate higher exposure due to lifestyle. This method permits accurate and high-throughput analysis of parabens for epidemiological studies. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Ultrasound-assisted hydrolysis of conjugated parabens in human urine and their determination by UPLC-MS/MS and UPLC-HRMS.

    Science.gov (United States)

    Schlittenbauer, Linda; Seiwert, Bettina; Reemtsma, Thorsten

    2016-02-01

    Parabens are preservatives widely used in personal care products, pharmaceutical formulations as well as in food, and they are considered endocrine disruptors. For application in biomonitoring studies we developed a method for the determination of eight parabens from human urine. Sample preparation was enhanced and simplified by the combination of ultrasound-assisted enzymatic hydrolysis of conjugates (glucuronide and sulfate) followed by an extraction-free cleanup step. Quantification, using deuterated parabens as internal standards, was performed by ultrahigh-performance liquid chromatography coupled to either triple-quadrupole (UPLC-QqQ) or time-of-flight (UPLC-QqTOF) mass spectrometry. Full chromatographic separation of three butyl paraben isomers was achieved. Limits of quantification for both mass analyzers ranged from 0.1 to 0.5 μg/L for methyl, ethyl, n-/isopropyl, n-/isobutyl, and benzyl paraben in 200 μL of urine sample. The method was tested for applicability and showed high precision (intra- and interday 0.9-14.5%) as well as high accuracy (relative recovery 95-132%). A total of 39 urine samples were analyzed by both mass analyzers. The results agreed well, with a trend to higher deviation at low concentrations (less than 10 μg/L). Methyl, ethyl, and n-propyl paraben were detected most frequently (in more than 87% of the samples) with median concentrations ranging from 0.8 to 16.6 μg/L. Female urine showed higher median concentrations for all parabens, which may indicate higher exposure due to lifestyle. This method permits accurate and high-throughput analysis of parabens for epidemiological studies. Further, the UPLC-QqTOF approach provides additional information on human exposure to other compounds by post-acquisition analysis.

  4. Studies on electrical double layer capacitor with a low-viscosity ionic ...

    Indian Academy of Sciences (India)

    1Present address: Center for Autonomous Solar Power (CASP), Binghamton University, State University of New York,. Binghamton, NY 13902, USA. MS received 4 October 2011; revised 22 ... Recently, some ionic liquids based EDLCs are reported with different car- bon electrodes (Lewandowski and Galinski 2004; Xu et ...

  5. A novel solution configuration on liquid-based endometrial cytology.

    Directory of Open Access Journals (Sweden)

    Shulan Lv

    Full Text Available Early detection and diagnosis of endometrial carcinoma and precancerous change would undoubtedly become the most alluring part for researchers. With the emergence of endometrial brush samplers, a new upsurge in endometrial cytology is in the making. But endometrial specimens obtained by the endometrial brush samplers require special preservation solution. The objective of this study is to develop a new kind of endometrial-cell preservation solution and to test the availability compared with a patented liquid-based cell preservation solution.In this controlled study, we had 5 endometrial cases collected with Li Brush from the First Affiliated Hospital of Xi'an Jiaotong University (09/2016 to 12/2016. The samples of each case were collected 2 times separately and perserved in different perservation solutions. One was a kind of novel endometrial cell preservation solution and the other was a kind of patented liquid-based cell (LBC preservation solution. The endometrial cells were smeared on slides by using the ZP-C automated slide preparation system and stained with Papanicolaou stain. A semi-quantitative scoring system was used to analyze the quality of slides. Statistical analysis was performed using the Wilcoxon signed rank test on the SPSS program (SPSS 18.0. In all LBC preparations, endometrial cells from the novel endometrial cells preservation solution had more cell quantity, less red blood cell fragments, and the background was cleaner compared with control group. Although the novel endometrial-cell preservation solution showed cellularity and absence of blood and debris expressed by no statistically significant differences (p = 0.063 and 0.102 respectively. The preservation period of the two kinds of liquids was equivalent.The novel endometrial-cell preservation solution is superior to the liquid-base cell preservation solution for cervical cells, with clear background, diagnostic cells and low cost.

  6. Utility of ultrasound assisted-cloud point extraction and spectophotometry as a preconcentration and determination tool for the sensitive quantification of mercury species in fish samples

    Science.gov (United States)

    Altunay, Nail

    2018-01-01

    The current study reports, for the first time, the development of a new analytical method employing ultrasound assisted-cloud point extraction (UA-CPE) for the extraction of CH3Hg+ and Hg2 + species from fish samples. Detection and quantification of mercury species were performed at 550 nm by spectrophotometry. The analytical variables affecting complex formation and extraction efficiency were extensively evaluated and optimized by univariate method. Due to behave 14-fold more sensitive and selective of thiophene 2,5-dicarboxylic acid (H2TDC) to Hg2 + ions than CH3Hg+ in presence of mixed surfactant, Tween 20 and SDS at pH 5.0, the amounts of free Hg2 + and total Hg were spectrophotometrically established at 550 nm by monitoring Hg2 + in the pretreated- and extracted-fish samples in ultrasonic bath to speed up extraction using diluted acid mixture (1:1:1, v/v, 4 mol L- 1 HNO3, 4 mol L- 1 HCl, and 0.5 mol L- 1 H2O2), before and after pre-oxidation with permanganate in acidic media. The amount of CH3Hg+ was calculated from difference between total Hg and Hg2 + amounts. The UA-CPE method showed to be suitable for the extraction and determination of mercury species in certified reference materials. The results were in a good agreement (with Student's t-test at 95% confidence limit) with the certified values, and the relative standard deviation was lower than 3.2%. The limits of detection have been 0.27 and 1.20 μg L- 1, for Hg2 + from aqueous calibration solutions and matrix-matched calibration solutions spiked before digestion, respectively, while it is 2.43 μg L- 1 for CH3Hg+ from matrix-matched calibration solutions. A significant matrix effect was not observed from comparison of slopes of both calibration curves, so as to represent the sample matrix. The method was applied to fish samples for speciation analysis of Hg2 + and CH3Hg+. In terms of speciation, while total Hg is detected in range of 2.42-32.08 μg kg- 1, the distribution of mercury in fish were in

  7. Determination of gardenia yellow colorants in soft drink, pastry, instant noodles with ultrasound-assisted extraction by high performance liquid chromatography-electrospray ionization tandem mass spectrum.

    Science.gov (United States)

    Zhou, Wei-E; Zhang, Yuan; Li, Yang; Ling, Yun; Li, Hong-Na; Li, Shao-Hui; Jiang, Shou-Jun; Ren, Zhi-Qin; Huang, Zhi-Qiang; Zhang, Feng

    2016-05-13

    A novel, rapid and simple analytical method was developed for the quantitative determination of crocin, crocetin and geniposide in soft drink, pastry and instant noodles. The solid samples were relatively homogenized into powders and fragments. The gardenia yellow colorants were successively extracted with methanol using ultrasound-assisted extraction. The analytes were quantitatively measured in the extracts by liquid chromatography coupled with electrospray ionization tandem mass spectrometry. High correlation coefficients (r(2)>0.995) of crocin, crocetin and geniposide were obtained within their linear ranges respectively (50-1000ng/mL, 50-1000ng/mL, 15-240ng/mL) by external standard method. The limits of detection (LODs) were 0.02μg/g for crocin, 0.01μg/g for crocetin and 0.002μg/g for geniposide. And the limits of quantitation (LOQs) were in the ranges of 0.05-0.45μg/g for crocin, and in the ranges of 0.042-0.32μg/g for crocetin, and in the ranges of 0.02-0.15μg/g for geniposide in soft drink, pastry and instant noodles samples. The average recoveries of crocin, crocetin and geniposide ranged from 81.3% to 117.6% in soft drink, pastry and instant noodles. The intra- and inter-day precisions were respectively in the range of 1.3-4.8% and 1.7-11.8% in soft drink, pastry and instant noodle. The developed methods were successfully validated and applied to the soft drink, pastry, and instant noodles collected from the located market in Beijing from China. Crocin, crocetin and geniposide were detected in the collected samples. The average concentrations ranged from 0.84 to 4.20mg/g for crocin, and from 0.62 to 3.11mg/g for crocetin, and from 0.18 to 0.79mg/g for gardenia in various food samples. The method can provide evidences for government to determine gardenia yellow pigments and geniposide in food. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Thermotropic Ionic Liquid Crystals

    Directory of Open Access Journals (Sweden)

    Sabine Laschat

    2011-01-01

    Full Text Available The last five years’ achievements in the synthesis and investigation of thermotropic ionic liquid crystals are reviewed. The present review describes the mesomorphic properties displayed by organic, as well as metal-containing ionic mesogens. In addition, a short overview on the ionic polymer and self-assembled liquid crystals is given. Potential and actual applications of ionic mesogens are also discussed.

  9. Newly developed liquid-based cytology. TACAS™: cytological appearance and HPV testing using liquid-based sample.

    Science.gov (United States)

    Kubushiro, Kaneyuki; Taoka, Hideki; Sakurai, Nobuyuki; Yamamoto, Yasuhiro; Kurasaki, Akiko; Asakawa, Yasuyuki; Iwahara, Minoru; Takahashi, Kei

    2011-09-01

    Cell profiles determined by the thin-layer advanced cytology assay system (TACAS™), a liquid-based cytology technique newly developed in Japan, were analyzed in this study. Hybrid capture 2 (HC-2) was also performed using the liquid-based samples prepared by TACAS to ascertain its ability to detect human papillomavirus (HPV). Cell collection samples from uterine cervix were obtained from 359 patients and examined cytologically. A HC-2 assay for HPV was carried out in the cell specimens. All specimens were found to show background factors such as leukocytes. After excluding the 5 unsatisfactory cases from the total 354 cases, 82 cases (23.2%) were positive and 272 cases (76.8%) were negative for HPV. Cell specimens from 30 HPV-positive cases and 166 HPV-negative cases were subjected to 4 weeks of preservation at room temperature. Then, when subsequently re-assayed, 28 cases (93.3%) in the former group were found to be HPV positive and 164 cases (98.8%) in the latter group were found to be HPV negative. These results supported the excellent reproducibility of TACAS for HPV testing. A reasonable inference from the foregoing analysis is that TACAS may be distinguished from other liquid-based cytological approaches, such as ThinPrep and SurePath, in that it can retain the cell backgrounds. Furthermore, this study raises the possibility that cell specimens prepared using TACAS could be preserved for at least 4 weeks prior to carrying out a HC-2 assay for HPV.

  10. Ionic Liquid-Liquid Chromatography: A New General Purpose Separation Methodology.

    Science.gov (United States)

    Brown, Leslie; Earle, Martyn J; Gîlea, Manuela A; Plechkova, Natalia V; Seddon, Kenneth R

    2017-08-10

    Ionic liquids can form biphasic solvent systems with many organic solvents and water, and these solvent systems can be used in liquid-liquid separations and countercurrent chromatography. The wide range of ionic liquids that can by synthesised, with specifically tailored properties, represents a new philosophy for the separation of organic, inorganic and bio-based materials. A customised countercurrent chromatograph has been designed and constructed specifically to allow the more viscous character of ionic liquid-based solvent systems to be used in a wide variety of separations (including transition metal salts, arenes, alkenes, alkanes, bio-oils and sugars).

  11. 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.

  12. Determining heterocyclic aromatic amines in aqueous samples: A novel dispersive liquid-liquid micro-extraction method based on solidification of floating organic drop and ultrasound assisted back extraction followed by UPLC-MS/MS.

    Science.gov (United States)

    Canales, Romina; Guiñez, María; Bazán, Cristian; Reta, Mario; Cerutti, Soledad

    2017-11-01

    A novel dispersive liquid-liquid microextraction based on solidification of floating organic droplet combined with ultrasound assisted back extraction for the determination of four heterocyclic aromatic amines in natural water samples prior ultra high-performance liquid chromatography-tandem mass spectrometry was developed. The analytes were extracted from the water samples by a dispersive liquid-liquid microextraction procedure based on solidification of floating organic drop, which was performed by a mixture composed by a less dense than water extraction solvent, 1-undecanol, and a dispersive solvent, methanol. After that, a novel ultrasound assisted back extraction step was performed in order to make the clean-up/enrichment procedure compatible with the detection requirements. Under optimum conditions, linearity ranged from 2.2 to 50ngmL -1 , with enrichment factors from 130 to 136-folds. Thus limits of detection between 0.7 and 2.9ngmL -1 were obtained. Precision of the method was evaluated in terms of repeatability, relative standard deviations varied from 4.3% to 6.7%. Relative recoveries ranged from 92% to 106% for all analytes. The satisfactory performance demonstrated that the proposed methodology has a strong potential for application in the multi-residue analysis of heterocyclic aromatic amines present in complex environmental matrices. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. IONIC LIQUIDS MATERIAL AS MODERN CONTEXT OF CHEMISTRY IN SCHOOL

    Directory of Open Access Journals (Sweden)

    Hernani Hernani

    2016-04-01

    Full Text Available One way to improve students’ chemistry literacy which is demanded in the modernization of modern technology-based chemistry learning is by studying ionic liquids. Low level of scientific literacy of students in Indonesia as revealed in the PISA in 2012 was the main reason of the research. Ionic liquids-based technology are necessary to be applied as a context for learning chemistry because: (1 the attention of the scientific an technology community in the use of ionic liquids as a new generation of green solvent, electrolyte material and fluidic engineering in recent years becomes larger, in line with the strong demands of the industry for the provision of new materials that are reliable, safe, and friendly for various purposes; (2 scientific explanations related to the context of the ionic liquid contains a lot of facts, concepts, principles, laws, models and theories can be used to reinforce the learning content as a media to develop thinking skill (process/competence as demanded by PISA; (3 The modern technology-based ionic liquid can also be used as a discourse to strengthen scientific attitude. The process of synthesis of ionic liquid involves fairly simple organic reagents, so it deserves to be included in the chemistry subject in school.

  14. Jet-noise reduction through liquid-base foam injection.

    Science.gov (United States)

    Manson, L.; Burge, H. L.

    1971-01-01

    An experimental investigation has been made of the sound-absorbing properties of liquid-base foams and of their ability to reduce jet noise. Protein, detergent, and polymer foaming agents were used in water solutions. A method of foam generation was developed to permit systematic variation of the foam density. The investigation included measurements of sound-absorption coefficents for both plane normal incidence waves and diffuse sound fields. The intrinsic acoustic properties of foam, e.g., the characteristic impedance and the propagation constant, were also determined. The sound emitted by a 1-in.-diam cold nitrogen jet was measured for subsonic (300 m/sec) and supersonic (422 m/sec) jets, with and without foam injection. Noise reductions up to 10 PNdB were measured.

  15. Research progress of SO2 removal from flue gas by functionalized ionic liquids

    Directory of Open Access Journals (Sweden)

    Xinle SHI

    2017-02-01

    Full Text Available Functionalized ionic liquids are receiving increasing attention in the field of flue gas desulfurization due to its unique physical and chemical properties. Research progress on the field of SO2 removal by ionic liquids (ILs including guanidinium-based, amines-based and ether-based ILs is summarized. Industrial application of polymerization ILs and loaded ILs to desulfurization is reviewed. Relevant suggestions on industrial application of ionic liquids based on fundamental research are put forward. The first thing is to develop functional ionic liquid for desulfurization,and thus investigate and propose its desulfurization mechanism and model; the second is to carry out the research work on immobilized ionic liquid, and explore its recycling properties, thus prolonging its service life.

  16. Electrochemical functionalization of glassy carbon electrode by reduction of diazonium cations in protic ionic liquid

    International Nuclear Information System (INIS)

    Shul, Galyna; Ruiz, Carlos Alberto Castro; Rochefort, Dominic; Brooksby, Paula A.; Bélanger, Daniel

    2013-01-01

    Protic ionic liquid based on 2-methoxypyridine and trifluoroacetic acid was used as electrolyte for the functionalization of a glassy carbon electrode surface by electrochemical reduction of in situ generated 4-chlorobenzene diazonium and 4-nitrobenzene diazonium cations. The diazonium cations were synthesized in an electrochemical cell by reaction of the corresponding amines with NaNO 2 dissolved in protic ionic liquid. The resulting electrografted organic layers exhibit similar properties to those layers obtained by the derivatization from isolated diazonium salts dissolved in protic ionic liquid. Functionalized glassy carbon electrode surfaces were characterized by cyclic voltammetry, Fourier transform infrared and X-ray photoelectron spectroscopies. Atomic force microscopy thickness measurements revealed that, in our experimental conditions, the use of protic ionic liquid led to the formation of film with a thickness of about 1.5 nm. It is also demonstrated that the nitrobenzene chemisorbed on glassy carbon electrode or dissolved in protic ionic liquid undergoes electrochemical conversion to hydroxyaminobenzene

  17. Radiation stability of diglycolamide functionalized calix[4]arenes in ionic liquid: Solvent extraction, EPR and GC–MS studies

    NARCIS (Netherlands)

    Sengupta, A; Mohapatra, P.K.; Patil, A.B.; Kadam, R.M.; Verboom, Willem

    2016-01-01

    Ionic liquid-based solvent systems containing diglycolamide-functionalized calix[4]arenes (C4DGAs) are efficient for actinide ion extraction from nitric acid feeds. Therefore, the radiolytic stability of three C4DGAs (wide-rim, narrow-rim and both side DGA-functionalized calix[4]arenes) and TODGA

  18. Novel developments in hydrogen storage, hydrogen activation and ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    Doroodian, Amir

    2010-12-03

    This dissertation is divided into three chapters. Recently, metal-free hydrogen activation using phosphorous compounds has been reported in science magazine. We have investigated the interaction between hydrogen and phosphorous compounds in presence of strong Lewis acids (chapter one). A new generation of metal-free hydrogen activation, using amines and strong Lewis acids with sterically demanding nature, was already developed in our group. Shortage of high storage capacity using large substitution to improve sterical effect led us to explore the amine borane derivatives, which are explained in chapter two. Due to the high storage capacity of hydrogen in aminoborane derivatives, we have explored these materials to extend hydrogen release. These compounds store hydrogen as proton and hydride on adjacent atoms or ions. These investigations resulted in developing hydrogen storage based on ionic liquids containing methyl guanidinium cation. Then we have continued to develop ionic liquids based on methyl guanidinium cation with different anions, such as tetrafluoro borate (chapter three). We have replaced these anions with transition metal anions to investigate hydrogen bonding and catalytic activity of ionic liquids. This chapter illustrates the world of ionic liquid as a green solvent for organic, inorganic and catalytic reactions and combines the concept of catalysts and solvents based on ionic liquids. The catalytic activity is investigated particularly with respect to the interaction with CO{sub 2}. (orig.)

  19. Pysico-chemical properties of hydrophobic ionic liquids containing1-octylpyridinium, 1-octyl-2-methylpyridinium or1-octyl-4-methylpyridinium cations

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-09-15

    This paper reports synthesis of some ionic liquids based on cations 1-octylpyridinium, 1-octyl-2-methylpyridinium or 1-octyl-4-methylpyridinium and anions dicyanamide [N(CN)2]-, bis(trifluoromethylsulfonyl)imide [Tf2N]-, bis(pentafluoroethylsulfonyl)imide [BETI]-, trifluoromethyl sulfonate [TfO]-, nonafluorobutyl sulfonate [NfO]-, tetrafluoroborate [BF4]-, trifluorophenylborate [BF3Ph]- or hexafluoroarsenate [AsF6]-. Melting points, decomposition temperatures, densities, mutual solubilities with water, and viscosities have been measured. Unlike similar ionic liquids containing imidazolium cations, pyridinium ionic liquids studied here are nearly immiscible in water. Viscosities are similar and water content is slightly lower than those for ionic liquids containing imidazolium cations.

  20. Liquid-based cervical cytology in the United Kingdom and South Africa

    African Journals Online (AJOL)

    2012-02-01

    Feb 1, 2012 ... blood or mucus, which obscure the sample. Women with inadequate test results are required to attend for a repeat test, which is inconvenient and may cause anxiety.6. What is liquid-based cytology? Liquid-based cytology (LBC) is a new method of cervical cell sample preparation. Samples are collected in ...

  1. Chromium(VI Removal from Aqueous Solution by Magnetite Coated by a Polymeric Ionic Liquid-Based Adsorbent

    Directory of Open Access Journals (Sweden)

    Thania Alexandra Ferreira

    2017-05-01

    Full Text Available An evaluation of the chromium(VI adsorption capacity of four magnetite sorbents coated with a polymer phase containing polymethacrylic acid or polyallyl-3-methylimidazolium is presented. Factors that influence the chromium(VI removal such as solution pH and contact time were investigated in batch experiments and in stirred tank reactor mode. Affinity and rate constants increased with the molar ratio of the imidazolium. The highest adsorption was obtained at pH 2.0 due to the contribution of electrostatic interactions.

  2. Mechanical heterogeneity in ionic liquids

    Science.gov (United States)

    Veldhorst, Arno A.; Ribeiro, Mauro C. C.

    2018-05-01

    Molecular dynamics (MD) simulations of five ionic liquids based on 1-alkyl-3-methylimidazolium cations, [CnC1im]+, have been performed in order to calculate high-frequency elastic moduli and to evaluate heterogeneity of local elastic moduli. The MD simulations of [CnC1im][NO3], n = 2, 4, 6, and 8, assessed the effect of domain segregation when the alkyl chain length increases, and [C8C1im][PF6] assessed the effect of strength of anion-cation interaction. Dispersion curves of excitation energies of longitudinal and transverse acoustic, LA and TA, modes were obtained from time correlation functions of mass currents at different wavevectors. High-frequency sound velocity of LA modes depends on the alkyl chain length, but sound velocity for TA modes does not. High-frequency bulk and shear moduli, K∞ and G∞, depend on the alkyl chain length because of a density effect. Both K∞ and G∞ are strongly dependent on the anion. The calculation of local bulk and shear moduli was accomplished by performing bulk and shear deformations of the systems cooled to 0 K. The simulations showed a clear connection between structural and elastic modulus heterogeneities. The development of nano-heterogeneous structure with increasing length of the alkyl chain in [CnC1im][NO3] implies lower values for local bulk and shear moduli in the non-polar domains. The mean value and the standard deviations of distributions of local elastic moduli decrease when [NO3]- is replaced by the less coordinating [PF6]- anion.

  3. The potential for ionic liquid electrolytes to stabilise the magnesium interface for magnesium/air batteries

    International Nuclear Information System (INIS)

    Khoo, Timothy; Howlett, Patrick C.; Tsagouria, Maureen; MacFarlane, Douglas R.; Forsyth, Maria

    2011-01-01

    Magnesium/air batteries are a possible high-energy density power source that, to date, have not received strong commercial interest due to issues with the corrosion of the magnesium and evaporation of the electrolyte. In this work we report on the use of ionic liquid based electrolytes to stabilise the metal/electrolyte interface and their impact on the electrochemical performance. Galvanostatic measurements indicate that the water content of the ionic liquid electrolyte plays an important role in the cell discharge characteristics. Surface characterisation using EIS, ATR-FTIR and powder diffraction examined the unique properties of the surface film formed on the magnesium anode.

  4. Photophysics of ionic biochromophores

    CERN Document Server

    Brøndsted Nielsen, Steen

    2014-01-01

    This concise guide to studying ionic biochromophores features the first integrated overview of the photophysics of differing classes of biomolecules, from single amino acids to DNA. It includes an appraisal of the latest theories and experimental techniques.

  5. Cycling performance of lithium polymer cells assembled by in situ polymerization of a non-flammable ionic liquid monomer

    International Nuclear Information System (INIS)

    Lee, Yoon-Sung; Kim, Dong-Won

    2013-01-01

    Highlights: • Gel polymer electrolytes were synthesized by in situ polymerization of ionic liquid in the lithium polymer cells. • Flammability of the electrolyte was significantly reduced by polymerizing electrolyte containing a non-flammable ionic liquid monomer. • The cells assembled with polymeric ionic liquid-based electrolytes exhibited reversible cycling behavior with good capacity retention. -- Abstract: Lithium polymer cells composed of a lithium negative electrode and a LiCoO 2 positive electrode were assembled with a gel polymer electrolyte obtained by in situ polymerization of an electrolyte solution containing an ionic liquid monomer with vinyl groups. The polymerization of the electrolyte solution containing the non-flammable ionic liquid monomer resulted in a significant reduction of the flammability of the gel polymer electrolytes. The lithium polymer cell assembled with the stable gel polymer electrolyte delivered a discharge capacity of 134.3 mAh g −1 at ambient temperature and exhibited good capacity retention

  6. Fullerol ionic fluids

    KAUST Repository

    Fernandes, Nikhil

    2010-01-01

    We report for the first time an ionic fluid based on hydroxylated fullerenes (fullerols). The ionic fluid was synthesized by neutralizing the fully protonated fullerol with an amine terminated polyethylene/polypropylene oxide oligomer (Jeffamine®). The ionic fluid was compared to a control synthesized by mixing the partially protonated form (sodium form) of the fullerols with the same oligomeric amine in the same ratio as in the ionic fluids (20 wt% fullerol). In the fullerol fluid the ionic bonding significantly perturbs the thermal transitions and melting/crystallization behavior of the amine. In contrast, both the normalized heat of fusion and crystallization of the amine in the control are similar to those of the neat amine consistent with a physical mixture of the fullerols/amine with minimal interactions. In addition to differences in thermal behavior, the fullerol ionic fluid exhibits a complex viscoelastic behavior intermediate between the neat Jeffamine® (liquid-like) and the control (solid-like). © 2010 The Royal Society of Chemistry.

  7. Comparison of liquid-based cytology with conventional cytology for detection of cervical cancer precursors: a randomized controlled trial.

    NARCIS (Netherlands)

    Siebers, A.G.; Klinkhamer, P.J.; Grefte, J.M.M.; Massuger, L.F.A.G.; Vedder, J.E.; Beijers-Broos, A.; Bulten, J.; Arbyn, M.

    2009-01-01

    CONTEXT: Liquid-based cytology has been developed as an alternative for conventional cervical cytology. Despite numerous studies and systematic reviews, controversy remains about its diagnostic accuracy. OBJECTIVE: To assess the performance of liquid-based cytology compared with conventional

  8. Thermoelectric Power in Bilayer Graphene Device with Ionic Liquid Gating.

    Science.gov (United States)

    Chien, Yung-Yu; Yuan, Hongtao; Wang, Chang-Ran; Lee, Wei-Li

    2016-02-08

    The quest for materials showing large thermoelectric power has long been one of the important subjects in material science and technology. Such materials have great potential for thermoelectric cooling and also high figure of merit ZT thermoelectric applications. We have fabricated bilayer graphene devices with ionic-liquid gating in order to tune its band gap via application of a perpendicular electric field on a bilayer graphene. By keeping the Fermi level at charge neutral point during the cool-down, we found that the charge puddles effect can be greatly reduced and thus largely improve the transport properties at low T in graphene-based devices using ionic liquid gating. At (Vig, Vbg) = (-1 V, +23 V), a band gap of about 36.6 ± 3 meV forms, and a nearly 40% enhancement of thermoelectric power at T = 120 K is clearly observed. Our works demonstrate the feasibility of band gap tuning in a bilayer graphene using ionic liquid gating. We also remark on the significant influence of the charge puddles effect in ionic-liquid-based devices.

  9. Functional ionic liquids

    International Nuclear Information System (INIS)

    Baecker, Tobias

    2012-01-01

    In the thesis at hand, new functional ionic liquids were investigated. Main focus was attended to their structure property relations and the structural features leading to a decrease of the melting point. New compounds of the type 1-butyl-3-methylimidazolium tris(N,Ndialkyldithiocarbamato) uranylate with variously substituated dithiocarbamato ligands were synthesized and characterized. Ligands with asymmetrical substitution pattern proved to be most suitable for ionic liquid formation. The single-crystal X-ray structures revealed the interactions in the solid state. Here, the first spectroscopic investigation of the U-S bond in sulfur donated uranyl complexes, up to now only observed in single-crystal X-ray structures, is presented, and the participation of the uranium f-orbitals is shown by theoretical calculations. Electrochemical investigations showed the accessibility of the respective U V O 2 + compounds. As well, ionic liquids with [FeCl 4 ] - and [Cl 3 FeOFeCl 3 ] 2- as anion were synthesized. Both of these anions contain high-spin Fe(III) centres in distorted tetrahedral environment, but exhibit different magnetic behaviour. The tetrachloroferrates show the usual paramagnetism, the m-oxobis(trichloroferrate) exhibits unexpectedly strong antiferromagnetic coupling, as was observed by NMR experiments and susceptibility measurements. To investigate structure-property relations in functionalized ionic liquids, a set of protic, primary alkylammonium and aprotic, quarternary trimethylalkylammonium based ionic liquids was synthesized, and characterized. The length of the alkyl chain was systematically varied, and all compounds were synthesized with and without hydroxyl group, as well as formate and bis(triflyl)amide salts, aiming at getting insight into the influence of the different structure parts on the respective ionic liquid's properties.

  10. Rapid and sensitive determination of phytosterols in functional foods and medicinal herbs by using UHPLC-MS/MS with microwave-assisted derivatization combined with dual ultrasound-assisted dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Sun, Jing; Zhao, Xian-En; Dang, Jun; Sun, Xiaoyan; Zheng, Longfang; You, Jinmao; Wang, Xiao

    2017-02-01

    In this work, a hyphenated technique of dual ultrasound-assisted dispersive liquid-liquid microextraction combined with microwave-assisted derivatization followed by ultra high performance liquid chromatography tandem mass spectrometry has been developed for the determination of phytosterols in functional foods and medicinal herbs. Multiple reaction monitoring mode was used for the tandem mass spectrometry detection. A mass spectrometry sensitive reagent, 4'-carboxy-substituted rosamine, has been used as the derivatization reagent for five phytosterols, and internal standard diosgenin was used for the first time. Parameters for the dual microextraction, microwave-assisted derivatization, and ultra high performance liquid chromatography tandem mass spectrometry were all optimized in detail. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect, extremely low limits of detection (0.005-0.015 ng/mL) and limits of quantification (0.030-0.10 ng/mL) were achieved. The proposed method was compared with previously reported methods. It showed better sensitivity, selectivity, and accuracy. The matrix effect was also significantly reduced. The proposed method was successfully applied to the determination of five phytosterols in vegetable oil (sunflower oil, olive oil, corn oil, peanut oil), milk and orange juice (soymilk, peanut milk, orange juice), and medicinal herbs (Ginseng, Ganoderma lucidum, Cordyceps, Polygonum multiflorum) for the quality control of functional foods and medicinal herbs. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Extraction of Dihydroquercetin from Larix gmelinii with Ultrasound-Assisted and Microwave-Assisted Alternant Digestion

    Directory of Open Access Journals (Sweden)

    Yuangang Zu

    2012-07-01

    Full Text Available An ultrasound and microwave assisted alternant extraction method (UMAE was applied for extracting dihydroquercetin (DHQ from Larix gmelinii wood. This investigation was conducted using 60% ethanol as solvent, 1:12 solid to liquid ratio, and 3 h soaking time. The optimum treatment time was ultrasound 40 min, microwave 20 min, respectively, and the extraction was performed once. Under the optimized conditions, satisfactory extraction yield of the target analyte was obtained. Relative to ultrasound-assisted or microwave-assisted method, the proposed approach provides higher extraction yield. The effect of DHQ of different concentrations and synthetic antioxidants on oxidative stability in soy bean oil stored for 20 days at different temperatures (25 °C and 60 °C was compared. DHQ was more effective in restraining soy bean oil oxidation, and a dose-response relationship was observed. The antioxidant activity of DHQ was a little stronger than that of BHA and BHT. Soy bean oil supplemented with 0.08 mg/g DHQ exhibited favorable antioxidant effects and is preferable for effectively avoiding oxidation. The L. gmelinii wood samples before and after extraction were characterized by scanning electron microscopy. The results showed that the UMAE method is a simple and efficient technique for sample preparation.

  12. Optimisation of ultrasound-assisted extraction conditions for maximal recovery of active monacolins and removal of toxic citrinin from red yeast rice by a full factorial design coupled with response surface methodology.

    Science.gov (United States)

    Zhou, Guisheng; Fu, Lei; Li, Xiaobo

    2015-03-01

    This study optimised the ultrasound-assisted extraction (UAE) conditions to achieve maximal recovery of active monacolins with minimal contents of citrinin from red yeast rice (RYR). A central composite design after a full factorial design was utilised to examine the different UAE parameters. The studies revealed that HAc%, extraction time and EtOH% had significant influences on the recovery yield of monacolins, while HAc% and EtOH% were key factors for the elimination of citrinin. The resulting optimal conditions were as follows: ultrasound power of 250 W, HAc% of 7.7%, RYR amount of 0.2 g (solvent-to-solid ratio 40 mL/g), extraction time of 50.7 min, EtOH% of 57.2% and extraction temperature of 20 °C. Under these conditions, at least 94.7% of monacolins was recovered and 87.7% of citrinin was removed from RYR. This optimised UAE condition was further evaluated for potential industrial application in manufacturing of RYR as pharmaceuticals and nutraceuticals. Copyright © 2014 Elsevier Ltd. All rights reserved.

  13. Optimization of ultrasound-assisted extraction of phenolic compounds from grapefruit (citrus paradisi macf.) leaves via D-optimal Design and Artificial Neural Network Design with Categorical and Quantitative Variables.

    Science.gov (United States)

    Ciğeroğlu, Zeynep; Aras, Ömür; Pinto, Carlos A; Bayramoglu, Mahmut; İsmail Kırbaşlar, Ş; Lorenzo, José M; Barba, Francisco J; Saraiva, Jorge A; Şahin, Selin

    2018-03-06

    The extraction of phenolic compounds from grapefruit leaves assisted by ultrasound-assisted extraction (UAE) was optimized using a response surface methodology (RSM) by means of D-optimal experimental design and artificial neural network (ANN). For this purpose, five numeric factors were selected: ethanol concentration (0-50 %), extraction time (15-60 min), extraction temperature (25-50 °C), solid/liquid ratio (50-100 g L -1 ) and calorimetric energy density of ultrasound (0.25-0.50 kW L -1 ), whereas ultrasound probe horn diameter (13, 19 mm) was chosen as categorical factor. The optimized experimental conditions yielded by RSM were: 10.80 % for ethanol concentration, 58.52 min for extraction time, 30.37 o C for extraction temperature, 52.33 g L -1 for solid/liquid ratio, 0.457 kW L -1 for ultrasonic power density, thick probe for probe type, for which TPC was found as 19.04 mg of gallic acid equivalent per g of dried leaf (mg-GAE g -1 -DL). Besides, the same dataset was used to train the multilayer feed-forward networks with different approaches via MATLAB, with ANN exhibiting superior performance than RSM (differ from including categorical factor in one model, and higher regression coefficients), while close values were obtained for the extraction variables under study, except ethanol concentration and extraction time. This article is protected by copyright. All rights reserved.

  14. Multivariate optimisation of an ultrasound assisted-matrix solid-phase dispersion method combined with LC-fluorescence detection for simultaneous extraction and determination of aflatoxins in pistachio nut samples.

    Science.gov (United States)

    Manoochehri, Mahboobeh; Asgharinezhad, Ali Akbar; Safaei, Mahdi

    2013-01-01

    This paper describes the application of ultrasound-assisted matrix solid-phase dispersion as an extraction and clean-up procedure for aflatoxins (B1, B2, G1 and G2) and subsequent determination by LC-fluorescence detection. A Box-Behnken design was used to determine the parameters influencing the extraction procedure through response surface methodology and experimental design. The influence of different variables including type of dispersing phase, sample-to-dispersing phase ratio, type and quantity of clean-up phase, ultrasonication time, ultrasonication temperature, nature and volume of the elution solvent were investigated in the optimisation study. C18, graphitic carbon black and acetonitrile were selected as dispersing phase, clean-up phase and elution solvent, respectively. The optimised values were sample-to-dispersing phase ratio of 1:1, 50 mg of graphitic carbon black, 11 min ultrasonication time, 30°C ultrasonication temperature and 3 ml acetonitrile. Under the optimal conditions the limits of detection (LODs) were ranged from 0.04-0.11 µg kg(-1) and the relative standard deviations (RSDs) of the extraction method were less than 8.6%. The recoveries of the matrix solid-phase dispersion process ranged from 74% to 78% with relative standard deviation lower than 9% in all cases. Finally, the matrix solid-phase dispersion was successfully applied to extraction of trace amounts of aflatoxins in pistachio samples.

  15. Ultrasound-assisted combined with nano-sized molecularly imprinted polymer for selective extraction and pre-concentration of amitriptyline in human plasma with gas chromatography-flame detection.

    Science.gov (United States)

    Khanahmadzadeh, Salah; Tarigh, Ahmad

    2014-12-01

    A new process was developed for the selective extraction and pre-concentration of amitriptyline (AT) from human plasma using nano-sized molecularly imprinted polymer (MIP) with ultrasound-assisted extraction (UAE). The nano-sized AT imprinted polymer particles were synthesized using suspension polymerization in silicon oil and characterized by Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscope (SEM) methods. With the application of optimized values, linearity values in the ranges of 20-200μgmL(-1) and 35-200μgmL(-1) were obtained for AT with the correlation of determination values (r(2)) 0.998 and 0.995 in water and plasma, respectively. The limits of detections (S/N=3) for AT were found to be 0.7 and 1.2μgmL(-1) in water and plasma, respectively. The enrichment factors of AT in water and plasma were 52 and 40, respectively. The inter-day precisions (%) were in the range of 5.8-9.2%. Relative recovery rates ranged from 82.4% to 92.3%. The method was successfully applied to determine AT in the human plasma samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Ultrasound assisted dispersion of Bi2Sn2O7-C3N4 nanophotocatalyst over various amount of zeolite Y for enhanced solar-light photocatalytic degradation of tetracycline in aqueous solution.

    Science.gov (United States)

    Heidari, Shirin; Haghighi, Mohammad; Shabani, Maryam

    2018-05-01

    Bi 2 Sn 2 O 7 -C 3 N 4 /Y nanophotocatalyst with various ratios of zeolite and high activity under simulated solar light irradiation were successfully synthesized using ultrasound-assisted dispersion method. The effect of different amounts of zeolite (10, 20 and 30 wt%) on the photocatalytic degradation of antibiotic tetracycline was investigated. The as-prepared nanophotocatalysts were characterized by XRD, FESEM, EDX, BET, FTIR, DRS and pH pzc techniques. The degradation results demonstrated that, Bi 2 Sn 2 O 7 -C 3 N 4 /Y(10) nanophotocatalyst with a degradation efficiency of about 80.4% is an optimum sample. This result can be attributed to the zeolite as a support that prevented the accumulation of Bi 2 Sn 2 O 7 -C 3 N 4 active phase and increased access to active sites. Furthermore, it enhanced the adsorption capacity of tetracycline on the photocatalyst surface; that it is beneficial for tetracycline photocatalytic oxidation. Also the results of the DRS analysis indicated that the sharp absorption edge for optimum sample Bi 2 Sn 2 O 7 -C 3 N 4 /Y at about 480 nm and was active in the visible light range. Eventually, different operational parameters such as photocatalyst loading, concentrations of pollutant and pH solution were investigated. In addition, the degradation mechanism was suggested for TC removal. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Trace determination of five triazole fungicide residues in traditional Chinese medicine samples by dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction and UHPLC-MS/MS.

    Science.gov (United States)

    Ma, Shuping; Yuan, Xucan; Zhao, Pengfei; Sun, Hong; Ye, Xiu; Liang, Ning; Zhao, Longshan

    2017-08-01

    A novel and reliable method for determination of five triazole fungicide residues (triadimenol, tebuconazole, diniconazole, flutriafol, and hexaconazol) in traditional Chinese medicine samples was developed using dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction before ultra-high performance liquid chromatography with tandem mass spectrometry. The clean up of the extract was conducted using dispersive solid-phase extraction by directly adding sorbents into the extraction solution, followed by shaking and centrifugation. After that, a mixture of 400 μL trichloromethane (extraction solvent) and 0.5 mL of the above supernatant was injected rapidly into water for the dispersive liquid-liquid microextraction procedure. The factors affecting the extraction efficiency were optimized. Under the optimum conditions, the calibration curves showed good linearity in the range of 2.0-400 (tebuconazole, diniconazole, and hexaconazole) and 4.0-800 ng/g (triadimenol and flutriafol) with the regression coefficients higher than 0.9958. The limit of detection and limit of quantification for the present method were 0.5-1.1 and 1.8-4.0 ng/g, respectively. The recoveries of the target analytes ranged from 80.2 to 103.2%. The proposed method has been successfully applied to the analysis of five triazole fungicides in traditional Chinese medicine samples, and satisfactory results were obtained. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. A simple, rapid and sensitive ultraviolet-visible spectrophotometric technique for the determination of ultra-trace copper based on injection-ultrasound-assisted dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Liao, Xiaoxiang; Liang, Bing; Li, Zhenzhen; Li, Yanfang

    2011-11-07

    In this work, a simple, rapid and sensitive UV-visible spectrophotometric technique for the determination of copper based on injection-ultrasound-assisted dispersive liquid-liquid microextraction (IUSA-DLLME) was developed, using sodium diethyl-dithiocarbamate (Na-DDTC) as a complexing agent. The fabrication of a home-made microporous plastic tip was first reported, and by using it, contamination from a metallic tip was avoided; moreover cloudy solutions were easily obtained. Several parameters were investigated including the extraction solvent type and volume, pH of the reaction solution, concentration of DDTC, salt addition, reaction time and temperature, and sonication and centrifugation time. The results showed that carbon tetrachloride was a better extraction solvent. Under the optimal conditions, the calibration curve was linear in the range of 0.5-50 ng mL(-1) of copper with a R(2) of 0.9996. The relative standard deviation (RSD) for the determination of 0.5 ng mL(-1) copper was ±3.3% (n = 7), and the detection limit (3*Sb*c/m) was 0.05 ng mL(-1) in the original solution. An enrichment factor of 222 was obtained. The developed method was validated by analysis of a certified reference solution and applied successfully to the determination of copper in tap water, bottled pure water and river water. The advantages of the IUSA-DLLME method are simplicity of operation, rapidity, low cost, low LOD and high enrichment factor.

  20. A Simple Method for the Simultaneous Determination of Pharmaceuticals and Personal Care Products in River Sediment by Ultrasound-Assisted Extraction Followed by Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Díaz, Alejandro; Peña-Alvarez, Araceli

    2017-10-01

    A simple method was developed using ultrasound-assisted extraction (UAE) combined with solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of eight different pharmaceuticals and personal care products (PPCPs) (ibuprofen, 2-benzyl-4-chlorophenol, naproxen, triclosan, ketoprofen, diclofenac, bisphenol A and estrone) in river sediment. UAE conditions were optimized involving extraction variables such as extraction solvent, extraction time, sample amount, extraction temperature, pH and salt addition. A 100 mg of sediment was extracted by optimized UAE process using 7 mL deionized water (pH 3) + 1% methanol as solvent, room temperature and 1 min extraction at 70% of amplitude. A 5 mL of supernatant was subsequently extracted by SPME; the extracted analytes were derivatized on fiber in head-space mode with N-methyl-N-(tertbutyldimethylsilyl) trifluoroacetamide and then analyzed by GC-MS. The developed method was evaluated by testing: precision (CV 0.98), recoveries (56-108%), limits of detection (simple and environmentally friendly, and provides straightforward analyses of these trace organic pollutants in sediment samples. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  1. A new combined method of stable isotope-labeling derivatization-ultrasound-assisted dispersive liquid-liquid microextraction for the determination of neurotransmitters in rat brain microdialysates by ultra high performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Zheng, Longfang; Zhao, Xian-En; Zhu, Shuyun; Tao, Yanduo; Ji, Wenhua; Geng, Yanling; Wang, Xiao; Chen, Guang; You, Jinmao

    2017-06-01

    In this work, for the first time, a new hyphenated technique of stable isotope-labeling derivatization-ultrasound-assisted dispersive liquid-liquid microextraction has been developed for the simultaneous determination of monoamine neurotransmitters (MANTs) and their biosynthesis precursors and metabolites. The developed method was based on ultra high performance liquid chromatography tandem mass spectrometry detection using multiple-reaction monitoring mode. A pair of mass spectrometry sensitizing reagents, d 0 -10-methyl-acridone-2-sulfonyl chloride and d 3 -10-methyl-acridone-2-sulfonyl chloride, as stable isotope probes was utilized to facilely label neurotransmitters, respectively. The heavy labeled MANTs standards were prepared and used as internal standards for quantification to minimize the matrix effects in mass spectrometry analysis. Low toxic bromobenzene (extractant) and acetonitrile (dispersant) were utilized in microextraction procedure. Under the optimized conditions, good linearity was observed with the limits of detection (S/N>3) and limits of quantification (S/N>10) in the range of 0.002-0.010 and 0.015-0.040nmol/L, respectively. Meanwhile, it also brought acceptable precision (4.2-8.8%, peak area RSDs %) and accuracy (recovery, 96.9-104.1%) results. This method was successfully applied to the simultaneous determination of monoamine neurotransmitters and their biosynthesis precursors and metabolites in rat brain microdialysates of Parkinson's disease and normal rats. This provided a new method for the neurotransmitters related studies in the future. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Optimisation of ultrasound-assisted reverse micelles dispersive liquid-liquid micro-extraction by Box-Behnken design for determination of acetoin in butter followed by high performance liquid chromatography.

    Science.gov (United States)

    Roosta, Mostafa; Ghaedi, Mehrorang; Daneshfar, Ali

    2014-10-15

    A novel approach, ultrasound-assisted reverse micelles dispersive liquid-liquid microextraction (USA-RM-DLLME) followed by high performance liquid chromatography (HPLC) was developed for selective determination of acetoin in butter. The melted butter sample was diluted and homogenised by n-hexane and Triton X-100, respectively. Subsequently, 400μL of distilled water was added and the microextraction was accelerated by 4min sonication. After 8.5min of centrifugation, sedimented phase (surfactant-rich phase) was withdrawn by microsyringe and injected into the HPLC system for analysis. The influence of effective variables was optimised using Box-Behnken design (BBD) combined with desirability function (DF). Under optimised experimental conditions, the calibration graph was linear over the range of 0.6-200mgL(-1). The detection limit of method was 0.2mgL(-1) and coefficient of determination was 0.9992. The relative standard deviations (RSDs) were less than 5% (n=5) while the recoveries were in the range of 93.9-107.8%. Copyright © 2014. Published by Elsevier Ltd.

  3. Functionalized ionic liquids and their applications

    Energy Technology Data Exchange (ETDEWEB)

    Hariprakasha, Humcha Krishnamurthy; Rangan, Krishnaswamy Kasthuri; Sudarshan, Tirumalai Srinivas

    2018-01-16

    Disclosure of functionalized ionic liquids. Use of disclosed ionic liquids as solvent for carbon dioxide. Use of disclosed ionic liquids as flame retardant. Use of disclosed ionic liquids for coating fabric to obtain flame retardant fabric.

  4. Ionic smoke detectors

    CERN Document Server

    2002-01-01

    Ionic smoke detectors are products incorporating radioactive material. This article summarises the process for their commercialization and marketing, and how the activity is controlled, according to regulations establishing strict design and production requisites to guarantee the absence of radiological risk associated both with their use and their final handling as conventional waste. (Author)

  5. Synthesis of ionic liquids

    Science.gov (United States)

    Dai, Sheng [Knoxville, TN; Luo, Huimin [Knoxville, TN

    2008-09-09

    Ionic compounds which are liquids at room temperature are formed by the method of mixing a neutral organic liqand with the salt of a metal cation and its conjugate anion. The liquids are hydrophobic, conductive and stable and have uses as solvents and in electrochemical devices.

  6. Positrons in ionic crystals

    International Nuclear Information System (INIS)

    Pareja, R.

    1988-01-01

    Positron annihilation experiments in ionic crystals are reviewed and their results are arranged. A discussion about the positron states in these materials is made in the light of these results and the different proposed models. The positronium in alkali halides is specially considered. (Author)

  7. Ionic liquid solutions as extractive solvents for value-added compounds from biomass

    Science.gov (United States)

    Passos, Helena; Freire, Mara G.; Coutinho, João A. P.

    2014-01-01

    In the past few years, the number of studies regarding the application of ionic liquids (ILs) as alternative solvents to extract value-added compounds from biomass has been growing. Based on an extended compilation and analysis of the data hitherto reported, the main objective of this review is to provide an overview on the use of ILs and their mixtures with molecular solvents for the extraction of value-added compounds present in natural sources. The ILs (or IL solutions) investigated as solvents for the extraction of natural compounds, such as alkaloids, flavonoids, terpenoids, lipids, among others, are outlined. The extraction techniques employed, namely solid–liquid extraction, and microwave-assisted and ultrasound-assisted extractions, are emphasized and discussed in terms of extraction yields and purification factors. Furthermore, the evaluation of the IL chemical structure and the optimization of the process conditions (IL concentration, temperature, biomass–solvent ratio, etc.) are critically addressed. Major conclusions on the role of the ILs towards the extraction mechanisms and improved extraction yields are additionally provided. The isolation and recovery procedures of the value-added compounds are ascertained as well as some scattered strategies already reported for the IL solvent recovery and reusability. Finally, a critical analysis on the economic impact versus the extraction performance of IL-based methodologies was also carried out and is here presented and discussed. PMID:25516718

  8. 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. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Reclamation of niobium compounds from ionic liquid electrochemical polishing of superconducting radio frequency cavities

    Energy Technology Data Exchange (ETDEWEB)

    Wixtrom, Alex I. [Christopher Newport University, Newport News, VA (United States); Buhler, Jessica E. [Christopher Newport University, Newport News, VA (United States); Reece, Charles E. [Thomas Jefferson National Accelerator Facility, Newport News, VA (United States); Abdel-Fattah, Tarek M. [Christopher Newport University, Newport News, VA (United States)

    2013-06-01

    Recent research has shown that choline chloride (vitamin B4)-based solutions can be used as a greener alternative to acid-based electrochemical polishing solutions. This study demonstrated a successful method for electrochemical deposition of niobium compounds onto the surface of copper substrates using a novel choline chloride-based ionic liquid. Niobium ions present in the ionic liquid solution were dissolved into the solution prior to deposition via electrochemical polishing of solid niobium. A black coating was clearly visible on the surface of the Cu following deposition. This coating was analyzed using scanning electron microscopy (SEM), electron dispersive X-ray spectroscopy (EDX), atomic force microscopy (AFM), and X-ray fluorescence spectroscopy (XRF). This ionic liquid-based electrochemical deposition method effectively recycles previously dissolved niobium from electrochemical polishing of superconducting radio frequency (SRF) cavities.

  10. IONIC LIQUIDS: PREPARATIONS AND LIMITATIONS

    Directory of Open Access Journals (Sweden)

    Dzulkefly Kuang Abdullah

    2010-11-01

    Full Text Available Ionic liquids are considered as an ideal alternative to volatile organic solvents and chemical industries in the future,because they are non-volatile. Ionic liquids are also considered as new novel chemical agents and widely regarded as agreener alternative to many commonly used solvents. Ionic liquids have been studied for a wide range of syntheticapplications and have attracted considerable interest for use as electrolytes in the areas of organic synthesis, catalysis,solar cell, fuel cells, electrodeposition and supercapacitors. However, some ionic liquids suffer from more or less somedrawbacks such as toxicity, preparation and high cost in the process for use. Most recently, three types of ionic liquidsare attracted much attentions specifically traditional ionic liquid, protic ionic liquid and deep eutectic solvent, wheretheir preparation, mechanism and limitation were differentiated. However, those liquids are having their ownadvantages and limitations based on applications. Traditional ionic liquid and protic ionic liquid are highly cost andtoxic for applied engineering research, but they consist of micro-biphasic systems composed of ionic compounds whichhave more varieties in the applications. The deep eutectic solvent is very economic for large-scale possessing but thereare only limited ionic mixtures to certain application such as electrochemistry.

  11. Dissolving Polymers in Ionic Liquids.

    Science.gov (United States)

    Hoagland, David; Harner, John

    2009-03-01

    Dissolution and phase behavior of polymers in ionic liquids have been assessed by solution characterization techniques such as intrinsic viscosity and light scattering (static and dynamic). Elevated viscosity proved the greatest obstacle. As yet, whether principles standard to conventional polymer solutions apply to ionic liquid solutions is uncertain, especially for polymers such as polyelectrolytes and hydrophilic block copolymers that may specifically interact with ionic liquid anions or cations. For flexible polyelectrolytes (polymers releasing counterions into high dielectric solvents), characterization in ionic liquids suggests behaviors more typical of neutral polymer. Coil sizes and conformations are approximately the same as in aqueous buffer. Further, several globular proteins dissolve in a hydrophilic ionic liquid with conformations analogous to those in buffer. General principles of solubility, however, remain unclear, making predictions of which polymer dissolves in which ionic liquid difficult; several otherwise intractable polymers (e.g., cellulose, polyvinyl alcohol) dissolve and can be efficiently functionalized in ionic liquids.

  12. Review of available scientific and technical evidence regarding liquid-based cytology

    Directory of Open Access Journals (Sweden)

    Alberto Frutos Pérez-Surio

    2017-06-01

    Full Text Available Introduction. Cervical cancer can be prevented by early diagnosis and treatment of patients with abnormal results, thus decreasing their incidence and mortality. In contrast to conventional techniques (Papanicolau, diagnostic techniques have been developed based on the preservation of the sample in a stabilizing solution (liquid-based cytology. The different methods of liquid-based cytology used in the screening of cervical cancer against the Papanicolau technique are evaluated. Material and methods. A systematic review of the literature has been performed (2010-2015. The search was developed by including MeSH terms as cervical intraepithelial neoplasia and papilloma virus infection in the MedLine, Embase, Cochrane Library, CRD, LILACS and IBECS databases. Inclusion criteria were adult women screened for cervical cancer using liquid-based cytology techniques, compared with conventional methods. Results. 464 references were found related to the reliability-precision of the test, of which 13 were included in the report. A health technology assessment report was conducted in 2013 by the Agency for Health Technology Assessment of Andalusia (AETSA. The quality of the studies was moderate and moderate-low. AETSA found studies that included more than 700,000 women between 14 and 90 years old, who were screened by liquid-based cytology, compared to the conventional one. Studies have shown that liquid-based cytology techniques reduce the percentage of unsatisfactory samples compared to conventional ones. The analysis of detection of cellular abnormalities and diagnostic validity indexes showed significant differences when comparing both methods. Conclusions. The studies analyzed presented methodological limitations. Hence, the results should be interpreted with caution. Liquid-based cytology did not present greater diagnostic capacity than conventional methods, but it reduced, with statistically significant results, the number of samples unsatisfactory

  13. Fabrication of Greener Membranes from Ionic Liquid Solutions

    KAUST Repository

    Kim, DooLi

    2017-06-01

    Membrane technology plays a crucial role in different separation processes such as biotechnology, pharmaceutical, and food industries, drinking water supply, and wastewater treatment. However, there is a growing concern that solvents commonly used for membrane fabrication, such as dimethylformamide (DMF), dimethylacetamide (DMAc), and 1-methyl-2-pyrrolidone (NMP), are toxic to the environment and human health. To explore the possibility of substituting these toxic solvents by less toxic or safer solvents, polymers commonly used for membrane fabrication, such as polyacrylonitrile (PAN), cellulose acetate (CA), polyethersulfone (PES), and poly(ether imide sulfone) (EXTEMTM), were dissolved in ionic liquids. Flat sheet and hollow fiber membranes were then fabricated. The thermodynamics of the polymer solutions, the kinetics of phase inversion and other factors, which resulted in significant differences in the membrane structure, compared to those of membranes fabricated from more toxic solvents, were investigated. Higher water permeance with smaller pores, unique and uniform morphologies, and narrower pore size distribution, were observed in the ionic liquid-based membranes. Furthermore, comparable performance on separation of peptides and proteins with various molecular weights was achieved with the membranes fabricated from ionic liquid solutions. In summary, we propose less hazardous polymer solutions to the environment, which can be used for the membrane fabrication with better performance and more regular morphology.

  14. On the concept of ionicity in ionic liquids.

    Science.gov (United States)

    MacFarlane, Douglas R; Forsyth, Maria; Izgorodina, Ekaterina I; Abbott, Andrew P; Annat, Gary; Fraser, Kevin

    2009-07-07

    Ionic liquids are liquids comprised totally of ions. However, not all of the ions present appear to be available to participate in conduction processes, to a degree that is dependent on the nature of the ionic liquid and its structure. There is much interest in quantifying and understanding this 'degree of ionicity' phenomenon. In this paper we present transport data for a range of ionic liquids and evaluate the data firstly in terms of the Walden plot as an approximate and readily accessible approach to estimating ionicity. An adjusted Walden plot that makes explicit allowance for differences in ion sizes is shown to be an improvement to this approach for the series of ionic liquids described. In some cases, where diffusion measurements are possible, it is feasible to directly quantify ionicity via the Nernst-Einstein equation, confirming the validity of the adjusted Walden plot approach. Some of the ionic liquids studied exhibit ionicity values very close to ideal; this is discussed in terms of a model of a highly associated liquid in which the ion correlations have similar impact on both the diffusive and conductive motions. Ionicity, as defined, is thus a useful measure of adherence to the Nernst-Einstein equation, but is not necessarily a measure of ion availability in the chemical sense.

  15. Comparison of hollow fiber liquid-phase microextraction and ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction for the determination of drugs of abuse in biological samples by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Meng, Liang; Zhang, Wenwen; Meng, Pinjia; Zhu, Binling; Zheng, Kefang

    2015-05-01

    Two microextraction techniques based on hollow fiber liquid-phase microextraction (HF-LPME) and ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction (UA-LDS-DLLME) had been applied for the determination of drugs of abuse (methamphetamine, amphetamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyamphetamine, methcathinone, ketamine, meperidine, and methadone) in urine and blood samples by gas chromatography-mass spectrometry. Parameters affecting extraction efficiency have been investigated and optimized for both methods. Under the optimum conditions, linearities were observed for all analytes in the range 0.0030-10 μg/ml with the correlation coefficient (R) ranging from 0.9985 to 0.9995 for HF-LPME and in the range 0.0030-10 μg/ml with the R ranging from 0.9985 to 0.9994 for DLLME. The recovery of 79.3-98.6% with RSDs of 1.2-4.5% was obtained for HF-LPME, and the recovery of 79.3-103.4% with RSDs of 2.4-5.7% was obtained for DLLME. The LODs (S/N=3) were estimated to be in the range from 0.5 to 5 ng/ml and 0.5 to 4 ng/ml, respectively. Compared with HF-LPME, the UA-LDS-DLLME technique had the advantages of less extraction time, suitability for batches of sample pretreatment simultaneously, and higher extraction efficiency, while HF-LPME has excellent sample clean-up effect, and is a robust and suitable technique for various sample matrices with better repeatability. Both methods were successfully applied to the analysis of drugs of abuse in real human blood sample. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Evaluation of ultrasound-assisted extraction as sample pre-treatment for quantitative determination of rare earth elements in marine biological tissues by inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Costas, M.; Lavilla, I.; Gil, S.; Pena, F.; Calle, I.; Cabaleiro, N. de la; Bendicho, C.

    2010-01-01

    In this work, the determination of rare earth elements (REEs), i.e. Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu in marine biological tissues by inductively coupled-mass spectrometry (ICP-MS) after a sample preparation method based on ultrasound-assisted extraction (UAE) is described. The suitability of the extracts for ICP-MS measurements was evaluated. For that, studies were focused on the following issues: (i) use of clean up of extracts with a C18 cartridge for non-polar solid phase extraction; (ii) use of different internal standards; (iii) signal drift caused by changes in the nebulization efficiency and salt deposition on the cones during the analysis. The signal drift produced by direct introduction of biological extracts in the instrument was evaluated using a calibration verification standard for bracketing (standard-sample bracketing, SSB) and cumulative sum (CUSUM) control charts. Parameters influencing extraction such as extractant composition, mass-to-volume ratio, particle size, sonication time and sonication amplitude were optimized. Diluted single acids (HNO 3 and HCl) and mixtures (HNO 3 + HCl) were evaluated for improving the extraction efficiency. Quantitative recoveries for REEs were achieved using 5 mL of 3% (v/v) HNO 3 + 2% (v/v) HCl, particle size <200 μm, 3 min of sonication time and 50% of sonication amplitude. Precision, expressed as relative standard deviation from three independent extractions, ranged from 0.1 to 8%. In general, LODs were improved by a factor of 5 in comparison with those obtained after microwave-assisted digestion (MAD). The accuracy of the method was evaluated using the CRM BCR-668 (mussel tissue). Different seafood samples of common consumption were analyzed by ICP-MS after UAE and MAD.

  17. Deep eutectic solvent-based ultrasound-assisted dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the determination of ultraviolet filters in water samples.

    Science.gov (United States)

    Wang, Huazi; Hu, Lu; Liu, Xinya; Yin, Shujun; Lu, Runhua; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang

    2017-09-22

    In the present study, a simple and rapid sample preparation method designated ultrasound-assisted dispersive liquid-liquid microextraction based on a deep eutectic solvent (DES) followed by high-performance liquid chromatography with ultraviolet (UV) detection (HPLC-UVD) was developed for the extraction and determination of UV filters from water samples. The model analytes were 2,4-dihydroxybenzophenone (BP-1), benzophenone (BP) and 2-hydroxy-4-methoxybenzophenone (BP-3). The hydrophobic DES was prepared by mixing trioctylmethylammonium chloride (TAC) and decanoic acid (DecA). Various influencing factors (selection of the extractant, amount of DES, ultrasound duration, salt addition, sample volume, sample pH, centrifuge rate and duration) on UV filter recovery were systematically investigated. Under optimal conditions, the proposed method provided good recoveries in the range of 90.2-103.5% and relative standard deviations (inter-day and intra-day precision, n=5) below 5.9%. The enrichment factors for the analytes ranged from 67 to 76. The limits of detection varied from 0.15 to 0.30ngmL -1 , depending on the analytes. The linearities were between 0.5 and 500ngmL -1 for BP-1 and BP and between 1 and 500ngmL -1 for BP-3, with coefficients of determination greater than 0.99. Finally, the proposed method was applied to the determination of UV filters in swimming pool and river water samples, and acceptable relative recoveries ranging from 82.1 to 106.5% were obtained. Copyright © 2017. Published by Elsevier B.V.

  18. Determination of fluorine in herbs and water samples by molecular absorption spectrometry after preconcentration on nano-TiO2 using ultrasound-assisted dispersive micro solid phase extraction.

    Science.gov (United States)

    Krawczyk-Coda, Magdalena; Stanisz, Ewa

    2017-11-01

    This work presents ultrasound-assisted dispersive micro solid phase extraction (USA DMSPE) for preconcentration of fluorine (F) in water and herb samples. TiO 2 nanoparticles (NPs) were used as an adsorbent. The determination with slurry sampling was performed via molecular absorption of calcium monofluoride (CaF) at 606.440 nm using a high-resolution continuum source electrothermal absorption spectrometry (HR-CS ET MAS). Several factors influencing the efficiency of the preconcentration technique, such as the amount of TiO 2 , pH of sample solution, ultrasonication and centrifugation time and TiO 2 slurry solution preparation before injection to HR-CS ET MAS, were investigated in detail. The conditions of detection step (wavelength, calcium amount, pyrolysis and molecule-forming temperatures) were also studied. After extraction, adsorbent with the analyte was mixed with 200 μL of H 2 O to prepare a slurry solution. The concentration limit of detection was 0.13 ng mL -1 . The achieved preconcentration factor was 7. The relative standard deviations (RSDs, %) for F in real samples were 3-15%. The accuracy of this method was evaluated by analyses of certified reference materials after spiking: INCT-MPH-2 (Mixed Polish Herbs), INCT-SBF-4 (Soya Bean Flour), ERM-CAO11b (Hard Drinking Water) and TMDA-54.5 (Lake Ontario Water). The measured F contents in reference materials were in satisfactory agreement with the added amounts, and the recoveries were found to be 97-109%. Under the developed extraction conditions, the proposed method has been successfully applied for the determination of F in real water samples (lake, sea, tap water) and herbs.

  19. Effect of ultrasound-assisted crystallization in the diastereomeric salt resolution of tetramisole enantiomers in ternary system with O,O'-dibenzoyl-(2R,3R)-tartaric acid.

    Science.gov (United States)

    Szeleczky, Zsolt; Kis-Mihály, Erzsébet; Semsey, Sándor; Pataki, Hajnalka; Bagi, Péter; Pálovics, Emese; Marosi, György; Pokol, György; Fogassy, Elemér; Madarász, János

    2016-09-01

    The diastereomeric salt resolution of racemic tetramisole was studied using ultrasound irradiation. We examined the effect of power and duration of ultrasonic irradiation on the properties of the crystalline phase formed by ultrasound-assisted crystallization and the result of the whole optical resolution. The results were compared with reference experiment without using ultrasound. The US time (5-30min) caused higher enantiomeric excess. Although yield was lower continuously high resolving efficiency could have been reached through ultrasound. We had the best results with 4.3W ultrasound power when resolvability was even higher than the best of reference. Furthermore, we accomplished a deep and thorough examination of the salts that possibly could form in this resolution. One of the four diastereomeric salts, which have been identified by powder X-ray diffraction, FTIR-spectroscopy, and differential scanning calorimetry (DSC) in the ternary system of the two tetramisole enantiomers and the resolving agent, namely the bis[(S)-tetramisole]-dibenzoyl-(R,R)-tartrate salt have been proven the key compound in the resolution process, and presented the highest melting point of 166°C (dec.) among the four salts. The originally expected diastereomeric bitartrate salts with 1:1M base:acid ratio [(S)-tetramisole-dibenzoyl-(R,R)-hydrogen-tartrate salt and (R)-tetramisole-dibenzoyl-(R,R)-hydrogen-tartrate salt] and their 'racemic' co-crystal [(RS)-tetramisole-dibenzoyl-(R,R)-hydrogen-tartrate salt] showed somewhat lower melting points (152, 145, and 150°C, respectively) and their crystallization was also prevented by application of ultrasound. Based on the melting points and enthalpies of fusion measured by DSC, all the binary and ternary phase diagrams have been newly established and calculated in the system with help of classical modelling equations of liquidus curves. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Fe3O4/hydroxyapatite/graphene quantum dots as a novel nano-sorbent for preconcentration of copper residue in Thai food ingredients: Optimization of ultrasound-assisted magnetic solid phase extraction.

    Science.gov (United States)

    Sricharoen, Phitchan; Limchoowong, Nunticha; Areerob, Yonrapach; Nuengmatcha, Prawit; Techawongstien, Suchila; Chanthai, Saksit

    2017-07-01

    Fe 3 O 4 /hydroxyapatite/graphene quantum dots (Fe 3 O 4 /HAP/GQDs) nanocomposite was synthesized and used as a novel magnetic adsorbent. This nanocomposite was characterized using scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, and magnetization property. The Fe 3 O 4 /HAP/GQDs was applied to pre-concentrate copper residues in Thai food ingredients (so-called "Tom Yum Kung") prior to determination by inductively coupled plasma-atomic emission spectrometry. Based on ultrasound-assisted extraction optimization, various parameters affecting the magnetic solid-phase extraction, such as solution pH, amount of magnetic nanoparticles, adsorption and desorption time, and type of elution solvent and its concentration were evaluated. Under optimal conditions, the linear range was 0.05-1500ngmL -1 (R 2 >0.999), limit of detection was 0.58ngmL -1 , and limit of quantification was 1.94ngmL -1 . The precision, expressed as the relative standard deviation of the calibration curve slope (n=5), for intra-day and inter-day analyses was 0.87% and 4.47%, respectively. The recovery study of Cu for real samples was ranged between 83.5% and 104.8%. This approach gave the enrichment factor of 39.2, which guarantees trace analysis of Cu residues. Therefore, Fe 3 O 4 /HAP/GQDs can be a potential and suitable candidate for the pre-concentration and separation of Cu from food samples. It can easily be reused after treatment with deionized water. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Analysis of amino acid and monoamine neurotransmitters and their metabolites in rat urine of Alzheimer's disease using in situ ultrasound-assisted derivatization dispersive liquid-liquid microextraction with UHPLC-MS/MS.

    Science.gov (United States)

    Zhao, Xian-En; He, Yongrui; Li, Meng; Chen, Guang; Wei, Na; Wang, Xiao; Sun, Jing; Zhu, Shuyun; You, Jinmao

    2017-02-20

    Neurotransmitters (NTs) may play an important role in neurodegenerative disorders such as Alzheimer's disease (AD). In order to investigate the potential links, a new simple, fast, accurate and sensitive analytical method, based on in situ ultrasound-assisted derivatization dispersive liquid-liquid microextraction (in situ UA-DDLLME) coupled with ultra high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS), has been developed and validated. The quantitation of amino acid neurotransmitters (AANTs) and monoamine neurotransmitters (MANTs) in urine of AD rats were performed in this work. The in situ UA-DDLLME procedure involved the rapid injection of the mixture of low toxic 4-bromoanisole (extractant) and acetonitrile (dispersant), which containing the new designed and synthesized 4'-carbonyl chloride rosamine (CCR) as derivatization reagent, into the aqueous phase of real sample and buffer. Under the selected conditions, the derivatization and microextraction of analytes were simultaneously completed within 1min. Good linearity for each analyte (R>0.992) was observed with low limit of detections (LODs, S/N>3). Moreover, the proposed method was compared with direct detection or other reported methods, and the results showed that low matrix effects and good recoveries results were obtained in this work. Taken together, in situ UA-DDLLME coupled with UHPLC-MS/MS analysis was demonstrated to be a good method for sensitive, accurate and simultaneous monitoring of AANTs and MANTs. This method would be expected to be highly useful in AD diseases' clinical diagnostics and may have potential value in monitoring the efficacy of treatment. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction for the determination of 4 designer benzodiazepines in urine samples by gas chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Meng, Liang; Zhu, Binling; Zheng, Kefang; Fu, Shanlin

    2017-05-15

    A novel microextraction technique based on ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction (UA-LDS-DLLME) had been applied for the determination of 4 designer benzodiazepines (phenazepam, diclazepam, flubromazepam and etizolam) in urine samples by gas chromatography- triple quadrupole mass spectrometry (GC-QQQ-MS). Ethyl acetate (168μL) was added into the urine samples after adjusting pH to 11.3. The samples were sonicated in an ultrasonic bath for 5.5min to form a cloudy suspension. After centrifugation at 10000rpm for 3min, the supernatant extractant was withdrawn and injected into the GC-QQQ-MS for analysis. Parameters affecting the extraction efficiency have been investigated and optimized by means of single factor experiment and response surface methodology (Box-Behnken design). Under the optimum extraction conditions, a recovery of 73.8-85.5% were obtained for all analytes. The analytical method was linear for all analytes in the range from 0.003 to 10μg/mL with the correlation coefficient ranging from 0.9978 to 0.9990. The LODs were estimated to be 1-3ng/mL. The accuracy (expressed as mean relative error MRE) was within ±5.8% and the precision (expressed as relative standard error RSD) was less than 5.9%. UA-LDS-DLLME technique has the advantages of shorter extraction time and is suitable for simultaneous pretreatment of samples in batches. The combination of UA-LDS-DLLME with GC-QQQ-MS offers an alternative analytical approach for the sensitive detection of these designer benzodiazepines in urine matrix for clinical and medico-legal purposes. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. In situ ultrasound-assisted preparation of Fe3O4@MnO2 core-shell nanoparticles integrated with ion co-precipitation for multielemental analysis by total reflection X-ray fluorescence

    Science.gov (United States)

    Nourbala-Tafti, Elaheh; Romero, Vanesa; Lavilla, Isela; Dadfarnia, Shayesteh; Bendicho, Carlos

    2017-05-01

    In this work, a new analytical approach based on in situ ultrasound-assisted preparation of manganese dioxide coated magnetite nanoparticles (Fe3O4@MnO2 NPs) was applied for extraction and preconcentration of Ni, Cu, Zn, Tl, Pb, Bi and Se. The Fe3O4@MnO2 core-shell nanocomposite was synthesized by application of high-intensity sonication to an aqueous reaction medium in the presence of the target analytes, which are trapped during NPs formation. In this way, synthesis of the nanosorbent and extraction can be simultaneously accomplished within only 30 s. After the extraction step, the resulting Fe3O4@MnO2 NPs enriched with the target analytes were separated by an external magnetic field, so that filtration or centrifugation steps were unnecessary. A 10 μL aliquot of the solid phase was deposited onto a sample carrier (quartz reflector) and directly analyzed by total-reflection X-ray fluorescence (TXRF) without the need for an elution step. A comprehensive characterization of the Fe3O4@MnO2 NPs was carried out by transmission electron microscopy and TXRF. Detection limits ranged from 0.19 to 0.98 μg L- 1 depending on the analyte. Enrichment factors in the range of 402-540 were obtained. The repeatability expressed as relative standard deviation was around 1.7% (N = 5). The accuracy of the proposed method was assessed by analyzing the certified reference material BCR®-610 (groundwater). An effective, simple, rapid and sensitive procedure for multielemental analysis of water samples was accomplished.

  4. Fast ultrasound-assisted extraction followed by capillary gas chromatography combined with nitrogen-phosphorous selective detector for the trace determination of tebuconazole in garlic, soil and water samples.

    Science.gov (United States)

    Singh, Sunil Kumar; Padmaja, P; Pandey, S Y

    2014-06-01

    A fast and an efficient ultrasound-assisted extraction technique using a lower density extraction solvent than water was developed for the trace-level determination of tebuconazole in garlic, soil and water samples followed by capillary gas chromatography combined with nitrogen-phosphorous selective detector (GC-NPD). In this approach, ultrasound radiation was applied to accelerate the emulsification of the ethyl acetate in aqueous samples to enhance the extraction efficiency of tebuconazole without requiring extra partitioning or cleaning, and the use of capillary GC-NPD was a more sensitive detection technique for organonitrogen pesticides. The experimental results indicate an excellent linear relationship between peak area and concentration obtained in the range 1-50 μg/kg or μg/L. The limit of detection (S/N, 3 ± 0.5) and limit of quantification (S/N, 7.5 ± 2.5) were obtained in the range 0.2-3 and 1-10 μg/kg or μg/L. Good spiked recoveries were achieved from ranges 95.55-101.26%, 96.28-99.33% and 95.04-105.15% in garlic, Nanivaliyal soil and Par River water, respectively, at levels 5 and 20 μg/kg or μg/L, and the method precision (% RSD) was ≤5%. Our results demonstrate that the proposed technique is a viable alternative for the determination of tebuconazole in complex samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Super ionic conductive glass

    Science.gov (United States)

    Susman, S.; Volin, K.J.

    Described is an ionically conducting glass for use as a solid electrolyte in a power or secondary cell containing an alkali metal-containing anode and a cathode separated by an alkali metal ion conducting glass having an ionic transference number of unity and the general formula: A/sub 1 + x/D/sub 2-x/3/Si/sub x/P/sub 3 - x/O/sub 12 - 2x/3/, wherein A is a network modifier for the glass and is an alkali metal of the anode, D is an intermediate for the glass and is selected from the class consisting of Zr, Ti, Ge, Al, Sb, Be, and Zn and X is in the range of from 2.25 to 3.0. Of the alkali metals, Na and Li are preferred and of the intermediate, Zr, Ti and Ge are preferred.

  6. Nanoscale Ionic Materials

    KAUST Repository

    Rodriguez, Robert

    2008-11-18

    Polymer nanocomposites (nanoparticles dispersed in a polymer matrix) have been the subject of intense research for almost two decades in both academic and industrial settings. This interest has been fueled by the ability of nanocomposites to not only improve the performance of polymers, but also by their ability to introduce new properties. Yet, there are still challenges that polymer nanocomposites must overcome to reach their full potential. In this Research News article we discuss a new class of hybrids termed nanoparticle ionic materials (NIMS). NIMS are organic-inorganic hybrid materials comprising a nanoparticle core functionalized with a covalently tethered ionic corona. They are facilely engineered to display flow properties that span the range from glassy solids to free flowing liquids. These new systems have unique properties that can overcome some of the challenges facing nanocomosite materials. © 2008 WILEY-VCH Verlag GmbH & Co. KGaA.

  7. Thermodynamic estimation: Ionic materials

    International Nuclear Information System (INIS)

    Glasser, Leslie

    2013-01-01

    Thermodynamics establishes equilibrium relations among thermodynamic parameters (“properties”) and delineates the effects of variation of the thermodynamic functions (typically temperature and pressure) on those parameters. However, classical thermodynamics does not provide values for the necessary thermodynamic properties, which must be established by extra-thermodynamic means such as experiment, theoretical calculation, or empirical estimation. While many values may be found in the numerous collected tables in the literature, these are necessarily incomplete because either the experimental measurements have not been made or the materials may be hypothetical. The current paper presents a number of simple and relible estimation methods for thermodynamic properties, principally for ionic materials. The results may also be used as a check for obvious errors in published values. The estimation methods described are typically based on addition of properties of individual ions, or sums of properties of neutral ion groups (such as “double” salts, in the Simple Salt Approximation), or based upon correlations such as with formula unit volumes (Volume-Based Thermodynamics). - Graphical abstract: Thermodynamic properties of ionic materials may be readily estimated by summation of the properties of individual ions, by summation of the properties of ‘double salts’, and by correlation with formula volume. Such estimates may fill gaps in the literature, and may also be used as checks of published values. This simplicity arises from exploitation of the fact that repulsive energy terms are of short range and very similar across materials, while coulombic interactions provide a very large component of the attractive energy in ionic systems. Display Omitted - Highlights: • Estimation methods for thermodynamic properties of ionic materials are introduced. • Methods are based on summation of single ions, multiple salts, and correlations. • Heat capacity, entropy

  8. Course on Ionic Channels

    CERN Document Server

    1986-01-01

    This book is based on a series of lectures for a course on ionic channels held in Santiago, Chile, on November 17-20, 1984. It is intended as a tutorial guide on the properties, function, modulation, and reconstitution of ionic channels, and it should be accessible to graduate students taking their first steps in this field. In the presentation there has been a deliberate emphasis on the spe­ cific methodologies used toward the understanding of the workings and function of channels. Thus, in the first section, we learn to "read" single­ channel records: how to interpret them in the theoretical frame of kinetic models, which information can be extracted from gating currents in re­ lation to the closing and opening processes, and how ion transport through an open channel can be explained in terms of fluctuating energy barriers. The importance of assessing unequivocally the origin and purity of mem­ brane preparations and the use of membrane vesicles and optical tech­ niques in the stUGY of ionic channels a...

  9. Cost and cost-effectiveness of conventional and liquid-based ...

    African Journals Online (AJOL)

    Background. South Africa has a high prevalence of cervical cancer. Early detection can significantly reduce the burden of this disease. New screening technologies to detect cervical pathology have become available in recent years. Objectives. To determine the cost and cost-effectiveness of liquid-based cytology (LBC) ...

  10. Novel routes to liquid-based self-healing polymer systems

    NARCIS (Netherlands)

    Mookhoek, S.D.

    2010-01-01

    Inspired by the current state-of-the-art and the progressing advancements in the field of self-healing materials, this thesis addresses several novel routes to advance the concept of liquid-based self-healing polymer systems. This thesis presents the concept and characterisation of a one-component

  11. Flavonoids in Different Parts of Lysimachia clethroides Duby Extracted by Ionic Liquid: Analysis by HPLC and Antioxidant Activity Assay

    Directory of Open Access Journals (Sweden)

    Jin-feng Wei

    2017-01-01

    Full Text Available To establish methods for simultaneous determination of isoquercitrin, astragalin in leaves, quercetin, and kaempferol in flowers of Lysimachia clethroides Duby, respectively, the methods were ultrasound-assisted extraction combined with RP-HPLC, and ionic liquid was used as the extraction solvent. Meanwhile, the antioxidant activity of the different extracts of L. clethroides was evaluated. Purospher STAR RP-C18 column (4.6 mm × 250 mm, 5 μm was used for analysis. The flow rate was 0.6 mL·min−1, and the column temperature was 25°C. The detection wavelength was 360 nm. The mobile phases a and b consisted of acetonitrile-0.4% phosphoric acid (18 : 82, v/v, methanol (A, and 0.4% phosphoric acid (B, respectively. Linear ranges were 0.068~1.64, 0.060~1.44, 0.0080~0.19, and 0.0077~0.18 μg for isoquercitrin, astragalin, quercetin, and kaempferol, respectively. The average recoveries of the four constituents were 99.17%, 98.39%, 100.68%, and 98.81%, respectively. The antioxidant activity of the extracts was detected by DPPH, ABTS, and FRAP. Under the optimized conditions, all the test solutions showed a certain antioxidant activity and the ionic liquid extracts were better than that of extract of methanol. Ionic liquid used as the extraction solvent had the potential to extract active ingredients efficiently from L. clethroides, and this method improved the antioxidant activity with accurate and reliable results.

  12. Controlled electrodeposition of Au monolayer film on ionic liquid

    Science.gov (United States)

    Ma, Qiang; Pang, Liuqing; Li, Man; Zhang, Yunxia; Ren, Xianpei; Liu, Shengzhong Frank

    2016-05-01

    Gold (Au) nanoparticles have been attractive for centuries for their vibrant appearance enhanced by their interaction with sunlight. Nowadays, there have been tremendous research efforts to develop them for high-tech applications including therapeutic agents, sensors, organic photovoltaics, medical applications, electronics and catalysis. However, there remains to be a challenge to fabricate a monolayer Au coating with complete coverage in controlled fashion. Here we present a facile method to deposit a uniform Au monolayer (ML) film on the [BMIM][PF6] ionic liquid substrate using an electrochemical deposition process. It demonstrates that it is feasible to prepare a solid phase coating on the liquid-based substrate. Moreover, the thickness of the monolayer coating can be controlled to a layer-by-layer accuracy.

  13. Ionic liquids, electrolyte solutions including the ionic liquids, and energy storage devices including the ionic liquids

    Science.gov (United States)

    Gering, Kevin L.; Harrup, Mason K.; Rollins, Harry W.

    2015-12-08

    An ionic liquid including a phosphazene compound that has a plurality of phosphorus-nitrogen units and at least one pendant group bonded to each phosphorus atom of the plurality of phosphorus-nitrogen units. One pendant group of the at least one pendant group comprises a positively charged pendant group. Additional embodiments of ionic liquids are disclosed, as are electrolyte solutions and energy storage devices including the embodiments of the ionic liquid.

  14. Energy consumption analysis for CO2 separation using imidazolium-based ionic liquids

    International Nuclear Information System (INIS)

    Xie, Yujiao; Zhang, Yingying; Lu, Xiaohua; Ji, Xiaoyan

    2014-01-01

    Highlights: • CO 2 solubility in imidazolium-based ionic liquids was surveyed and evaluated. • CO 2 absorption enthalpy was calculated based on thermodynamic model. • The effects of cation and anion on CO 2 absorption enthalpy were discussed. • Energy consumption for a CO 2 separation process was investigated. - Abstract: CO 2 solubility in ionic liquids has been measured extensively in order to develop ionic liquid-based technology for CO 2 separation. However, the energy consumption analysis has not been investigated well for such technology. In order to carry out the energy consumption analysis for CO 2 separation using ionic liquids based on available experimental data, in this work, the experimental data of the CO 2 solubility in imidazolium-based ionic liquids at pressures below 10 MPa was surveyed and evaluated by a semi-empirical thermodynamic model firstly. Based on the reliable experimental solubility data, the enthalpy of CO 2 absorption was further calculated by the thermodynamic model. The results show that the CO 2 absorption enthalpy in the studied ionic liquids is dominated by the enthalpy of CO 2 dissolution and the contribution of excess enthalpy increases with increasing CO 2 solubility in ionic liquids. The magnitude of the CO 2 absorption enthalpy decreases with increasing chain length in cation and strongly depends on the anion of ionic liquids. Furthermore, the energy consumption for a CO 2 separation process by pressure swing and/or temperature swing was investigated. For the pressure swing process, the Henry’s constant of CO 2 in ionic liquids is an important factor for energy consumption analysis; If CO 2 is absorbed at 298 K and 1 MPa and ionic liquid is regenerated by decreasing the pressure to 0.1 MPa at the same temperature, among the studied ionic liquids, [emim][EtSO 4 ] is the solvent with the lowest energy consumption of 9.840 kJ/mol CO 2 . For the temperature swing process, the heat capacity of ionic liquids plays a more

  15. Ultrasound-assisted dealumination of zeolite Y

    Indian Academy of Sciences (India)

    We demonstrate a new procedure for dealumination of zeolite Y. The method employs a 28 KHz ultrasound bath and an ethanolic acetylacetone solution. Acetylacetone was used as chelating agent and ultrasound irradiation was used as extraction intensifier. Four types of samples, as-synthesized, ammoniumexchanged, ...

  16. Ultrasound-assisted dealumination of zeolite Y

    Indian Academy of Sciences (India)

    Higher dealumination was observed for those samples subjected to both ultrasound irradiation and acetylacetone extraction. Keywords. Microporous; zeolite Y; dealumination; ultrasound irradiation; extraction. 1. ..... ture has also been claimed while ultrasound waves were used for the extraction of contaminants in food and.

  17. Microbial Inactivation by Ultrasound Assisted Supercritical Fluids

    Science.gov (United States)

    Benedito, Jose; Ortuño, Carmen; Castillo-Zamudio, Rosa Isela; Mulet, Antonio

    A method combining supercritical carbon dioxide (SC-CO2) and high power ultrasound (HPU) has been developed and tested for microbial/enzyme inactivation purposes, at different process conditions for both liquid and solid matrices. In culture media, using only SC-CO2, the inactivation rate of E. coli and S. cerevisiae increased with pressure and temperature; and the total inactivation (7-8 log-cycles) was attained after 25 and 140 min of SC-CO2 (350 bar, 36 °C) treatment, respectively. Using SC-CO2+HPU, the time for the total inactivation of both microorganisms was reduced to only 1-2 min, at any condition selected. The SC-CO2+HPU inactivation of both microorganisms was slower in juices (avg. 4.9 min) than in culture media (avg. 1.5 min). In solid samples (chicken, turkey ham and dry-cured pork cured ham) treated with SC-CO2 and SC-CO2+HPU, the inactivation rate of E. coli increased with temperature. The application of HPU to the SC-CO2 treatments accelerated the inactivation rate of E. coli and that effect was more pronounced in treatments with isotonic solution surrounding the solid food samples. The application of HPU enhanced the SC-CO2 inactivation mechanisms of microorganisms, generating a vigorous agitation that facilitated the CO2 solubilization and the mass transfer process. The cavitation generated by HPU could damage the cell walls accelerating the extraction of vital constituents and the microbial death. Thus, using the combined technique, reasonable industrial processing times and mild process conditions could be used which could result into a cost reduction and lead to the minimization in the food nutritional and organoleptic changes.

  18. Application of Ultrasound-assisted Emulsification Microextraction ...

    African Journals Online (AJOL)

    NICOLAAS

    passed through a PTFE syringe filter (13 mm, 0.22 µm) (Sigma-. Aldrich) to remove particles. For USAEME, a 2.0 mL aliquot of the residual filtrate and 10.0 mL of water was placed in a 12 mL home-designed centrifuge glass vial and ultrapure water was added to fill the tube. Then the sample was submitted to. USAEME as ...

  19. Ultrasound-assisted liquefaction of honey

    OpenAIRE

    Kabbani, Dania

    2014-01-01

    Crystallization of honey is a common process of the honey industry. Liquid honey is preferred by most of the consumers and by food companies for ease of handling. Honey is commonly heated during pasteurization in order to liquefy it and inhibit any microbial growth. However, heating can degrade the main quality parameters of honey. A better method compared to expensive and time-consuming heating is desirable to pasteurize, accelerate the liquefaction and retard the crystallization process...

  20. Ultrasound-assisted dealumination of zeolite Y

    Indian Academy of Sciences (India)

    Higher dealumination was observed for those samples subjected to both ultrasound irradiation and acetylacetone extraction ... lite was prepared upon conventional ion-exchange treat- ment using an aqueous solution of 0.4 M NH4Cl at 25. ◦. C ... form of the zeolite to acidic one, it was heated in a muf- fle furnace at rate of 10.

  1. An innovative ultrasound assisted extraction micro-scale cell combined with gas chromatography/mass spectrometry in negative chemical ionization to determine persistent organic pollutants in air particulate matter.

    Science.gov (United States)

    Beristain-Montiel, E; Villalobos-Pietrini, R; Arias-Loaiza, G E; Gómez-Arroyo, S L; Amador-Muñoz, O

    2016-12-16

    New clean technologies are needed to determine concentration of organic pollutants without generating more pollution. A method to extract Persistent Organic Pollutants (POPs) from airborne particulate matter was developed using a novel technology recently patented called ultrasound assisted extraction micro-scale cell (UAE-MSC). This technology extracts, filters, collects the sample, and evaporates the solvent, on-line. No sample transfer is needed. The cell minimizes sample manipulation, solvent consumption, waste generation, time, and energy; fulfilling most of the analytical green chemistry protocol. The methodology was optimized applying a centred 2 3 factorial experimental design. Optimum conditions were used to validate and determine concentration of 16 organochlorine pesticides (OCls) and 6 polybrominated diphenyl ethers (PBDEs). The best conditions achieved were 2 extractions with 5mL (each) of dichloromethane over 5min (each) at 60°C and 80% ultrasound potency. POPs were determined by gas chromatography/mass spectrometry in negative chemical ionization (GC/MS-NCI). Analytical method validation was carried out on airborne particles spiked with POPs at seven concentration levels between 0.5 and 26.9pgm -3 . This procedure was done by triplicate (N=21). Recovery, ranged between 65.5±2.3% and 107.5±3.0% for OCls and between 79.1±6.5% and 105.2±3.8% for PBDEs. Linearity (r 2 ) was ≥0.94 for all compounds. Method detection limits, ranged from 0.5 to 2.7pgm -3 , while limits of quantification (LOQ), ranged from 1.7 to 9.0pgm -3 . A Bias from -18.6% to 9% for PBDEs was observed in the Standard Reference Material (SRM) 2787. SRM 2787 did not contain OCls. OCls recoveries were equivalent by UAE-MSC and Soxhlet methods UAE-MSC optimized extraction conditions reduced 30 times less solvent and decreased the extraction time from several hours to ten minutes, respect to Soxhlet. UAE-MSC was applied to 15 samples of particles less than 2.5μm (PM 2.5 ) from three

  2. In situ derivatization-ultrasound-assisted dispersive liquid-liquid microextraction for the determination of neurotransmitters in Parkinson's rat brain microdialysates by ultra high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    He, Yongrui; Zhao, Xian-En; Zhu, Shuyun; Wei, Na; Sun, Jing; Zhou, Yubi; Liu, Shu; Liu, Zhiqiang; Chen, Guang; Suo, Yourui; You, Jinmao

    2016-08-05

    Simultaneous monitoring of several neurotransmitters (NTs) linked to Parkinson's disease (PD) has important scientific significance for PD related pathology, pharmacology and drug screening. A new simple, fast and sensitive analytical method, based on in situ derivatization-ultrasound-assisted dispersive liquid-liquid microextraction (in situ DUADLLME) in a single step, has been proposed for the quantitative determination of catecholamines and their biosynthesis precursors and metabolites in rat brain microdialysates. The method involved the rapid injection of the mixture of low toxic bromobenzene (extractant) and acetonitrile (dispersant), which containing commercial Lissamine rhodamine B sulfonyl chloride (LRSC) as derivatization reagent, into the aqueous phase of sample and buffer, and the following in situ DUADLLME procedure. After centrifugation, 50μL of the sedimented phase (bromobenzene) was directly injected for ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) detection in multiple reaction monitoring (MRM) mode. This interesting combination brought the advantages of speediness, simpleness, low matrix effects and high sensitivity in an effective way. Parameters of in situ DUADLLME and UHPLC-MS/MS conditions were all optimized in detail. The optimum conditions of in situ DUADLLME were found to be 30μL of microdialysates, 150μL of acetonitrile containing LRSC, 50μL of bromobenzene and 800μL of NaHCO3-Na2CO3 buffer (pH 10.5) for 3.0min at 37°C. Under the optimized conditions, good linearity was observed with LODs (S/N>3) and LOQs (S/N>10) of LRSC derivatized-NTs in the range of 0.002-0.004 and 0.007-0.015 nmol/L, respectively. It also brought good precision (3.2-12.8%, peak area CVs%), accuracy (94.2-108.6%), recovery (94.5-105.5%) and stability (3.8-8.1%, peak area CVs%) results. Moreover, LRSC derivatization significantly improved chromatographic resolution and MS detection sensitivity of NTs when compared with the

  3. Thermophysical characterization of N-methyl-2-hydroxyethylammonium carboxilate ionic liquids

    OpenAIRE

    Talavera-Prieto, Nieves M. C.; Ferreira, Abel G. M.; Simões, Pedro N.; Carvalho, Pedro J.; Mattedi, Silvana; Coutinho, João A. P.

    2014-01-01

    The thermophysical properties including density, heat capacity, thermal stability and phase behaviour of protic ionic liquids based on the N-methyl-2-hydroxyethylammonium cation, [C2OHC1NH2]+, with the carboxylate anions (propionate, [C2COO]−, butyrate, [C3COO]−, and pentanoate, [C4COO]−) are reported and used to evaluate structure-property relationships. The density was measured over the temperature and pressure ranges, T = (298.15 to 358.15) K and p = (0.1 to 25) MPa, respectively, with an ...

  4. Noble metal ionic catalysts.

    Science.gov (United States)

    Hegde, M S; Madras, Giridhar; Patil, K C

    2009-06-16

    Because of growing environmental concerns and increasingly stringent regulations governing auto emissions, new more efficient exhaust catalysts are needed to reduce the amount of pollutants released from internal combustion engines. To accomplish this goal, the major pollutants in exhaust-CO, NO(x), and unburned hydrocarbons-need to be fully converted to CO(2), N(2), and H(2)O. Most exhaust catalysts contain nanocrystalline noble metals (Pt, Pd, Rh) dispersed on oxide supports such as Al(2)O(3) or SiO(2) promoted by CeO(2). However, in conventional catalysts, only the surface atoms of the noble metal particles serve as adsorption sites, and even in 4-6 nm metal particles, only 1/4 to 1/5 of the total noble metal atoms are utilized for catalytic conversion. The complete dispersion of noble metals can be achieved only as ions within an oxide support. In this Account, we describe a novel solution to this dispersion problem: a new solution combustion method for synthesizing dispersed noble metal ionic catalysts. We have synthesized nanocrystalline, single-phase Ce(1-x)M(x)O(2-delta) and Ce(1-x-y)Ti(y)M(x)O(2-delta) (M = Pt, Pd, Rh; x = 0.01-0.02, delta approximately x, y = 0.15-0.25) oxides in fluorite structure. In these oxide catalysts, Pt(2+), Pd(2+), or Rh(3+) ions are substituted only to the extent of 1-2% of Ce(4+) ion. Lower-valent noble metal ion substitution in CeO(2) creates oxygen vacancies. Reducing molecules (CO, H(2), NH(3)) are adsorbed onto electron-deficient noble metal ions, while oxidizing (O(2), NO) molecules are absorbed onto electron-rich oxide ion vacancy sites. The rates of CO and hydrocarbon oxidation and NO(x) reduction (with >80% N(2) selectivity) are 15-30 times higher in the presence of these ionic catalysts than when the same amount of noble metal loaded on an oxide support is used. Catalysts with palladium ion dispersed in CeO(2) or Ce(1-x)Ti(x)O(2) were far superior to Pt or Rh ionic catalysts. Therefore, we have demonstrated that the

  5. Surface-active ionic liquids in micellar catalysis: impact of anion selection on reaction rates in nucleophilic substitutions.

    Science.gov (United States)

    Cognigni, Alice; Gaertner, Peter; Zirbs, Ronald; Peterlik, Herwig; Prochazka, Katharina; Schröder, Christian; Bica, Katharina

    2016-05-21

    A series of surface-active ionic liquids based on the 1-dodecyl-3-methylimidazolium cation and different anions such as halides and alkylsulfates was synthesized. The aggregation behavior of these ionic liquids in water was characterized by surface tension, conductivity measurements and UV-Vis spectroscopy in order to determine the critical micelle concentration (CMC) and to provide aggregation parameters. The determination of surface activity and aggregation properties of amphiphilic ionic liquids was accompanied by SAXS studies on selected surface-active ionic liquids. The application of these surface-active ionic liquids with different anions was tested in nucleophilic substitution reactions for the degradation of organophosphorus compounds. Kinetic studies via UV-Vis spectrophotometry showed a strong acceleration of the reaction in the micellar system compared to pure water. In addition, an influence of the anion was observed, resulting in a correlation between the anion binding to the micelle and the reaction rate constants, indicating that the careful choice of the surface-active ionic liquid can considerably affect the outcome of reactions.

  6. Ionic Liquid Crystals: Versatile Materials.

    Science.gov (United States)

    Goossens, Karel; Lava, Kathleen; Bielawski, Christopher W; Binnemans, Koen

    2016-04-27

    This Review covers the recent developments (2005-2015) in the design, synthesis, characterization, and application of thermotropic ionic liquid crystals. It was designed to give a comprehensive overview of the "state-of-the-art" in the field. The discussion is focused on low molar mass and dendrimeric thermotropic ionic mesogens, as well as selected metal-containing compounds (metallomesogens), but some references to polymeric and/or lyotropic ionic liquid crystals and particularly to ionic liquids will also be provided. Although zwitterionic and mesoionic mesogens are also treated to some extent, emphasis will be directed toward liquid-crystalline materials consisting of organic cations and organic/inorganic anions that are not covalently bound but interact via electrostatic and other noncovalent interactions.

  7. Biopolymer Processing Using Ionic Liquids

    Science.gov (United States)

    2014-08-07

    reaction and degradation products of the conversion of chitin and chitosan, and 3) investigate the effects of various reaction conditions, such as...reaction temperature, and catalyst loading, on the reaction rate and degradation products from the depolymerization of chitin and chitosan. 15. SUBJECT... based ionic liquid for the dissolution of chitin and a sulfonic acid functionalized ionic liquid, chitin can be hydrolyzed into its monomer unit, N

  8. Ionic Liquid Epoxy Resin Monomers

    Science.gov (United States)

    Paley, Mark S. (Inventor)

    2013-01-01

    Ionic liquid epoxide monomers capable of reacting with cross-linking agents to form polymers with high tensile and adhesive strengths. Ionic liquid epoxide monomers comprising at least one bis(glycidyl) N-substituted nitrogen heterocyclic cation are made from nitrogen heterocycles corresponding to the bis(glycidyl) N-substituted nitrogen heterocyclic cations by a method involving a non-nucleophilic anion, an alkali metal cation, epichlorohydrin, and a strong base.

  9. Fluctuating hydrodynamics for ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    Lazaridis, Konstantinos [Department of Mathematics and Statistics, Washington State University, Pullman, 99163 (United States); Wickham, Logan [Department of Computer Science, Washington State University, Richland, 99354 (United States); Voulgarakis, Nikolaos, E-mail: n.voulgarakis@wsu.edu [Department of Mathematics and Statistics, Washington State University, Pullman, 99163 (United States)

    2017-04-25

    We present a mean-field fluctuating hydrodynamics (FHD) method for studying the structural and transport properties of ionic liquids in bulk and near electrified surfaces. The free energy of the system consists of two competing terms: (1) a Landau–Lifshitz functional that models the spontaneous separation of the ionic groups, and (2) the standard mean-field electrostatic interaction between the ions in the liquid. The numerical approach used to solve the resulting FHD-Poisson equations is very efficient and models thermal fluctuations with remarkable accuracy. Such density fluctuations are sufficiently strong to excite the experimentally observed spontaneous formation of liquid nano-domains. Statistical analysis of our simulations provides quantitative information about the properties of ionic liquids, such as the mixing quality, stability, and the size of the nano-domains. Our model, thus, can be adequately parameterized by directly comparing our prediction with experimental measurements and all-atom simulations. Conclusively, this work can serve as a practical mathematical tool for testing various theories and designing more efficient mixtures of ionic liquids. - Highlights: • A new fluctuating hydrodynamics method for ionic liquids. • Description of ionic liquid morphology in bulk and near electrified surfaces. • Direct comparison with experimental measurements.

  10. Developing Ionic Liquid Know-How for the Design of Modular Functionality, Versatile Platforms, and New Synthetic Methodologies for Energetic Materials

    Science.gov (United States)

    2013-12-05

    filtration, and the filtrate checked for the presence of silver ions using HCl. The solvent was then evaporated at 80 °C under vacuum . A final...10. Graphene and Graphene Oxide Can ‘ Lubricate ’ Ionic Liquids based on Specific 36 Surface Interactions Leading to Improved Low Temperature...16-20[DCA]) salts were prepared by metathesis of the analogous halides (4-20[X]), either by using an ion exchange resin (nitrate salts) or a silver

  11. NOvel Fission Product Separation Based on Room-Temperature Ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    Hussey, Charles L.

    2005-11-13

    The effective extraction of Cs+ and Sr2+ into a relatively new and heretofore untested hydrophobic ionic liquid, tri-n-butylmethylammonium bis[(trifluoromethyl)sulfonyl]imide was demonstrated with calix[4]arene-bis(tert-octylbenzo-crown-6) and dicyclohexano-18-crown-6, respectively. The coordinated Cs+ and Sr2+ were subsequently removed from the ionic liquid extraction solvent by an electrochemical reduction process carried out at mercury electrodes. This process is non-destructive, permitting the ionic liquid and ionophores to be recycled. Although the process is based on mercury electrodes, this is a benefit rather than a detriment because the liquid mercury containing the Cs and Sr can be easily transported to another electrochemical cell where the Cs and Sr could be electrochemically recovered from the mercury amalgam and concentrated into a minimum volume of water or some other inexpensive solvent. This should facilitate the development of a suitable waste form for the extracted Cs+ and Sr2+. Thus, the feasibility of the proposed ionic liquid-based extraction cycle for the removal of 137Cs+ and 90Sr2+ from simulated aqueous tank waste was demonstrated.

  12. Solvation of an excess electron in pyrrolidinium dicyanamide based ionic liquids.

    Science.gov (United States)

    Xu, Changhui; Margulis, Claudio J

    2015-01-15

    In a recent article [J. Am. Chem. Soc. 2011, 133, 20186], we described the nature of the "dry" excess electron in a variety of different ionic liquids. We found that this could delocalize over cations or anions depending on the nature of the ions involved. A second article [J. Am. Chem. Soc. 2013, 135, 17528] explored the nature of the "dry to trapped" excess electron transition, the early localization dynamics, and associated spectroscopic signatures in alkylamonium and pyrrolidinium bis(trifluoromethylsulfonyl)amide based ionic liquids. In this study we predicted that the trapped electron localizes on an anion, resulting in fragmentation that is undesirable for photochemical, electrochemical, and radiation chemistry applications. The current work focuses instead on an ionic liquid based on the dicyanamide anion that on a time scale relevant to electron transfer and solvation dynamics does not appear to undergo facile fragmentation. Although electrochemical cathodic and anodic limits were correctly predicted by our recent study, it is unclear whether the reaction channels explored are necessarily those responsible for the observed near-infrared (NIR) band typical of excess electrons at long time. Could it be possible that the electrochemically relevant reaction channel is not necessarily the one giving rise to the NIR signal? This work attempts to approach such structural and dynamical aspects relevant to photodegradation, radiation chemistry, and electrochemistry in the case of pyrrolidinium dicyanamide based ionic liquids.

  13. Ionic Conductivity of Polyelectrolyte Hydrogels.

    Science.gov (United States)

    Lee, Chen-Jung; Wu, Haiyan; Hu, Yang; Young, Megan; Wang, Huifeng; Lynch, Dylan; Xu, Fujian; Cong, Hongbo; Cheng, Gang

    2018-02-14

    Polyelectrolytes have many important functions in both living organisms and man-made applications. One key property of polyelectrolytes is the ionic conductivity due to their porous networks that allow the transport of water and small molecular solutes. Among polyelectrolytes, zwitterionic polymers have attracted huge attention for applications that involve ion transport in a polyelectrolyte matrix; however, it is still unclear how the functional groups of zwitterionic polymer side chains affect their ion transport and swelling properties. In this study, zwitterionic poly(carboxybetaine acrylamide), poly(2-methacryloyloxyethyl phosphorylcholine), and poly(sulfobetaine methacrylate) hydrogels were synthesized and their ionic conductivity was studied and compared to cationic, anionic, and nonionic hydrogels. The change of the ionic conductivity of zwitterionic and nonionic hydrogels in different saline solutions was investigated in detail. Zwitterionic hydrogels showed much higher ionic conductivity than that of the widely used nonionic poly(ethylene glycol) methyl ether methacrylate hydrogel in all tested solutions. For both cationic and anionic hydrogels, the presence of mobile counterions led to high ionic conductivity in low salt solutions; however, the ionic conductivity of zwitterionic hydrogels surpassed that of cationic and ionic hydrogels in high salt solutions. Cationic and anionic hydrogels showed much higher water content than that of zwitterionic hydrogels in deionized water; however, the cationic hydrogels shrank significantly with increasing saline concentration. This work provides insight into the effects of polyelectrolyte side chains on ion transport. This can guide us in choosing better polyelectrolytes for a broad spectrum of applications, including bioelectronics, neural implants, battery, and so on.

  14. Liquid-Based Cytology of the Cerebrospinal Fluid in a Case of Cryptococcal Meningitis

    Directory of Open Access Journals (Sweden)

    Jiwoon Choi

    2018-01-01

    Full Text Available Cryptococcus neoformans is the most common microorganism found in cerebrospinal fluid (CSF cytology and causes life-threatening infections in immunocompromised hosts. Although its cytomorphologic features in conventional smear cytology have been well described, those in liquid-based cytology have rarely been. A 73-year-old woman with diffuse large B-cell lymphoma presented with mental confusion and a spiking fever. To rule out infectious conditions, CSF examination was performed. A cytology slide that was prepared using the ThinPrep method showed numerous spherical yeast-form organisms with diameters of 4–11 μm and thick capsules. Occasional asymmetrical, narrow-based budding but no true hyphae or pseudohyphae were observed. Gomori methenamine silver staining was positive. Cryptococcosis was confirmed in blood and CSF through the cryptococcal antigen test and culture. Liquid-based cytology allows for a clean background and additional slides for ancillary testing, facilitating the detection of microorganisms in CSF specimens, particularly when the number of organisms is small.

  15. Liquid-Based Cytology of the Cerebrospinal Fluid in a Case of Cryptococcal Meningitis.

    Science.gov (United States)

    Choi, Jiwoon; Kim, Se Hoon

    2018-01-01

    Cryptococcus neoformans is the most common microorganism found in cerebrospinal fluid (CSF) cytology and causes life-threatening infections in immunocompromised hosts. Although its cytomorphologic features in conventional smear cytology have been well described, those in liquid-based cytology have rarely been. A 73-year-old woman with diffuse large B-cell lymphoma presented with mental confusion and a spiking fever. To rule out infectious conditions, CSF examination was performed. A cytology slide that was prepared using the ThinPrep method showed numerous spherical yeast-form organisms with diameters of 4-11 μm and thick capsules. Occasional asymmetrical, narrow-based budding but no true hyphae or pseudohyphae were observed. Gomori methenamine silver staining was positive. Cryptococcosis was confirmed in blood and CSF through the cryptococcal antigen test and culture. Liquid-based cytology allows for a clean background and additional slides for ancillary testing, facilitating the detection of microorganisms in CSF specimens, particularly when the number of organisms is small.

  16. Raman spectral signatures of cervical exfoliated cells from liquid-based cytology samples

    Science.gov (United States)

    Kearney, Padraig; Traynor, Damien; Bonnier, Franck; Lyng, Fiona M.; O'Leary, John J.; Martin, Cara M.

    2017-10-01

    It is widely accepted that cervical screening has significantly reduced the incidence of cervical cancer worldwide. The primary screening test for cervical cancer is the Papanicolaou (Pap) test, which has extremely variable specificity and sensitivity. There is an unmet clinical need for methods to aid clinicians in the early detection of cervical precancer. Raman spectroscopy is a label-free objective method that can provide a biochemical fingerprint of a given sample. Compared with studies on infrared spectroscopy, relatively few Raman spectroscopy studies have been carried out to date on cervical cytology. The aim of this study was to define the Raman spectral signatures of cervical exfoliated cells present in liquid-based cytology Pap test specimens and to compare the signature of high-grade dysplastic cells to each of the normal cell types. Raman spectra were recorded from single exfoliated cells and subjected to multivariate statistical analysis. The study demonstrated that Raman spectroscopy can identify biochemical signatures associated with the most common cell types seen in liquid-based cytology samples; superficial, intermediate, and parabasal cells. In addition, biochemical changes associated with high-grade dysplasia could be identified suggesting that Raman spectroscopy could be used to aid current cervical screening tests.

  17. Ionic conductivity in irradiated KCL

    International Nuclear Information System (INIS)

    Vignolo Rubio, J.

    1979-01-01

    The ionic conductivity of X and gamma irradiated KCL single crystals has been studied between room temperature and 600 degree centigree. the radiation induced damage resulting in a decrease of the conductivity heals by thermal annealing in two steps which are at about 350 and 550 degree centigree respectively. It has been found that the radiation induced colour centres are not involved in the observed decrease of the ionic conductivity. However. It has been observed that the effects of quenching and plastic deformation on the conductivity of the samples are very similar to the effect induced by irradiation. It is suggested that, samples radiation induced dislocation loops might cause the ionic conductivity decrease observed in irradiated samples. (Author)

  18. Ionic conductivity in irradiated KCL

    International Nuclear Information System (INIS)

    Vignolo Rubio, J.

    1979-01-01

    The ionic conductivity of X and gamma irradiated KCl single crystals has been studied between room temperature and 600 deg C. The radiation induced damage resulting in a decrease of the conductivity heals by thermal annealing in two steps which are at about 350 and 550 deg C respectively. It has been found that the radiation induced colour centres are not involved in the observed decrease of the ionic conductivity. Howewer, it has been observed that the effects of quenching and plastic deformation on the conductivity of the samples are very similar to the effect induced by irradiation. It is suggested that small radiation induced dislocation loops might cause the ionic conductivity decrease observed in irradiated samples. (auth)

  19. Ionic conducting poly-benzimidazoles

    International Nuclear Information System (INIS)

    Jouanneau, J.

    2006-11-01

    Over the last years, many research works have been focused on new clean energy systems. Hydrogen fuel cell seems to be the most promising one. However, the large scale development of this technology is still limited by some key elements. One of them is the polymer electrolyte membrane 'Nafion' currently used, for which the ratio performance/cost is too low. The investigations we carried out during this thesis work are related to a new class of ionic conducting polymer, the sulfonated poly-benzimidazoles (sPBI). Poly-benzimidazoles (PBI) are aromatic heterocyclic polymers well-known for their excellent thermal and chemical stability. Ionic conduction properties are obtained by having strong acid groups (sulfonic acid SO 3 H) on the macromolecular structure. For that purpose, we first synthesized sulfonated monomers. Their poly-condensation with an appropriate non-sulfonated co-monomer yields to sPBI with sulfonation range from 0 to 100 per cent. Three different sPBI structures were obtained, and verified by appropriate analytical techniques. We also showed that the protocol used for the synthesis resulted in high molecular weights polymers. We prepared ionic conducting membrane by casting sPBI solutions on glass plates. Their properties of stability, water swelling and ionic conductivity were investigated. Surprisingly, the behaviour of sPBI was quite different from the other sulfonated aromatic polymers with same amount of SO 3 H, their stability was much higher, but their water swelling and ionic conductivity were quite low. We attributed these differences to strong ionic interactions between the sulfonic acid groups and the basic benzimidazole groups of our polymers. However, we managed to solve this problem synthesizing very highly sulfonated PBI, obtaining membranes with a good balance between all the properties necessary. (author)

  20. Local fields in ionic crystals

    International Nuclear Information System (INIS)

    Claro, F.

    1981-08-01

    Local fields arising from the electronic distortion in perfect ionic crystals are described in terms of multipolar excitations. Field factors for the alkali halides and chalcogenide ions are found to differ significantly from the Lorentz value of 4π/3, the correction size following an exponential dependence on the difference in ionic radii. Local fields are only slightly modified by these corrections however, and together with the Clausius-Mossotti relation may be regarded as accurate to within 2% if the Lorentz value is adopted. (author)

  1. Lithium ion conducting ionic electrolytes

    Science.gov (United States)

    Angell, C.A.; Xu, K.; Liu, C.

    1996-01-16

    A liquid, predominantly lithium-conducting, ionic electrolyte is described which has exceptionally high conductivity at temperatures of 100 C or lower, including room temperature. It comprises molten lithium salts or salt mixtures in which a small amount of an anionic polymer lithium salt is dissolved to stabilize the liquid against recrystallization. Further, a liquid ionic electrolyte which has been rubberized by addition of an extra proportion of anionic polymer, and which has good chemical and electrochemical stability, is described. This presents an attractive alternative to conventional salt-in-polymer electrolytes which are not cationic conductors. 4 figs.

  2. Surface tension of ionic liquids and ionic liquid solutions.

    Science.gov (United States)

    Tariq, Mohammad; Freire, Mara G; Saramago, Benilde; Coutinho, João A P; Lopes, José N Canongia; Rebelo, Luís Paulo N

    2012-01-21

    Some of the most active scientific research fronts of the past decade are centered on ionic liquids. These fluids present characteristic surface behavior and distinctive trends of their surface tension versus temperature. One way to explore and understand their unique nature is to study their surface properties. This critical review analyses most of the surface tension data reported between 2001 and 2010 (187 references).

  3. CO2/CH4 Separation Performance of Ionic-Liquid-Based Epoxy-Amine Ion Gel Membranes under Mixed Feed Conditions Relevant to Biogas Processing.

    Czech Academy of Sciences Publication Activity Database

    Friess, K.; Lanč, M.; Pilnáček, Kryštof; Fíla, V.; Vopička, O.; Sedláková, Zuzana; Cowan, M.G.; McDaniel, W.M.; Noble, R.D.; Gin, D.L.; Izák, Pavel

    2017-01-01

    Roč. 528, APRIL (2017), s. 64-71 ISSN 0376-7388 R&D Projects: GA ČR GA14-12695S; GA MŠk LH14006; GA TA ČR TE01020080 Institutional support: RVO:67985858 Keywords : epoxy-amine-based ion gel membranes * biogas processing * humid mixed-gas permeation Subject RIV: CI - Industrial Chemistry, Chemical Engineering OBOR OECD: Chemical process engineering Impact factor: 6.035, year: 2016

  4. Ionic liquid based on α-amino acid anion and N7,N9-dimethylguaninium cation ([dMG][AA]): theoretical study on the structure and electronic properties.

    Science.gov (United States)

    Shakourian-Fard, Mehdi; Fattahi, Alireza; Bayat, Ahmad

    2012-06-07

    The interactions between five amino acid based anions ([AA](-) (AA = Gly, Phe, His, Try, and Tyr)) and N7,N9-dimethylguaninium cation ([dMG](+)) have been investigated by the hybrid density functional theory method B3LYP together with the basis set 6-311++G(d,p). The calculated interaction energy was found to decrease in magnitude with increasing side-chain length in the amino acid anion. The interaction between the [dMG](+) cation and [AA](-) anion in the most stable configurations of ion pairs is a hydrogen bonding interaction. These hydrogen bonds (H bonds) were analyzed by the quantum theory of atoms in molecules (QTAIM) and natural bond orbital (NBO) analysis. Finally, several correlations between electron densities in bond critical points of hydrogen bonds and interaction energy as well as vibrational frequencies in the most stable configurations of ion pairs have been checked.

  5. CO2/CH4 Separation Performance of Ionic-Liquid-Based Epoxy-Amine Ion Gel Membranes under Mixed Feed Conditions Relevant to Biogas Processing.

    Czech Academy of Sciences Publication Activity Database

    Friess, K.; Lanč, M.; Pilnáček, Kryštof; Fíla, V.; Vopička, O.; Sedláková, Zuzana; Cowan, M.G.; McDaniel, W.M.; Noble, R.D.; Gin, D.L.; Izák, Pavel

    2017-01-01

    Roč. 528, APRIL (2017), s. 64-71 ISSN 0376-7388 R&D Projects: GA ČR GA14-12695S; GA MŠk LH14006; GA TA ČR TE01020080 Institutional support: RVO:67985858 Keywords : epoxy-amine-based ion gel membranes * biogas processing * humid mixed- gas permeation Subject RIV: CI - Industrial Chemistry, Chemical Engineering OBOR OECD: Chemical process engineering Impact factor: 6.035, year: 2016

  6. Ionic liquid-tolerant cellulase enzymes

    Energy Technology Data Exchange (ETDEWEB)

    Gladden, John; Park, Joshua; Singer, Steven; Simmons, Blake; Sale, Ken

    2017-10-31

    The present invention provides ionic liquid-tolerant cellulases and method of producing and using such cellulases. The cellulases of the invention are useful in saccharification reactions using ionic liquid treated biomass.

  7. Electric Current Fluctuations, Entropy and Ionic Conductivity

    OpenAIRE

    Zhang, Yong-Jun

    2016-01-01

    This paper reports a relation between ionic conductivity and electric current fluctuations. The relation was derived using statistical analysis and entropy approach. The relation can be used to calculate ionic conductivity.

  8. Nanoparticle enhanced ionic liquid heat transfer fluids

    Science.gov (United States)

    Fox, Elise B.; Visser, Ann E.; Bridges, Nicholas J.; Gray, Joshua R.; Garcia-Diaz, Brenda L.

    2014-08-12

    A heat transfer fluid created from nanoparticles that are dispersed into an ionic liquid is provided. Small volumes of nanoparticles are created from e.g., metals or metal oxides and/or alloys of such materials are dispersed into ionic liquids to create a heat transfer fluid. The nanoparticles can be dispersed directly into the ionic liquid during nanoparticle formation or the nanoparticles can be formed and then, in a subsequent step, dispersed into the ionic liquid using e.g., agitation.

  9. Ionic-Liquid-Tethered Nanoparticles: Hybrid Electrolytes

    KAUST Repository

    Moganty, Surya S.

    2010-10-22

    A new class of solventless electrolytes was created by tethering ionic liquids to hard inorganic ZrO2 nanostructures (see picture; NIM=nanoscale ionic material). These hybrid fluids exhibit exceptional redox stability windows, excellent thermal stability, good lithium transference numbers, long-term interfacial stability in the presence of a lithium anode and, when doped with lithium salt, reasonable ionic conductivities.

  10. Continuum electrostatics for ionic solutions with non-uniform ionic sizes

    International Nuclear Information System (INIS)

    Li Bo

    2009-01-01

    This work concerns electrostatic properties of an ionic solution with multiple ionic species of possibly different ionic sizes. Such properties are described by the minimization of an electrostatic free-energy functional of ionic concentrations. Bounds are obtained for ionic concentrations with low electrostatic free energies. Such bounds are used to show that there exists a unique set of equilibrium ionic concentrations that minimizes the free-energy functional. The equilibrium ionic concentrations are found to depend sorely on the equilibrium electrostatic potential, resembling the classical Boltzmann distributions that relate the equilibrium ionic concentrations to the equilibrium electrostatic potential. Unless all the ionic and solvent molecular sizes are assumed to be the same, explicit formulae of such dependence are, however, not available in general. It is nevertheless proved that in equilibrium the ionic charge density is a decreasing function of the electrostatic potential. This determines a variational principle with a convex functional for the electrostatic potential

  11. Phase behavior of ionic microemulsions

    NARCIS (Netherlands)

    Lekkerkerker, H.N.W.; Kegel, W.K.; Overbeek, J.Th.G.

    1996-01-01

    Non-polar oils and water can form thermodynamically stable quasi-homogeneous (colloidal) mixtures (called microemulsions) in the presence of relatively large amounts (several %) of ionic surfactants. If the surfactant contains a single hydrocarbon chain (e.g. Sodium Dodecyl Sulphate) the presence of

  12. Fluctuating hydrodynamics for ionic liquids

    Science.gov (United States)

    Lazaridis, Konstantinos; Wickham, Logan; Voulgarakis, Nikolaos

    2017-04-01

    We present a mean-field fluctuating hydrodynamics (FHD) method for studying the structural and transport properties of ionic liquids in bulk and near electrified surfaces. The free energy of the system consists of two competing terms: (1) a Landau-Lifshitz functional that models the spontaneous separation of the ionic groups, and (2) the standard mean-field electrostatic interaction between the ions in the liquid. The numerical approach used to solve the resulting FHD-Poisson equations is very efficient and models thermal fluctuations with remarkable accuracy. Such density fluctuations are sufficiently strong to excite the experimentally observed spontaneous formation of liquid nano-domains. Statistical analysis of our simulations provides quantitative information about the properties of ionic liquids, such as the mixing quality, stability, and the size of the nano-domains. Our model, thus, can be adequately parameterized by directly comparing our prediction with experimental measurements and all-atom simulations. Conclusively, this work can serve as a practical mathematical tool for testing various theories and designing more efficient mixtures of ionic liquids.

  13. Ionic liquid-dispersive liquid-liquid microextraction for the simultaneous determination of pesticides and metabolites in soils using high-performance liquid chromatography and fluorescence detection.

    Science.gov (United States)

    Asensio-Ramos, María; Hernández-Borges, Javier; Borges-Miquel, Teresa M; Rodríguez-Delgado, Miguel Ángel

    2011-07-29

    In this work, an ionic liquid-dispersive liquid-liquid microextraction (IL-DLLME) procedure was developed for the extraction of a group of pesticides (carbendazim/benomyl, thiabendazole, fuberidazole, carbaryl and triazophos) and some of their key metabolites in soils (2-aminobenzimidazole, metabolite of carbendazim and 1-naphthol, metabolite of carbaryl) from aqueous soil extracts, using high performance liquid chromatography (HPLC) with fluorescence detection (FD). Analytes were previously extracted from four soils with different physicochemical properties (forestal, ornamental, garden and lapilli soils) by ultrasound-assisted extraction (USE). The IL 1-hexyl-3-methylimidazolium hexafluorophosphate ([HMIm][PF(6)]) and methanol (MeOH) were used as extraction and dispersion solvent, respectively, for the DLLME procedure. Factors affecting IL-DLLME (sample pH, IL amount, volume of dispersion solvent and sodium chloride percentage) were optimized by means of an experimental design, obtaining the most favorable results when using 117.5 mg of IL and 418 μL of MeOH to extract the compounds from the aqueous soil extracts at pH 5.20 containing 30% (w/v) NaCl. Calibration of the USE-IL-DLLME-HPLC-FD method was carried out for every type of soil and accuracy and precision studies were developed at two levels of concentration, finding that no significant differences existed between real and spiked concentrations (Student's t test). LODs achieved were in the low ng/g range. Copyright © 2010 Elsevier B.V. All rights reserved.

  14. Oligomerization of ethylene catalysed by nickel complexes associated with nitrogen ligands in ionic liquids; Oligomerisation de l'ethylene catalysee par des complexes du nickel associes a des ligands azotes dans les liquides ioniques

    Energy Technology Data Exchange (ETDEWEB)

    Lecocq, V.

    2003-09-01

    We report here the use of a new class of catalytic systems based on a nickel active center associated with nitrogen ligands, such as di-imines, or imino-pyridines, for the oligomerization of ethylene in a biphasic medium using ionic liquids as the catalyst solvent. The nickel catalyst is immobilized in the ionic liquid phase in which the olefinic reaction products are poorly miscible. This biphasic system makes possible an easy separation and recycle of the catalyst. Numerous di-imine and imino-pyridine ligands with different steric and electronic properties have been synthesized and their corresponding nickel complexes isolated and characterized. Different ionic liquids, based on chloro-aluminates or non-chloro-aluminates anions, have also been prepared and characterized. The effect of the nature of the ligand, the ionic liquid, the nickel precursor and its mode of activation have been studied and correlated with the selectivity and activity of the transformation of ethylene. (author)

  15. Ionic conductivity studies of gel polyelectrolyte based on ionic liquid

    Energy Technology Data Exchange (ETDEWEB)

    Cha, E.H. [The Faculty of Liberal Arts (Chemistry), Hoseo University, Asan Choongnam 336-795 (Korea); Lim, S.A. [Functional Proteomics Center, Korea Institute of Science and Technology, Seoul 136-791 (Korea); Park, J.H. [Department of Herbal Medicine, Hoseo University, Asan Choongnam 336-795 (Korea); Kim, D.W. [Department of Chemical Technology, Han Bat National University, Daejon 305-719 (Korea); Macfarlane, D.R. [School of Chemistry, Monash University, Clayton, Vic. 3800 (Australia)

    2008-04-01

    Novel lithium polyelectrolyte-ionic liquids have been prepared and characterized of their properties. Poly(lithium 2-acrylamido-2-methyl propanesulfonate) (PAMPSLi) and its copolymer with N-vinyl formamide (VF) also has been prepared as a copolymer. 1-Ethyl-3-methylimidazolium tricyanomethanide (emImTCM) and N,N-dimethyl-N-propyl-N-butyl ammonium tricyanomethanide (N{sub 1134}TCM) which are chosen because of the same with the anion of ionic liquid were prepared. The ionic conductivity of copolymer system (PAMPSLi/PVF/emImTCM: 5.43 x 10{sup -3} S cm{sup -1} at 25 C) exhibits about over four times higher than that of homopolymer system (PAMPSLi/emImTCM: 1.28 x 10{sup -3} S cm{sup -1} at 25 C). Introduction of vinyl formamide into the copolymer type can increase the dissociation of the lithium cations from the polymer backbone. The ionic conductivity of copolymer with emImTCM (PAMPSLi/PVF/emImTCM) exhibits the higher conductivity than that of PAMPSLi/PVF/N{sub 1134}TCM (2.48 x 10{sup -3} S cm{sup -1}). Because of using the polymerizable anion it is seen to maintain high flexibility of imidazolium cation effectively to exhibit the higher conductivity. And also the viscosity of emImTCM (19.56 cP) is lower than that of N{sub 1134}TCM (28.61 cP). Low viscosity leads to a fast rate of diffusion of redox species. (author)

  16. Synthesis and physical properties of new layered double hydroxides based on ionic liquids: Application to a polylactide matrix

    KAUST Repository

    Livi, Sébastien

    2012-12-01

    Ionic liquids based on tetraalkylphosphonium salts combined with different anions (decanoate and dodecylsulfonate) have been used as intercalating agents of layered double hydroxides (LDHs) by ion