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Sample records for ionic liquid-based ultrasound-assisted

  1. A novel method: ionic liquid-based ultrasound-assisted extraction of polyphenols from Chinese purple yam.

    Science.gov (United States)

    Zhang, Junhong; Zong, Aizhen; Xu, Tongcheng; Zhan, Ping; Liu, Lina; Qiu, Bin; Liu, Wei; Jia, Min; Du, Fangling; Tian, Honglei

    2017-08-24

    Chinese purple yam is famous for therapeutic and nutritional values in lowering blood glucose, blood pressure and even preventing and treating cardiovascular diseases. However, traditional extraction techniques for the functional polyphenolic compounds mostly utilise unfriendly organic solvent and easily cause degradation of polyphenols. In this study, a novel ionic liquid-based ultrasound-assisted extraction (IL-UAE) technique was utilised to obtain polyphenols. The optimal extraction condition included: solid-liquid ratio (0.05 g/mL), ionic liquid concentration (1.05 M), extraction temperature (67°C) and ultrasonic time (37 min). The maximum free radical scavenging activity (86.21%) and total antioxidant activity (2.21 mM) were achieved and matched well with the predicted values, superior to that of the extract from regular ethanol-based UAE. IL-UAE could be a rapid and green technique for efficient extraction of polyphenols from purple yam with low solvent consumption and few structural deterioration, exhibiting application potential in food and pharmaceutical industries.

  2. 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.

  3. Determination of atenolol in human plasma using ionic-liquid-based ultrasound-assisted in situ solvent formation microextraction followed by high-performance liquid chromatography.

    Science.gov (United States)

    Zeeb, Mohsen; Farahani, Hadi; Papan, Mohammad Kazem

    2016-06-01

    An efficient analytical method called ionic-liquid-based ultrasound-assisted in situ solvent formation microextraction followed by high-performance liquid chromatography was developed for the determination of atenolol in human plasma. A hydrophobic ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate) was formed by the addition of a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate) to a sample solution containing an ion-pairing agent during microextraction. The analyte was extracted into the ionic liquid phase while the microextraction solvent was dispersed throughout the sample by utilizing ultrasound. The sample was then centrifuged, and the extracting phase retracted into the microsyringe and injected to liquid chromatography. After optimization, the calibration curve showed linearity in the range of 2-750 ng/mL with the regression coefficient corresponding to 0.998. The limits of detection (S/N = 3) and quantification (S/N = 10) were 0.5 and 2 ng/mL, respectively. A reasonable relative recovery range of 90-96.7% and satisfactory intra-assay (4.8-5.1%, n = 6) and interassay (5.0-5.6%, n = 9) precision along with a substantial sample clean-up demonstrated good performance of the procedure. It was applied for the determination of atenolol in human plasma after oral administration and some pharmacokinetic data were obtained.

  4. Ionic liquid-based ultrasound-assisted emulsification microextraction coupled with high performance liquid chromatography for the determination of four fungicides in environmental water samples.

    Science.gov (United States)

    Liang, Pei; Wang, Fang; Wan, Qin

    2013-02-15

    A highly efficient and environmentally friendly sample preparation method termed ionic liquid-based ultrasound-assisted emulsification microextraction (IL-USAEME) combined with high performance liquid chromatography has been developed for the determination of four fungicides (azoxystrobin, diethofencarb, pyrimethanil and kresoxim-methyl) in water samples. In this novel approach, ionic liquid (IL) was used as extraction solvent in place of the organic solvent used in conventional USAEME assay, and there is no need for using organic dispersive solvent which is typically required in the common dispersive liquid-liquid microextraction method. Various parameters that affect the extraction efficiency, such as the kind and volume of IL, ultrasound emulsification time, extraction temperature and salt addition were investigated and optimized. Under the optimum extraction condition, the linearities of calibration curves were in the range from 3 to 5000 ng mL(-1) for target analytes with the correlation coefficient higher than 0.9992. The enrichment factors and the limits of detection were in the range of 88-137 and 0.73-2.2 ng mL(-1), depending on the analytes. The environmental water samples were successfully analyzed using the proposed method, and the relative recoveries at fortified levels of 50 and 100 ng mL(-1) were in the range of 83.9%-116.2%.

  5. Ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry for a sensitive determination of cadmium in water samples

    Energy Technology Data Exchange (ETDEWEB)

    Li Shengqing [Department of Chemistry, College of Science, Huazhong Agricultural University, Wuhan 430070 (China); Supervision, Inspection and Testing Center of Microbial Products Quality (Wuhan), Ministry of Agriculture (China)], E-mail: sqingli@mail.hzau.edu.cn; Cai Shun; Hu Wei [Department of Chemistry, College of Science, Huazhong Agricultural University, Wuhan 430070 (China); Chen Hao [Department of Chemistry, College of Science, Huazhong Agricultural University, Wuhan 430070 (China)], E-mail: hchenhao@mail.hzau.edu.cn; Liu Hanlan [Department of Chemistry, College of Science, Huazhong Agricultural University, Wuhan 430070 (China)

    2009-07-15

    A new method was developed for the determination of cadmium in water samples using ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction (IL-based USA-DLLME) followed by electrothermal atomic absorption spectrometry (ETAAS). The IL-based USA-DLLME procedure is free of volatile organic solvents, and there is no need for a dispersive solvent, in contrast to conventional DLLME. The ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate (HMIMPF{sub 6}), was quickly disrupted by an ultrasonic probe for 1 min and dispersed in water samples like a cloud. At this stage, a hydrophobic cadmium-DDTC complex was formed and extracted into the fine droplets of HMIMPF{sub 6}. After centrifugation, the concentration of the enriched cadmium in the sedimented phase was determined by ETAAS. Some effective parameters of the complex formation and microextraction, such as the concentration of the chelating agent, the pH, the volume of the extraction solvent, the extraction time, and the salt effect, have been optimized. Under optimal conditions, a high extraction efficiency and selectivity were reached for the extraction of 1.0 ng of cadmium in 10.0 mL of water solution employing 73 {mu}L of HMIMPF{sub 6} as the extraction solvent. The enrichment factor of the method is 67. The detection limit was 7.4 ng L{sup - 1}, and the characteristic mass (m{sub 0}, 0.0044 absorbance) of the proposed method was 0.02 pg for cadmium (Cd). The relative standard deviation (RSD) for 11 replicates of 50 ng L{sup - 1} Cd was 3.3%. The method was applied to the analysis of tap, well, river, and lake water samples and the Environmental Water Reference Material GSBZ 50009-88 (200921). The recoveries of spiked samples were in the range of 87.2-106%.

  6. Ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry for a sensitive determination of cadmium in water samples

    Science.gov (United States)

    Li, Shengqing; Cai, Shun; Hu, Wei; Chen, Hao; Liu, Hanlan

    2009-07-01

    A new method was developed for the determination of cadmium in water samples using ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction (IL-based USA-DLLME) followed by electrothermal atomic absorption spectrometry (ETAAS). The IL-based USA-DLLME procedure is free of volatile organic solvents, and there is no need for a dispersive solvent, in contrast to conventional DLLME. The ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate (HMIMPF 6), was quickly disrupted by an ultrasonic probe for 1 min and dispersed in water samples like a cloud. At this stage, a hydrophobic cadmium-DDTC complex was formed and extracted into the fine droplets of HMIMPF 6. After centrifugation, the concentration of the enriched cadmium in the sedimented phase was determined by ETAAS. Some effective parameters of the complex formation and microextraction, such as the concentration of the chelating agent, the pH, the volume of the extraction solvent, the extraction time, and the salt effect, have been optimized. Under optimal conditions, a high extraction efficiency and selectivity were reached for the extraction of 1.0 ng of cadmium in 10.0 mL of water solution employing 73 µL of HMIMPF 6 as the extraction solvent. The enrichment factor of the method is 67. The detection limit was 7.4 ng L - 1 , and the characteristic mass ( m0, 0.0044 absorbance) of the proposed method was 0.02 pg for cadmium (Cd). The relative standard deviation (RSD) for 11 replicates of 50 ng L - 1 Cd was 3.3%. The method was applied to the analysis of tap, well, river, and lake water samples and the Environmental Water Reference Material GSBZ 50009-88 (200921). The recoveries of spiked samples were in the range of 87.2-106%.

  7. 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.

  8. Determination of metal ions in tea samples using task-specific ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction coupled to liquid chromatography with ultraviolet detection.

    Science.gov (United States)

    Werner, Justyna

    2016-04-01

    Task-specific ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction was used for the preconcentration of cadmium(II), cobalt(II), and lead(II) ions in tea samples, which were subsequently analyzed by liquid chromatography with UV detection. The proposed method of preconcentration is free of volatile organic compounds, which are often used as extractants and dispersing solvents in classic techniques of microextraction. A task-specific ionic liquid trioctylmethylammonium thiosalicylate was used as an extractant and a chelating agent. Ultrasound was used to disperse the ionic liquid. After microextraction, the phases were separated by centrifugation, and the ionic liquid phase was solubilized in methanol and directly injected into the liquid chromatograph. Selected microextraction parameters, such as the volume of ionic liquid, the pH of the sample, the duration of ultrasound treatment, the speed and time of centrifugation, and the effect of ionic strength, were optimized. Under optimal conditions an enrichment factor of 200 was obtained for each analyte. The limits of detection were 0.002 mg/kg for Cd(II), 0.009 mg/kg for Co(II), and 0.013 mg/kg for Pb(II). The accuracy of the proposed method was evaluated by an analysis of the Certified Reference Materials (INCT-TL-1, INCT-MPH-2) with the recovery values in the range of 90-104%.

  9. Ionic liquid-based ultrasound-assisted extraction and aqueous two-phase system for analysis of caffeoylquinic acids from Flos Lonicerae Japonicae.

    Science.gov (United States)

    Tan, Ting; Lai, Chang-Jiang-Sheng; OuYang, Hui; He, Ming-Zhen; Feng, Yulin

    2016-02-20

    In this work, an ionic liquid-based ultrasonic-assisted extraction (ILUAE) method was developed to extract caffeoylquinic acids (CQAs) from Flos Lonicerae Japonicae (FLJ). ILUAE parameters were optimized by response surface methodology, including IL concentration, ultrasonic time, and liquid-solid ratio. Optimized ILUAE approach gained the highest extraction yields of 28.53, 18.21, 3.84mg/g for 3-O-caffeoylquinic acid (C1), 3,5-di-O-caffeoylquinic acid (C2), 3,4-di-O-caffeoylquinic acid (C3), respectively. C1-C3 are the three most abundant CQAs compounds in FLJ. The method showed comparable extraction yield and shorter extraction time compared with conventional extraction techniques. Subsequently, an aqueous two-phase system (ATPS) was applied in extraction solutions. Two trace CQAs, 5-O-caffeoylquinic acid (C4) and 4,5-di-O-caffeoylquinic acid (C5), were significantly enriched with signal to noise values increasing from less than 10 to higher than 1475. The results indicated that ILUAE and ATPS are efficient and environmentally-friendly sample extraction and enrichment techniques for CQAs from herbal medicines.

  10. Temperature-controlled ionic liquid-based ultrasound-assisted microextraction for preconcentration of trace quantity of cadmium and nickel by using organic ligand in artificial saliva extract of smokeless tobacco products

    Science.gov (United States)

    Arain, Sadaf Sadia; Kazi, Tasneem Gul; Arain, Asma Jabeen; Afridi, Hassan Imran; Baig, Jameel Ahmed; Brahman, Kapil Dev; Naeemullah; Arain, Salma Aslam

    2015-03-01

    A new approach was developed for the preconcentration of cadmium (Cd) and nickel (Ni) in artificial saliva extract of dry snuff (brown and black) products using temperature-controlled ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction (TIL-UDLLμE) followed by electrothermal atomic absorption spectrometry (ETAAS). The Cd and Ni were complexed with ammonium pyrrolidinedithiocarbamate (APDC), extracted in ionic liquid drops, 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6]. The multivariate strategy was applied to estimate the optimum values of experimental variables influence the % recovery of analytes by TIL-UDLLμE method. At optimum experimental conditions, the limit of detection (3s) were 0.05 and 0.14 μg L-1 while relative standard deviations (% RSD) were 3.97 and 3.55 for Cd and Ni respectively. After extraction, the enhancement factors (EF) were 87 and 79 for Cd and Ni, respectively. The RSD for six replicates of 10 μg L-1 Cd and Ni were 3.97% and 3.55% respectively. To validate the proposed method, certified reference material (CRM) of Virginia tobacco leaves was analyzed, and the determined values of Cd and Ni were in good agreement with the certified values. The concentration of Cd and Ni in artificial saliva extracts corresponds to 39-52% and 21-32%, respectively, of the total contents of both elements in dry brown and black snuff products.

  11. 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.

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

    Science.gov (United States)

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

    2012-01-01

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

  13. 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.

  14. Spectrophotometric determination of iron species using ionic liquid ultrasound assisted dispersive liquid--liquid microextraction

    OpenAIRE

    BAZMANDEGAN, ALIREZA; Shabani,Ali Mohammad Haji; DADFARNIA, SAYESSTEH; Saeidi, Mahboubeh; Moghadam,Masoud Rohani

    2015-01-01

    A simple and efficient method for speciation and determination of iron in different water samples was developed. The method is based on ionic liquid ultrasound assisted dispersive liquid--liquid microextraction (IL-USA-DLLME) followed by spectrophotometric determination. Fe(II) is complexed with 2,4,6-tri(2'-pyridyl)-l,3,5-triazine (TPTZ{)}, neutralized through ion pair formation with sodium dodecyl sulfate (SDS) and extracted into 1-hexyl-3-methylimidazolium hexafluorophosphate [C$_...

  15. 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.

  16. Ionic liquid ultrasound assisted dispersive liquid-liquid microextraction method for preconcentration of trace amounts of rhodium prior to flame atomic absorption spectrometry determination

    Energy Technology Data Exchange (ETDEWEB)

    Molaakbari, Elaheh [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Young Research Society, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Mostafavi, Ali, E-mail: mostafavi.ali@gmail.com [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Afzali, Daryoush [Environment and Nanochemistry Department, Research Institute of Environmental Science, International Center for Science, High Technology and Environmental Science, Kerman (Iran, Islamic Republic of); Mineral Industries Research Center, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

    2011-01-30

    In this article, we consider ionic liquid based ultrasound-assisted dispersive liquid-liquid microextraction of trace amounts of rhodium from aqueous samples and show that this is a fast and reliable sample pre-treatment for the determination of rhodium ions by flame atomic absorption spectrometry. The Rh(III) was transferred into its complex with 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol as a chelating agent, and an ultrasonic bath with the ionic liquid, 1-octyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide at room temperature was used to extract the analyte. The centrifuged rhodium complex was then enriched in the form of ionic liquid droplets and prior to its analysis by flame atomic absorption spectrometry, 300 {mu}L ethanol was added to the ionic liquid-rich phase. Finally, the influence of various parameters on the recovery of Rh(III) was optimized. Under optimum conditions, the calibration graph was linear in the range of 4.0-500.0 ng mL{sup -1}, the detection limit was 0.37 ng mL{sup -1} (3S{sub b}/m, n = 7) and the relative standard deviation was {+-}1.63% (n = 7, C = 200 ng mL{sup -1}). The results show that ionic liquid based ultrasound assisted dispersive liquid-liquid microextraction, combined with flame atomic absorption spectrometry, is a rapid, simple, sensitive and efficient analytical method for the separation and determination of trace amounts of Rh(III) ions with minimum organic solvent consumption.

  17. An ionic liquid based strain sensor for large displacement measurement.

    Science.gov (United States)

    Keulemans, Grim; Ceyssens, Frederik; Puers, Robert

    2017-03-01

    A robust and low cost ionic liquid based strain sensor is fabricated for high strain measurements in biomedical applications (up to 40 % and higher). A tubular 5 mm long silicone microchannel with an inner diameter of 310 µm and an outer diameter of 650 µm is filled with an ionic liquid. Three ionic liquids have been investigated: 1-butyl-1-methylpyrrolidinium bis (trifluoromethylsulfonyl) imide, ethylammonium nitrate and cholinium ethanoate. When the channel is axially stretched, geometrical deformations change the electrical impedance of the liquid channel. The sensors display a linear response and low hysteresis with an average gauge factors of 1.99 for strains up to 40 %. Additionally, to fix the sensor by surgical stitching to soft biological tissue, a sensor with tube clamps consisting of photopatternable SU-8 epoxy-based resin is proposed.

  18. Ionic liquid-based stable nanofluids containing gold nanoparticles.

    Science.gov (United States)

    Wang, Baogang; Wang, Xiaobo; Lou, Wenjing; Hao, Jingcheng

    2011-10-01

    A one-phase and/or two-phase method were used to prepare the stable ionic liquid-based nanofluids containing same volume fraction but different sizes or surface states of gold nanoparticles (Au NPs) and their thermal conductivities were investigated in more detail. Five significant experiment parameters, i.e. temperature, dispersion condition, particle size and surface state, and viscosity of base liquid, were evaluated to supply experimental explanations for heat transport mechanisms. The conspicuously temperature-dependent and greatly enhanced thermal conductivity under high temperatures verify that Brownian motion should be one key effect factor in the heat transport processes of ionic liquid-based gold nanofluids. While the positive influences of proper aggregation and the optimized particle size on their thermal conductivity enhancements under some specific conditions demonstrate that clustering may be another critical effect factor in heat transport processes. Moreover, the remarkable difference of the thermal conductivity enhancements of the nanofluids containing Au NPs with different surface states could be attributed to the surface state which has a strong correlation with not only Brownian motion but also clustering. Whilst the close relationship between their thermal conductivity enhancements and the viscosity of base liquid further indicate Brownian motion must occupy the leading position among various influencing factors. Finally, a promisingly synergistic effect of Brownian motion and clustering based on experimental clues and theoretical analyses was first proposed, justifying different mechanisms are sure related. The results may shed lights on comprehensive understanding of heat transport mechanisms in nanofluids.

  19. Ultrasound-assisted magnetic solid-phase extraction based ionic liquid-coated Fe3O4@graphene for the determination of nitrobenzene compounds in environmental water samples.

    Science.gov (United States)

    Cao, Xiaoji; Shen, Lingxiao; Ye, Xuemin; Zhang, Feifei; Chen, Jiaoyu; Mo, Weimin

    2014-04-21

    An ultrasound-assisted magnetic solid-phase extraction procedure with the [C7MIM][PF6] ionic liquid-coated Fe3O4-grafted graphene nanocomposite as the magnetic adsorbent has been developed for the determination of five nitrobenzene compounds (NBs) in environmental water samples, in combination with high performance liquid chromatography-photodiode array detector (HPLC-PDA). Several significant factors that affect the extraction efficiency, such as the types of magnetic nanoparticle and ionic liquid, the volume of ionic liquid and the amount of magnetic nanoparticles, extraction time, ionic strength, and solution pH, were investigated. With the assistance of ultrasound, adsorbing nitrobenzene compounds by ionic liquid and self-aggregating ionic liquid onto the surface of the Fe3O4-grafted graphene proceeded synchronously, which made the extraction achieved the maximum within 20 min using only 144 μL [C7MIM][PF6] and 3 mg Fe3O4-grafted graphene. Under the optimized conditions, satisfactory linearities were obtained for all NBs with correlation coefficients larger than 0.9990. The mean recoveries at two spiked levels ranged from 80.35 to 102.77%. Attributed to the convenient magnetic separation, the Fe3O4-grafted graphene could be recycled many times. The proposed method was demonstrated to be feasible, simple, solvent-saving and easy to operate for the trace analysis of NBs in environmental water samples.

  20. Thermoreversible (Ionic-Liquid-Based) Aqueous Biphasic Systems.

    Science.gov (United States)

    Passos, Helena; Luís, Andreia; Coutinho, João A P; Freire, Mara G

    2016-02-04

    The ability to induce reversible phase transitions between homogeneous solutions and biphasic liquid-liquid systems, at pre-defined and suitable operating temperatures, is of crucial relevance in the design of separation processes. Ionic-liquid-based aqueous biphasic systems (IL-based ABS) have demonstrated superior performance as alternative extraction platforms, and their thermoreversible behaviour is here disclosed by the use of protic ILs. The applicability of the temperature-induced phase switching is further demonstrated with the complete extraction of two value-added proteins, achieved in a single-step. It is shown that these temperature-induced mono(bi)phasic systems are significantly more versatile than classical liquid-liquid systems which are constrained by their critical temperatures. IL-based ABS allow to work in a wide range of temperatures and compositions which can be tailored to fit the requirements of a given separation process.

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

    Directory of Open Access Journals (Sweden)

    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.

  2. 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.

  3. Determination of eight fluoroquinolones in groundwater samples with ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction prior to high-performance liquid chromatography and fluorescence detection.

    Science.gov (United States)

    Vázquez, M M Parrilla; Vázquez, P Parrilla; Galera, M Martínez; García, M D Gil

    2012-10-20

    An ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction (US-IL-DLLME) procedure was developed for the extraction of eight fluoroquinolones (marbofloxacin, norfloxacin, ciprofloxacin, lomefloxacin, danofloxacin, enrofloxacin, oxolinic acid and nalidixic acid) in groundwater, using high-performance liquid chromatography with fluorescence detection (HPLC-FD). The ultrasound-assisted process was applied to accelerate the formation of the fine cloudy solution using a small volume of disperser solvent (0.4 mL of methanol), which increased the extraction efficiency and reduced the equilibrium time. For the DLLME procedure, the IL 1-octyl-3-methylimidazolium hexafluorophosphate ([C(8)MIM] [PF(6)]) and methanol (MeOH) were used as extraction and disperser solvent, respectively. By comparing [C(8)MIM] [PF(6)] with 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM] [PF(6)]) and 1-butyl-3-methylimidazolium hexafluorophosphate ([C(4)MIM] [PF(6)]) as extraction solvents, it was observed that when using [C(8)MIM] [PF(6)] the cloudy solution was formed more readily than when using [C(6)MIM] [PF(6)] or [C(4)MIM] [PF(6)]. The factors affecting the extraction efficiency, such as the type and volume of ionic liquid, type and volume of disperser solvent, cooling in ice-water, sonication time, centrifuging time, sample pH and ionic strength, were optimised. A slight increase in the recoveries of fluoroquinolones was observed when an ice-water bath extraction step was included in the analytical procedure (85-107%) compared to those obtained without this step (83-96%). Under the optimum conditions, linearity of the method was observed over the range 10-300 ng L(-1) with correlation coefficient >0.9981. The proposed method has been found to have excellent sensitivity with limit of detection between 0.8 and 13 ng L(-1) and precision with relative standard deviation values between 4.8 and 9.4% (RSD, n=5). Good enrichment factors (122-205) and recoveries (85

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

    Science.gov (United States)

    Berton, Paula; Martinis, Estefanía M; Martinez, Luis D; Wuilloud, Rodolfo G

    2012-02-03

    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(6)mim][PF(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(-1), while the relative standard deviation (RSD) was 4.7% (at 0.5 μg L(-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. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. 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.

  6. Ionic liquid-based materials: a platform to design engineered CO2 separation membranes.

    Science.gov (United States)

    Tomé, Liliana C; Marrucho, Isabel M

    2016-05-21

    During the past decade, significant advances in ionic liquid-based materials for the development of CO2 separation membranes have been accomplished. This review presents a perspective on different strategies that use ionic liquid-based materials as a unique tuneable platform to design task-specific advanced materials for CO2 separation membranes. Based on compilation and analysis of the data hitherto reported, we provide a judicious assessment of the CO2 separation efficiency of different membranes, and highlight breakthroughs and key challenges in this field. In particular, configurations such as supported ionic liquid membranes, polymer/ionic liquid composite membranes, gelled ionic liquid membranes and poly(ionic liquid)-based membranes are detailed, discussed and evaluated in terms of their efficiency, which is attributed to their chemical and structural features. Finally, an integrated perspective on technology, economy and sustainability is provided.

  7. In-situ metathesis reaction combined with ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction method for the determination of phenylurea pesticides in water samples.

    Science.gov (United States)

    Zhang, Jiaheng; Liang, Zhe; Li, Songqing; Li, Yubo; Peng, Bing; Zhou, Wenfeng; Gao, Haixiang

    2012-08-30

    A novel microextraction technique, named in-situ metathesis reaction, combined with ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction was developed for the determination of five phenylurea pesticides (i.e., diuron, diflubenzuron, teflubenzuron, flufenoxuron, and chlorfluazuron) in environmental water samples. In the developed method, 360 μL LiNTf(2) aqueous solution (0.162 g/mL) was added to the sample solution containing a small amount of [C(6)MIM]Cl (0.034 g) to form a water-immiscible ionic liquid, [C(6)MIM]NTf(2), as extraction solution. The mixed solutions were placed in an ultrasonic water bath at 150 W for 4min and centrifuged at 3500 rpm for 10 min to achieve phase separation. After centrifugation, fine droplets of the extractant phase settled to the bottom of the centrifuge tube and were directly injected into the high-performance liquid chromatography system for analysis. The quantity of [C(6)MIM]Cl, the molar ratio of [C(6)MIM]Cl and LiNTf(2), ionic strength, ultrasound time, and centrifugation time, were optimized using a Plackett-Burman design. Significant factors obtained were optimized by employing a central composite design. The optimized technique provides good repeatability (RSD 2.4 to 3.5%), linearity (0.5 μg/L to 500 μg/L), low LODs (0.06 μg/L to 0.08 μg/L) and great enrichment factor (244 to 268). The developed method can be applied in routine analysis for the determining of phenylurea pesticides in environmental samples.

  8. 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.

  9. 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.

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

    Science.gov (United States)

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

    2015-12-04

    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.

  11. Development of novel ionic liquids based on biological molecules

    OpenAIRE

    Zalewska, Karolina Anna Maria

    2014-01-01

    Ionic Liquids (ILs) belong to a class of compounds with unusual properties: very low vapour pressure; high chemical and thermal stability and the ability to dissolve a wide range of substances. A new field in research is evaluating the possibility to use natural chiral biomolecules for the preparation of chiral ionic liquids (CILs). This important challenge in synthetic chemistry can open new avenues of research in order to avoid some problems related with the intrinsic biodegradability and t...

  12. Purification of Astaxanthin from Laminariajaponica by Ionic Liquid-based Monolithic Cartridge

    Institute of Scientific and Technical Information of China (English)

    YOON Chang-hwan; ZHU Tao; ROW Kyung-ho

    2012-01-01

    An effective and accurate method was developed for the extraction of astaxanthin from Laminariajaponica with subsequent separation by ionic liquid-based monolithic cartridge.The optimized extraction conditions including extraction solvent(ethanol),extraction time(90 min) and ultrasonic power(75 W) were obtained by systematical investigation.Chromatographic analysis was performed on a C18 column with ultraviolet(UV) detection at 476nm,and a solution consisting of methanol/acetonitrile/H20/dichloromethane(83:6:6:5,volume ratio) was used as the mobile phase at a flow rate of 0.7 mL/min.After ionic liquid-based monolithic solid phase extraction,17.82 μg/g astaxanthin was obtained from Laminariajaponica.This ionic liquid-based monolithic cartridge exhibits high affinity and selectivity for astaxanthin,and it can be potentially used as the stationary phase of high performance liquid chromatography( HPLC).

  13. Energetic Ionic Liquids Based on Lanthanide Nitrate Complex Anions (Postprint)

    Science.gov (United States)

    2008-01-01

    xH2O (x=27–44) [5a] and lanthanide complexes of the pseudohalide SCN in the hydrolytically unstable [ bmim ]4Ln ACHTUNGTRENNUNG(SCN)7·H2O ( bmim =1-butyl-3...Wiley-VCH Verlag GmbH&Co. KGaA, Weinheim These are not the final page numbers! &1& FULL PAPER cal ionic liquids. The instability of [ bmim ]4Ln... bmim ]4Ln ACHTUNGTRENNUNG(SCN)7·H2O ionic liquids by displacing the isothiocyanate ligand.[5b] In our syntheses, guanidinium ni- trate and lanthanum or

  14. New, ionic liquid-based membranes for lithium battery application

    Energy Technology Data Exchange (ETDEWEB)

    Sirisopanaporn, C.; Fernicola, A.; Scrosati, B. [Department of Chemistry, University of Rome La Sapienza, 00185 Rome (Italy)

    2009-01-15

    New types of dimensionally stable, flexible gel-type electrolyte membranes with a relatively wide electrochemical stability, high lithium ion conductivity and other desirable properties have been prepared by immobilizing N-n-butyl-N-ethylpyrrolidinium N,N-bis(trifluoromethane)sulfonimide-lithium N,N-bis(trifluoromethane)sulfonimide (Py{sub 24}TFSI-LiTFSI), ionic liquid, IL, solutions in a poly(vinylidene fluoride)-hexafluoropropylene copolymer (PVdF-HFP) matrix. The addition of a discrete amount of ethylene and propylene carbonate (EC-PC), solvent mixture to the membranes resulted in an improvement of the ionic conductivity and in a stabilization of the interface with the lithium electrode. These IL-based gel type membranes can operate without degradation up to a temperature of 110 C where they reach conductivity values of the order of 10{sup -2} S cm{sup -1}. All these properties make these polymer electrolyte membranes of interest for applications as separators in advanced lithium batteries. (author)

  15. Lithium conducting ionic liquids based on lithium borate salts

    Energy Technology Data Exchange (ETDEWEB)

    Zygadlo-Monikowska, E.; Florjanczyk, Z.; Sluzewska, K.; Ostrowska, J.; Langwald, N.; Tomaszewska, A. [Warsaw University of Technology, Faculty of Chemistry, ul. Noakowskiego 3, 00-664 Warsaw (Poland)

    2010-09-15

    The simple reaction of trialkoxyborates with butyllithium resulted in the obtaining of new lithium borate salts: Li{l_brace}[CH{sub 3}(OCH{sub 2}CH{sub 2}){sub n}O]{sub 3}BC{sub 4}H{sub 9}{r_brace}, containing oxyethylene substituents (EO) of n=1, 2, 3 and 7. Salts of n {>=} 2 show properties of room temperature ionic liquid (RTIL) of low glass transition temperature, T{sub g} of the order from -70 to -80 C. The ionic conductivity of the salts depends on the number of EO units, the highest conductivity is shown by the salt with n = 3; in bulk its ambient temperature conductivity is 2 x 10{sup -5} S cm{sup -1} and in solution in cyclic propylene sulfite or EC/PC mixture, conductivity increases by an order of magnitude. Solid polymer electrolytes with borate salts over a wide concentration range, from 10 to 90 mol.% were obtained and characterized. Three types of polymeric matrices: poly(ethylene oxide) (PEO), poly(trimethylene carbonate) (PTMC) and two copolymers of acrylonitrile and butyl acrylate p(AN-BuA) were used in them as polymer matrices. It has been found that for systems of low salt concentration (10 mol.%) the best conducting properties were shown by solid polymer electrolytes with PEO, whereas for systems of high salt concentration, of the polymer-in-salt type, good results were achieved for PTMC as polymer matrix. (author)

  16. 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

  17. 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.

  18. 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.

  19. A novel ionic liquids-based scrubbing process for efficient CO2 capture

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    A novel alkanolamine-based ionic liquid,N-methyl-diethanolammonium tetrafluoroborate ([MDEA][BF4]),was synthesized in our laboratory.The ionic liquid-based composite solution consisting of N-methyl-diethanolamine (MDEA),[MDEA][BF4],piperazine (PZ) and H2O was investigated for CO2 capture.The optimal performance for CO2 capture was found at 45°C,1.50 MPa,probably due to a synergistic action of the reaction and the transport.No apparent corrosion was found on stainless and carbon steel with the above composite solution.This finding is very significant to the promotion of its engineering application.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-01-15

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

  1. Highly Stretchable, Hysteresis-Free Ionic Liquid-Based Strain Sensor for Precise Human Motion Monitoring.

    Science.gov (United States)

    Choi, Dong Yun; Kim, Min Hyeong; Oh, Yong Suk; Jung, Soo-Ho; Jung, Jae Hee; Sung, Hyung Jin; Lee, Hyung Woo; Lee, Hye Moon

    2017-01-18

    A highly stretchable, low-cost strain sensor was successfully prepared using an extremely cost-effective ionic liquid of ethylene glycol/sodium chloride. The hysteresis performance of the ionic-liquid-based sensor was able to be improved by introducing a wavy-shaped fluidic channel diminishing the hysteresis by the viscoelastic relaxation of elastomers. From the simulations on visco-hyperelastic behavior of the elastomeric channel, we demonstrated that the wavy structure can offer lower energy dissipation compared to a flat structure under a given deformation. The resistance response of the ionic-liquid-based wavy (ILBW) sensor was fairly deterministic with no hysteresis, and it was well-matched to the theoretically estimated curves. The ILBW sensors exhibited a low degree of hysteresis (0.15% at 250%), low overshoot (1.7% at 150% strain), and outstanding durability (3000 cycles at 300% strain). The ILBW sensor has excellent potential for use in precise and quantitative strain detections in various areas, such as human motion monitoring, healthcare, virtual reality, and smart clothes.

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

    Science.gov (United States)

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

    2010-12-15

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

  3. Ionic liquids based on dicyanamide anion: influence of structural variations in cationic structures on ionic conductivity.

    Science.gov (United States)

    Yoshida, Yukihiro; Baba, Osamu; Saito, Gunzi

    2007-05-10

    A series of dicyanamide [N(CN)2]-based ionic liquids were prepared using 1-alkyl-3-methylimidazolium cations with different alkyl chain lengths and ethyl-containing heterocyclic cations with different ring structures, and the influence of such structural variations on their thermal property, density, electrochemical window, viscosity, ionic conductivity, and solvatochromic effects was investigated. We found that the 1,3-dimethylimidazolium salt shows the highest ionic conductivity among ionic liquids free from halogenated anions (3.6 x 10(-2) S cm(-1) at 25 degrees C), and the elongation of the alkyl chain causes the pronounced depression of fluidity and ionic conductivity. Also, such an elongation gives rise to the increase in the degree of ion association in the liquids, mainly caused by the van der Waals interactions between alkyl chains. N(CN)2 salts with 1-ethyl-2-methylpyrazolium (EMP) and N-ethyl-N-methylpyrrolidinium (PY(12)) cations as well as 1-ethyl-3-methylimidazolium (EMI) cation are liquids at room temperature (RT), while the N-ethylthiazolium salt shows a melting event at higher temperature (57 degrees C). Among the three RT ionic liquids with ethyl-containing cations, RT ionic conductivity follows the order EMI > PY(12) > EMP, which does not coincide with the order of fluidity at RT (EMI > EMP > PY(12)). Such a discrepancy is originated from a high degree of ion dissociation in the PY(12) salt, which was manifested in the Walden rule deviation and solvatochromic effects. A series of N(CN)2/C(CN)3 binary mixtures of the EMI salts were also prepared. RT ionic conductivity decreases linearly with increasing the molar fraction of C(CN)3 anion.

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

    Science.gov (United States)

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

    2016-01-15

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

  5. Ionic liquids based on S-alkylthiolanium cations and TFSI anion as potential electrolytes

    Institute of Scientific and Technical Information of China (English)

    ZHANG HuanQi; YANG Li; FANG ShaoHua; PENG ChengXin; LUO HongJun

    2009-01-01

    New ionic liquids based on S-alkylthiolanium cations with TFSI anions were synthesized and charac-terized.The physical and electrochemical properties,including melting point,thermal stability,solubil-ity,viscosity,conductivity and electrochemical window,were reported.Relation between these proper-ties and the structure of the cations was discussed.In this series,T4TFSI and T5TFSI have melting points below -60℃,and their conductivities are 2.10 mS/cm and 1.46 mS/cm;their electrochemical windows are 4.1 V and 4.5 V at room temperature.These cyclic alkylthiolanium-based ionic liquids are promising as novel electrolytes in various electrochemical devices,especially under low temperature condition.

  6. Pretreatment of Lignocellulosic Biomass with Ionic Liquids and Ionic Liquid-Based Solvent Systems

    OpenAIRE

    Qidong Hou; Meiting Ju; Weizun Li; Le Liu; Yu Chen; Qian Yang

    2017-01-01

    Pretreatment is very important for the efficient production of value-added products from lignocellulosic biomass. However, traditional pretreatment methods have several disadvantages, including low efficiency and high pollution. This article gives an overview on the applications of ionic liquids (ILs) and IL-based solvent systems in the pretreatment of lignocellulosic biomass. It is divided into three parts: the first deals with the dissolution of biomass in ILs and IL-based solvent systems; ...

  7. Pretreatment of Lignocellulosic Biomass with Ionic Liquids and Ionic Liquid-Based Solvent Systems.

    Science.gov (United States)

    Hou, Qidong; Ju, Meiting; Li, Weizun; Liu, Le; Chen, Yu; Yang, Qian

    2017-03-20

    Pretreatment is very important for the efficient production of value-added products from lignocellulosic biomass. However, traditional pretreatment methods have several disadvantages, including low efficiency and high pollution. This article gives an overview on the applications of ionic liquids (ILs) and IL-based solvent systems in the pretreatment of lignocellulosic biomass. It is divided into three parts: the first deals with the dissolution of biomass in ILs and IL-based solvent systems; the second focuses on the fractionation of biomass using ILs and IL-based solvent systems as solvents; the third emphasizes the enzymatic saccharification of biomass after pretreatment with ILs and IL-based solvent systems.

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

    Science.gov (United States)

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

    2012-02-24

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-02-24

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

  10. Pretreatment of Lignocellulosic Biomass with Ionic Liquids and Ionic Liquid-Based Solvent Systems

    Directory of Open Access Journals (Sweden)

    Qidong Hou

    2017-03-01

    Full Text Available Pretreatment is very important for the efficient production of value-added products from lignocellulosic biomass. However, traditional pretreatment methods have several disadvantages, including low efficiency and high pollution. This article gives an overview on the applications of ionic liquids (ILs and IL-based solvent systems in the pretreatment of lignocellulosic biomass. It is divided into three parts: the first deals with the dissolution of biomass in ILs and IL-based solvent systems; the second focuses on the fractionation of biomass using ILs and IL-based solvent systems as solvents; the third emphasizes the enzymatic saccharification of biomass after pretreatment with ILs and IL-based solvent systems.

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

    Science.gov (United States)

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

    2015-10-01

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

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

    Science.gov (United States)

    Sadi, Maryam

    2017-07-01

    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.

  13. Determination of pyrethroid pesticides in tomato using ionic liquid-based dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Han, Dandan; Tang, Baokun; Row, Kyung Ho

    2014-03-01

    A sensitive determination method was developed for the analysis of pyrethroid pesticide residues in tomato samples using ionic liquid-based dispersive liquid-liquid microextraction. A hydrophobic ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate) and acetonitrile were used as the extraction solvent and dispersive solvent, respectively. The following experimental parameters affecting the extraction efficiency were examined: types of extraction solvent and volume of extraction solvent, types of dispersive solvent and volume of dispersive solvent and pH and ion strength of the sample solution. Under the optimum conditions, the extraction recoveries ranged from 83.9 to 96.7%. Moreover, the enrichment factors for esbiothrin, fenpropathrin and cyhalothrin were 42, 48 and 45, respectively. The calibration curves were linear with correlation coefficients ranging from 0.9997 to 0.9999 at concentrations of 0.05-1.5 µg/kg. The relative standard deviation (n = 5) was 1.7-4.5%. The limits of detection for esbiothrin, fenpropathrin and cyhalothrin were 8.1, 9.9 and 14.3 µg/kg, respectively.

  14. Ionic liquid based dispersive liquid-liquid microextraction of aromatic amines in water samples

    Institute of Scientific and Technical Information of China (English)

    Yun Chang Fan; Zheng Liang Hu; Mei Lan Chen; Chao Shen Tu; Yan Zhu

    2008-01-01

    In this work, a new microextraction method termed ionic liquid based dispersive liquid-liquid microextraction (IL-DLLME) was demonstrated for the extraction of 2-methylaniline, 4-chloroaniline, 1-naphthylamine and 4-aminobiphenyl in aqueous matrices. After extraction the ionic liquid (IL) phase was injected directly into the high performance liquid chromatography (HPLC) system for determination. Some parameters that might affect the extraction efficiency were optimized. Under the optimum conditions, good linear relationship, sensitivity and reproducibility were obtained. The limits of detection (LOD, S/N = 3) for the four analytes were in the range of 0.45-2.6 μg L-1. The relative standard deviations (R.S.D., n = 6) were in the range of 6.2-9.8%. This method was applied for the analysis of the real water samples. The recoveries ranged from 93.4 to 106.4%. The main advantages of the method are high speed, high recovery, good repeatability and volatile organic solvent-free.

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

    Science.gov (United States)

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

    2011-11-30

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

  16. Comparison of the performance of conventional, temperature-controlled, and ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction combined with high-performance liquid chromatography in analyzing pyrethroid pesticides in honey samples.

    Science.gov (United States)

    Zhang, Jiaheng; Gao, Haixiang; Peng, Bing; Li, Songqing; Zhou, Zhiqiang

    2011-09-23

    This research paper presents a comparative study of the performance of conventional, ultrasound-assisted (UA), and temperature-controlled (TC) ionic liquid (IL) dispersive liquid-phase microextraction (IL-DLLME). Various parameters that affect extraction efficiency, such as type and volume of extraction and disperser solvent, centrifugation time, salt addition, effect of temperature on TC-IL-DLLME, and effect of sonication time on UA-IL-DLLME, were evaluated. UA-IL-DLLME was found to provide the best extraction efficiency. Under optimized conditions, great enrichment factors (506-515) and good recoveries (101.2-103.0%) were obtained by analyte extraction in real samples. The limit of detections (LODs) ranged from 0.21 to 0.38 μg L(-1). Good linearity was obtained in the range of 0.5-200 μg L(-1) for ethofenprox and tetramethrin, and 1-200 μg L(-1) for meperfluthrin and alpha-cypermethrin. Based on optimized conditions, the UA-IL-DLLME method was applied and combined with high-performance liquid chromatography with diode array detection (HPLC-DAD) to determine the presence of ethofenprox, tetramethrin, meperfluthrin, and alpha-cypermethrin in honey samples.

  17. Advances in the electrodeposition of aluminum from ionic liquid based electrolytes

    Science.gov (United States)

    Leadbetter, Kirt C.

    Aluminum plating is of considerable technical and economic interest because it provides an eco-friendly substitute for cadmium coatings used on many military systems. However, cadmium has been determined to be a significant environmental safety and occupational health (ESOH) hazard because of its toxicity and carcinogenic nature. Furthermore, the cost of treating and disposing of generated wastes, which often contain cyanide, is costly and is becoming prohibitive in the face of increasingly stringent regulatory standards. The non-toxic alternative aluminum is equivalent or superior in performance to cadmium. In addition, it could serve to provide an alternative to hexavalent chromium coatings used on military systems for similar reasons to that of cadmium. Aluminum is a beneficial alternative in that it demonstrates self-healing corrosion resistance in the form of a tightly-bound, impervious oxide layer. A successfully plated layer would be serviceable over a wider temperature range, 925 °F for aluminum compared to 450 oF for cadmium. In addition, an aluminum layer can be anodized to make it non-conducting and colorable. In consideration of the plating process, aluminum cannot be deposited from aqueous solutions because of its reduction potential. Therefore, nonaqueous electrolytes are required for deposition. Currently, aluminum can be electrodeposited in nonaqueous processes that use hazardous chemicals such as toluene and pyrophoric aluminum alkyls. Electrodeposition from ionic liquids provides the potential for a safer method that could be easily scaled up for industrial application. The plating process could be performed at a lower temperature and higher current density than other commercially available aluminum electrodeposition processes; thus a reduced process cost could be possible. The current ionic liquid based electrolytes are more expensive; however production on a larger scale and a long electrolyte lifetime are associated with a reduction in price

  18. Ionic liquid-based zwitterionic organic polymer monolithic column for capillary hydrophilic interaction chromatography.

    Science.gov (United States)

    Wang, Tingting; Chen, Yihui; Ma, Junfeng; Zhang, Xiaodan; Zhang, Lihua; Zhang, Yukui

    2015-08-21

    In the current study, a novel ionic liquid-based zwitterionic organic polymer monolithic column was developed by copolymerizing 1-vinyl-3-(butyl-4-sulfonate) imidazolium, acrylamide and N,N'-methylenebisacrylamide in a quaternary porogenic solvent consisting of formamide, dimethyl sulphoxide, polyethylene glycol 8000 and polyethylene glycol 10,000 for capillary hydrophilic interaction chromatography. The monolithic stationary phase was optimized by adjusting the amount of monomer in the polymerization solution along with the composition of porogenic solvent. The optimized monolith exhibited excellent selectivity and favorable retention for nucleosides and benzoic acid derivatives. The primary factors affecting the separation efficiency of the monolithic column (including acetonitrile content, pH, and buffer salt concentration in the mobile phase) have been thoroughly evaluated. Excellent reproducibility of the retention times for five nucleosides was achieved, with relative standard deviations of run-to-run (n = 3), column-to-column (n = 3) and batch-to-batch (n = 3) in the range of 0.18-0.48%, 2.33-4.20% and 3.07-6.50%, respectively.

  19. Multi-phase extraction of glycoraphanin from broccoli using aminium ionic liquid-based silica.

    Science.gov (United States)

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

    2013-01-01

    Glucosinolates, a class of phytochemicals found in broccoli, have attracted recent interest due to the potential health benefits associated with their dietary intake. Glucoraphanin, the most common glucosinolate in broccoli can be converted to a known cancer chemopreventive agent. Multi-phase extraction in solid-phase extraction cartridges was developed to simultaneously extract and separate this compound. Multi-phase extraction with functionalised ionic liquid-based silica as a sorbent was used to simultaneously extract and separate glucoraphanin from broccoli. The sorbent and broccoli sample were packed into a single cartridge, and a fixed volume of water was then used to extract and remove the target compound from the sample to the sorbent over 15 repetitions. The sorbent was then washed with n-hexane to remove any interference and the target compound was eluted with water-1% acetic acid (vol.). Under the optimised condition, 0.038 mg/g of glucoraphanin was obtained by multi-phase extraction with 0.2 g of sorbent. The adsorption isotherm allowed investigation of the interactions between the sorbent and target compound and provided evidence for the accuracy of this method. The low deviation error, small amount of solvents required, highly selective separation and stability of the method justify further research. Copyright © 2012 John Wiley & Sons, Ltd.

  20. 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.

  1. Application of Film-forming Additives for Ionic Liquid Based Electrolyte

    Institute of Scientific and Technical Information of China (English)

    孙敏倩; 胡志强; 蔡迎军; 董陶; 吕兴梅

    2012-01-01

    N-methyl-N-propylpiperidinium bis(trifluoromethanesulfonyl)imide was synthesized for the application in ionic liquid based electrolytes in lithium ion battery,10% vinylene carbonate (VC) and 10% 1,3-propane sultone (PS) were added to the electrolyte system respectively as additives to improve the property of solid electrolyte interface and cyclic performance.The results of cyclic voltammetry showed that homogenous and compact solid electrolyte interface film formed on graphite electrode which was detected by observing the morphology of cycled graphite anode,Charging and discharging performance of LiFePO4/Li half cell was tested in the electrolyte with or without additives.The initial specific discharging capacities were increased to 129.4 and 123.0 mA·h/g by the addition of VC and PS,respectively,compared with that of additive-free electrolyte.The discharging retentions were 88.9% and 84.6% in electrolyte containing VC and PS after 10 cycles.

  2. Pre-concentration and determination of amitriptyline residues in waste water by ionic liquid based immersed droplet microextraction and HPLC

    Institute of Scientific and Technical Information of China (English)

    M.T. Hamed Mosavian; Z. Es'haghi; N. Razavi; S. Banihashemi

    2012-01-01

    This paper describes a new approach for the determination of amitriptyline in wastewater by ionic liquid based immersed droplet microextraction (IL-IDME) prior to highperformance liquid chromatography with ultraviolet detection. 1-Hexyl-3-methylimidazolium hexafluorophosphate ([C6MIM][PF6]) was used as an ionic liquid. Various factors that affect extraction, such as volume of ionic liquid, stirring rate, extraction time, pH of the aqueous solution and salting effect, were optimized. The optimal conditions were as follows: microextraction time, 10 min; stirring rate, 720 rpm; pH, 11; ionic drop volume, 100 uL; and no sodium chloride addition. In quantitative experiments the method showed linearity in a range from 0.01 to 10 ug/mL, a limit of detection of 0.004 ug/mL and an excellent pre-concentration factor (PF) of 1100. Finally, the method was successfully applied to the determination of amitriptyline in the hospital wastewater samples.

  3. Efficient production of free fatty acids from ionic liquid-based acid- or enzyme-catalyzed bamboo hydrolysate.

    Science.gov (United States)

    Mi, Le; Qin, Dandan; Cheng, Jie; Wang, Dan; Li, Sha; Wei, Xuetuan

    2017-03-01

    Two engineered Escherichia coli strains, DQ101 (MG1655 fadD (-))/pDQTES and DQ101 (MG1655 fadD (-))/pDQTESZ were constructed to investigate the free fatty acid production using ionic liquid-based acid- or enzyme-catalyzed bamboo hydrolysate as carbon source in this study. The plasmid, pDQTES, carrying an acyl-ACP thioesterase 'TesA of E. coli in pTrc99A was constructed firstly, and then (3R)-hydroxyacyl-ACP dehydratase was ligated after the TesA to give the plasmid pDQTESZ. These two strains exhibited efficient fatty acid production when glucose was used as the sole carbon source, with a final concentration of 2.45 and 3.32 g/L, respectively. The free fatty acid production of the two strains on xylose is not as efficient as that on glucose, which was 2.32 and 2.96 g/L, respectively. For mixed sugars, DQ101 (MG1655 fadD (-))-based strains utilized glucose and pentose sequentially under the carbon catabolite repression (CCR) regulation. The highest total FFAs concentration from the mixed sugar culture reached 2.81 g/L by DQ101 (MG1655 fadD (-))/pDQTESZ. Furthermore, when ionic liquid-based enzyme-catalyzed bamboo hydrolysate was used as the carbon source, the strain DQ101 (MG1655 fadD (-))/pDQTESZ could produce 1.23 g/L FFAs with a yield of 0.13 g/g, and while it just produced 0.65 g/L free fatty acid with the ionic liquid-based acid-catalyzed bamboo hydrolysate as the feedstock. The results suggested that enzymatic catalyzed bamboo hydrolysate with ionic liquid pretreatment could serve as an efficient feedstock for free fatty acid production.

  4. Ionic-liquid-based proton conducting membranes for anhydrous H2/Cl2 fuel-cell applications.

    Science.gov (United States)

    Liu, Sa; Zhou, Li; Wang, Pengjie; Zhang, Fangfang; Yu, Shuchun; Shao, Zhigang; Yi, Baolian

    2014-03-12

    An ionic-liquid-doped poly(benzimidazole) (PBI) proton-conducting membrane for an anhydrous H2/Cl2 fuel cell has been proposed. Compared with other ionic liquids, such as imidazole-type ionic liquids, diethylmethylammonium trifluoromethanesulfonate ([dema][TfO]) showed better electrode reaction kinetics (H2 oxidation and Cl2 reduction reaction at platinum) and was more suitable for a H2/Cl2 fuel cell. PBI polymer and [dema][TfO] were compatible with each other, and the hybrid membranes exhibited high stability and good ionic conductivity, reaching 20.73 mS cm(-1) at 160 °C. We also analyzed the proton-transfer mechanism in this ionic-liquid-based membrane and considered that both proton-hopping and diffusion mechanisms existed. In addition, this composite electrolyte worked well in a H2/Cl2 fuel cell under non-water conditions. This work would give a good path to study the novel membranes for anhydrous H2/Cl2 fuel-cell application.

  5. Novel Brønsted-acidic ionic liquids based on benzothiazolium cations as catalysts for esterification reactions

    Directory of Open Access Journals (Sweden)

    Song Hang

    2011-01-01

    Full Text Available Three novel Brønsted-acidic ionic liquids based on benzothiazolium cations were prepared, which served as catalysts for the synthesis of benzoic esters. All three gave good yields of the target esters in esterification reactions. Moreover, they combine the advantages of both homogeneous and heterogeneous solid catalysts in esterification reactions, which enabled them to serve as homogeneous catalysts to catalyze the reactions and be conveniently recovered by simple filtration after the reactions. They could be reused several times without noticeable decrease in efficiency.

  6. 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.

  7. Theoretical study of ionic liquids based on the cholinium cation. Ab initio simulations of their condensed phases

    Science.gov (United States)

    Campetella, Marco; Bodo, Enrico; Montagna, Maria; De Santis, Serena; Gontrani, Lorenzo

    2016-03-01

    We have explored by means of ab initio molecular dynamics the homologue series of 11 different ionic liquids based on the combination of the cholinium cation with deprotonated amino acid anions. We present a structural analysis of the liquid states of these compounds as revealed by accurate ab initio computations of the forces. We highlight the persistent structural motifs that see the ionic couple as the basic building block of the liquid whereby a strong hydrogen bonding network substantially determines the short range structural behavior of the bulk state. Other minor docking features of the interaction network are also discovered and described. Special cases along the series such as Cysteine and Phenylalanine are discussed in the view of their peculiar properties due to zwitterion formation and additional long-range structural organization.

  8. Energetic Ionic Liquids Based on Anionic Rare Earth Nitrate Complexes (Preprint)

    Science.gov (United States)

    2008-07-10

    hydrolytically unstable [ bmim ]Ln(SCN)7. [5b] However, the former exist as hydrates and are not stable in the absence of water of hydration and are not typical...ionic liquids. The instability of [ bmim ]Ln(SCN)7 to moisture and air also limits their applications. Since our new rare-earth ionic liquids do not...component in energetic ionic liquids.[7] Rare earth metals coordinate with O-donor ligands more strongly than N-donor ligands,[8] e. g., in [ bmim ]Ln

  9. Deep Extractive Desulfurization of Gasoline with Ionic Liquids Based on Metal Halide

    Institute of Scientific and Technical Information of China (English)

    Wang Haojie; He Jianxun; Yang Cairong; Zhang Hang

    2014-01-01

    Ionic liquid [Et3NH]Cl-FeCl3/CuCl was synthesized by mixing [Et3NH]Cl, anhydrous FeCl3 and anhydrous CuCl, and the desulfurization activity of this ionic liquid was tested. It exhibited remarkable ability in effective desulfurization of model gasoline (thiophene in n-octane) and lfuid catalytic cracking (FCC) gasoline, and the sulfur removal of thiophene in model oil (V(IL):V(oil)=0.08) could reach 93.9%in 50 min at 50℃. Low-sulfur (﹤10μg/g) FCC gasoline could be obtained after three extraction runs at an ionic liquid/oil volume ratio of 0.1, with the yield of FCC gasoline reaching 94.3%. The ionic liquid could be recycled 5 times with merely a slight decrease in activity.

  10. A dual-emissive ionic liquid based on an anionic platinum(II) complex

    OpenAIRE

    Ogawa, Tomohiro; Yoshida, Masaki; Ohara, Hiroki; Kobayashia, Atsushi; Kato, Masako

    2015-01-01

    An ionic liquid fabricated froman anionic cyclometalated platinum(II) complex and an imidazolium cation exhibits dual emission from the monomeric and aggregated forms of the platinum complex anions, leading to temperature-dependent color changes of luminescence.

  11. A dual-emissive ionic liquid based on an anionic platinum(ii) complex.

    Science.gov (United States)

    Ogawa, Tomohiro; Yoshida, Masaki; Ohara, Hiroki; Kobayashi, Atsushi; Kato, Masako

    2015-09-07

    An ionic liquid fabricated from an anionic cyclometalated platinum(ii) complex and an imidazolium cation exhibits dual emission from the monomeric and aggregated forms of the platinum complex anions, leading to temperature-dependent color changes of luminescence.

  12. Experimental investigations of an ionic-liquid-based, magnesium ion conducting, polymer gel electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Pandey, G.P.; Hashmi, S.A. [Department of Physics and Astrophysics, University of Delhi, Delhi 110007 (India)

    2009-02-15

    Studies on a novel magnesium ion conducting gel polymer electrolyte based on a room temperature ionic liquid (RTIL) is reported. It comprises a Mg-salt, Mg(CF{sub 3}SO{sub 3}){sub 2} [or magnesium triflate, Mg(Tf){sub 2}] solution in an ionic liquid, 1-ethyl-3-methylimidazolium trifluoro-methanesulfonate (EMITf), immobilized with poly(vinylidene fluoride-hexafluoropropylene) (PVdF-HFP), which is a freestanding, semitransparent and flexible film with excellent mechanical strength. Physical and electrochemical analyses demonstrate promising characteristics of these films, suitable as electrolytes in rechargeable magnesium batteries. The material offers a maximum electrical conductivity of {proportional_to}4.8 x 10{sup -3} S cm{sup -1} at room temperature (20 C) with excellent thermal and electrochemical stabilities. Possible conformational changes in the polymer host PVdF-HFP due to ionic liquid solution entrapment and ion-polymer interaction are investigated by Fourier transform infra-red (FTIR), X-ray diffraction (XRD) and scanning electron microscopic (SEM) methods. The Mg{sup 2+} ion transport in the gel film is confirmed from cyclic voltammetry, impedance and transport number measurements. The Mg{sup 2+} ion transport number (t{sub +}) is {proportional_to}0.26, which indicates a substantial contribution of triflate anion transport along with ionic conduction due to the component ions of the ionic liquid. (author)

  13. Experimental investigations of an ionic-liquid-based, magnesium ion conducting, polymer gel electrolyte

    Science.gov (United States)

    Pandey, G. P.; Hashmi, S. A.

    Studies on a novel magnesium ion conducting gel polymer electrolyte based on a room temperature ionic liquid (RTIL) is reported. It comprises a Mg-salt, Mg(CF 3SO 3) 2 [or magnesium triflate, Mg(Tf) 2] solution in an ionic liquid, 1-ethyl-3-methylimidazolium trifluoro-methanesulfonate (EMITf), immobilized with poly(vinylidene fluoride-hexafluoropropylene) (PVdF-HFP), which is a freestanding, semitransparent and flexible film with excellent mechanical strength. Physical and electrochemical analyses demonstrate promising characteristics of these films, suitable as electrolytes in rechargeable magnesium batteries. The material offers a maximum electrical conductivity of ∼4.8 × 10 -3 S cm -1 at room temperature (20 °C) with excellent thermal and electrochemical stabilities. Possible conformational changes in the polymer host PVdF-HFP due to ionic liquid solution entrapment and ion-polymer interaction are investigated by Fourier transform infra-red (FTIR), X-ray diffraction (XRD) and scanning electron microscopic (SEM) methods. The Mg 2+ ion transport in the gel film is confirmed from cyclic voltammetry, impedance and transport number measurements. The Mg 2+ ion transport number (t +) is ∼0.26, which indicates a substantial contribution of triflate anion transport along with ionic conduction due to the component ions of the ionic liquid.

  14. Aqueous ionic liquid based ultrasonic assisted extraction of four acetophenones from the Chinese medicinal plant Cynanchum bungei Decne.

    Science.gov (United States)

    Sun, Yinshi; Liu, Zhengbo; Wang, Jianhua; Yang, Saifei; Li, Baiqing; Xu, Ning

    2013-01-01

    In this study, an aqueous ionic liquid based ultrasonic assisted extraction (ILUAE) method for the extraction of the four acetophenones, namely 4-hydroxyacetophenone (1), 2,5-dihydroxyacetophenone (2), baishouwubenzophenone (3) and 2,4-dihydroxyacetophenone (4) from the Chinese medicinal plant Cynanchum bungei was developed. Three kinds of aqueous l-alkyl-3-methylimidazolium ionic liquids with different anion and alkyl chain were investigated. The results indicated that ionic liquids (ILs) showed remarkable effects on the extraction efficiency of acetophenones. In addition, the ILUAE, including several ultrasonic parameters, such as the ILs concentration, solvent to solid ratio, power, particle size, temperature, and extraction time have been optimized. Under these optimal conditions (e.g., with 0.6M [C(4)MIM]BF(4), solvent to solid ratio of 35:1, power of 175 W, particle size of 60-80 mesh, temperature of 25 ° C and time of 50 min), this approach gained the highest extraction yields of four acetophenones 286.15, 21.65, 632.58 and 205.38 μg/g, respectively. The proposed approach has been evaluated by comparison with the conventional heat-reflux extraction (HRE) and regular UAE. The results indicated that ILUAE is an alternative method for extracting acetophenones from C. bungei.

  15. Prediction of the Physical Properties for the Ionic Liquid Based on Topological Index

    Institute of Scientific and Technical Information of China (English)

    SHU Qing; YANG Bo-Lun; WANG Fu-An

    2005-01-01

    Based on the distance matrix and adjacent matrix of molecular structure, a novel topological index is proposed. A set of topological parameters is built to reflect the magnitude,shape and other structure information of the substance. The interdependency between new topological index and conductivity for alkylimidazolium cations was analyzed and a quantitative relationship to describe this interdependency was obtained using the linear analyzing method. The analysis results show that the proposed topological index is quite satisfied with higher precision of the prediction. From the molecular structure of ionic liquid, the value of conductivity can be predicted correctly. This method can be also used to predict other physical properties of the ionic liquid.

  16. 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, wat...

  17. Ionic liquid-based variable focus electrowetting optics with bandwidths spanning the visible to mid-infrared

    CERN Document Server

    Watson, Alexander M; Niederriter, Robert D; Terrab, Soraya; Gopinath, Juliet T; Bright, Victor M

    2016-01-01

    Infrared optical materials and devices are important for a wide range of applications in the defense, scientific, and consumer markets. For imaging, spectroscopy, microscopy and persistent surveillance, adaptive optic systems that span the visible to infrared region are particularly useful. We address this need with novel electrowetting lens and prism elements that operate from 400 to 5000 nm. In contrast to conventional electrowetting devices that use polar liquids, limited by high absorption in the infrared region, we present room-temperature ionic liquid-based (RTIL, N-Propyl-Nmethylpyrrolidinium Bis(fluorosulfonyl)imide, Pyr1333a, Solvionic) lens and prism elements with unprecedented spectral bandwidths. Our electrowetting lenses tune over 20 diopters and have been demonstrated at 588, 1550 and 3000 nm wavelengths. Additionally, we have demonstrated prism elements with a steering angle of 0.56{\\deg} at 1550 nm.

  18. An ionic liquid based synthesis method for uniform luminescent lanthanide fluoride nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Nunez, Nuria O; Ocana, Manuel [Instituto de Ciencia de Materiales de Sevilla, CSIC, Americo Vespucio 49, 41092, Isla de la Cartuja, Sevilla (Spain)

    2007-11-14

    We describe a facile procedure for the synthesis of uniform lanthanide fluoride nanophosphors by homogeneous precipitation in ethylene glycol solutions containing lanthanide precursors and an ionic liquid (1-butyl, 2-methylimidazolium tetrafluoroborate). It is shown that the use of this ionic liquid as a fluoride source, an appropriate choice of the solvent and the lanthanide precursor, and the adjustment of reaction temperature, are essential to obtain uniform nanoparticles. This method is applied to the preparation of pure YF{sub 3}, EuF{sub 3} and TbF{sub 3} nanoparticles as well as of Eu-doped YF{sub 3} and Tb-doped YF{sub 3}. In most cases, highly uniform nanoparticles were obtained, the size of which could be tuned in the nanometer range by adjusting the nature and concentration of the starting lanthanide precursor. The luminescent properties of the synthesized materials are also evaluated.

  19. Ionic liquid-based membranes as electrolytes for advanced lithium polymer batteries.

    Science.gov (United States)

    Navarra, M A; Manzi, J; Lombardo, L; Panero, S; Scrosati, Bruno

    2011-01-17

    Gel-type polymer electrolytes are formed by immobilizing a solution of lithium N,N-bis(trifluoromethanesulfonyl)imide (LiTFSI) in N-n-butyl-N-ethylpyrrolidinium N,N-bis(trifluoromethanesulfonyl)imide (Py₂₄TFSI) ionic liquid (IL) with added mixtures of organic solvents, such as ethylene, propylene and dimethyl carbonates (EC, PC, and DMC, respectively), into a poly(vinylidenefluoride-co-hexafluoropropylene) (PVdF-HFP) matrix, and their properties investigated. The addition of the organic solvent mixtures results in an improvement of the ionic conductivity and in the stabilization of the interface with the lithium electrode. Conductivity values in the range of 10⁻³-10⁻²  S cm⁻¹ are obtained in a wide temperature range. These unique properties allow the effective use of these membranes as electrolytes for the development of advanced polymer batteries based on a lithium metal anode and an olivine-type lithium iron phosphate cathode.

  20. New ionic liquid-based preparative method for diosgenin from Rhizoma dioscoreae nipponicae

    Directory of Open Access Journals (Sweden)

    Wang Yan

    2013-01-01

    Full Text Available Background: Rhizoma dioscoreae nipponicae is a perennial herb and its roots have been widely used in Traditional Chinese Medicine (TCM. Objective: To develop and optimize the extraction and hydrolysis technology of diosgenin from Rhizoma dioscoreae nipponicae. Materials and Methods: 1-methyl-3-(3-sulfopropyl-imidazolium hydrogen sulfate ([PSMIM]HSO 4 , as a kind of functional ionic liquid, replaced inorganic acid, and was used in a one-step ultrasonic extraction and hydrolysis for the preparation of diosgenin (the aglycone of dioscin and an important precursor chemical in the pharmaceutical industry from Rhizoma dioscoreae nipponicae , for the first time. The effects of various factors were evaluated. The obtained product was studied using high performance liquid chromatography (HPLC. Results: About 6.35 mg of diosgenin could be obtained from 2.0 g of raw material. Reusability and recycling of the ionic liquid were validated with fairly good results. The ionic liquid solution was reused four times, and the final extraction efficiency only decreased by 5%. Conclusion: In virtue of the obvious advantages of the green extraction and catalytic solvent, with further study, it is believed that this new one-step preparative method promises to replace the traditional methods.

  1. Towards safer sodium-ion batteries via organic solvent/ionic liquid based hybrid electrolytes

    Science.gov (United States)

    Monti, Damien; Ponrouch, Alexandre; Palacín, M. Rosa; Johansson, Patrik

    2016-08-01

    Hybrid electrolytes aimed at application in sodium-ion batteries (SIB) consisting of an organic solvent mixture (EC:PC) and different ionic liquids (ILs); EMImTFSI, BMImTFSI, and Pyr13TFSI, and with the NaTFSI salt providing the Na+ charge carriers have here been extensively studied. The physico-chemical and electrochemical characterisation includes ionic conductivity, viscosity, density, cation coordination and solvation, various safety measures, and electrochemical stability window (ESW). Hybrid electrolytes with 10-50% of IL content were found to have ionic conductivities on par with comparable organic solvent based electrolytes, but with highly enhanced safety properties. A systematic Raman spectroscopy study of the cation coordination and solvation before and after electrolyte safety tests by ignition suggest that IL cations and TFSI remain stable when ignited while organic solvents are consumed. Finally, the solid electrolyte interphase (SEI) formed when using hybrid electrolytes has both better mechanical and electrochemical stability than the SEI derived from pure IL based electrolytes. For a half-cell with a hard carbon (HC) electrode and a hybrid electrolyte with a composition of 0.8 m NaTFSI in EC0.45:PC0.45:Pyr13TFSI0.10 encouraging results were obtained for IL based electrolytes - ca. 182 mAhg-1 at C/10 over 40 cycles.

  2. Ionic liquid-based dispersive liquid-liquid microextraction for the determination of formaldehyde in wastewaters and detergents.

    Science.gov (United States)

    Arvand, Majid; Bozorgzadeh, Elahe; Shariati, Shahab; Zanjanchi, Mohammad Ali

    2012-12-01

    Spectrophotometry in combination with ionic liquid-based dispersive liquid-liquid microextraction (DLLME) was applied for the extraction and determination of formaldehyde in real samples. The method is based on the reaction of formaldehyde with methyl acetoacetate in the presence of ammonia. The variation in the absorbance of the reaction product was measured at 375 nm. An appropriate mixture of ethanol (disperser solvent) and ionic liquid, 1-hexyl-3-methylimidazoliumhexafluoro-phosphate [C(6)MIM][PF(6)] (extraction solvent) was rapidly injected into a water sample containing formaldehyde. After extraction, sedimented phase was analyzed by spectrophotometry. Under the optimum conditions, the calibration graph was linear in the range of 0.1-20 ng mL(-1) with the detection limit of 0.02 ng mL(-1) and limit of quantification of 0.08 ng mL(-1) for formaldehyde. The relative standard deviation (RSD%, n = 5) for the extraction and determination of 0.8 ng mL(-1) of formaldehyde in the aqueous samples was 2.5%. The results showed that DLLME is a very simple, rapid, sensitive, and efficient analytical method for the determination of trace amounts of formaldehyde in wastewaters and detergents, and suitable results were obtained.

  3. Ionic liquid-based microwave-assisted extraction of essential oil and biphenyl cyclooctene lignans from Schisandra chinensis Baill fruits.

    Science.gov (United States)

    Ma, Chun-hui; Liu, Ting-ting; Yang, Lei; Zu, Yuan-gang; Chen, Xiaoqiang; Zhang, Lin; Zhang, Ying; Zhao, Chunjian

    2011-12-02

    Ionic liquid-based microwave-assisted extraction (ILMAE) has been successfully applied in extracting essential oil and four kinds of biphenyl cyclooctene lignans from Schisandra chinensis Baill. 0.25 M 1-lauryl-3-methylimidazolium bromide ionic liquid is selected as solvent. The optimum parameters of dealing with 25.0 g sample are 385 W irradiation power, 40 min microwave extraction time and 1:12 solid-liquid ratio. The yields of essential oil and lignans are 12.12±0.37 ml/kg and 250.2±38.2 mg/kg under the optimum conditions. The composition of the essential oil extracted by hydro-distillation, steam-distillation and ILMAE is analyzed by GC-MS. With ILMAE method, the energy consumption time has not only been shortened to 40 min (hydro-distillation 3.0 h for extracting essential oil and reflux extraction 4.0 h for extracting lignans, respectively), but also the extraction efficiency has been improved (extraction of lignans and distillation of essential oil at the same time) and reduces the environmental pollution. S. chinensis materials treated by different methods are observed by scanning electronic microscopy. Micrographs provide more evidence to prove that ILMAE is a better and faster method. The experimental results also indicate that ILMAE is a simple and efficient technique for sample preparation.

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

    DEFF Research Database (Denmark)

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

    2015-01-01

    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...... 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...

  5. High performance red phosphorus electrode in ionic liquid-based electrolyte for Na-ion batteries

    Science.gov (United States)

    Dahbi, Mouad; Fukunishi, Mika; Horiba, Tatsuo; Yabuuchi, Naoaki; Yasuno, Satoshi; Komaba, Shinichi

    2017-09-01

    Electrochemical performance of the red phosphorus electrode was examined in ionic-liquid electrolyte, 0.25 mol dm-3 sodium bisfluorosulfonylamide (NaFSA) dissolved N-methyl-N-propylpyridinium-bisfluorosulfonylamide (MPPFSA), at room temperature. We compared its electrochemical performance to conventional EC/PC/DEC, EC/DEC, and PC solutions containing 1 mol dm-3 NaPF6. The electrode in NaFSA/MPPFSA demonstrated a reversible capacity of 1480 mAh g-1 and excellent capacity retention of 93% over 80 cycles, which is much better than those in the conventional electrolytes. The difference in capacity retention for the electrolytes correlates to the different solid electrolyte interphase (SEI) layer formed on the phosphorus electrode. To understand the SEI formation in NaFSA/MPPFSA and its evolution during cycling, we investigate the surface layer of the red phosphorus electrodes with hard X-ray photoelectron spectroscopy (HAXPES) and time-of-flight secondary ion mass spectrometry (TOF-SIMS). A detailed analysis of HAXPES spectra demonstrates that SEI layer consists of major inorganic and minor organic species, originating from decomposition of MPP+ and FSA-. Homogenous surface layer is formed during the first cycle in NaFSA/MPPFSA while in alkyl carbonate ester electrolytes, continuous growth of surface film up to the 20th cycle is observed. Possibility of red phosphorous electrode for battery applications with pure ionic liquid is discussed.

  6. A new sonication-assisted ionic liquid-based route to microcrystals of lanthanide fluorides and their photoluminescent properties

    Energy Technology Data Exchange (ETDEWEB)

    Li, Yinyan; Xu, Shiqing, E-mail: sxucjlu@hotmail.com

    2014-07-15

    Highlights: • Microcrystals of lanthanide fluorides were prepared by sonication-assisted IL-based route. • It is a fast, simple, green and mild method to get lanthanide fluoride microcrystals. • The microcrystals are uniform, monodisperse, well-shaped and phase-pure. • IL served as reaction medium, fluoride source as well as template. • Sonication helped to accelerate reaction and get monodisperse uniform microcrystals. - Abstract: We introduce an ionic liquid-based method for the synthesis of uniform lanthanide fluoride microcrystals with the assistance of a sonication-accelerated reaction system. It is a fast, simple and mild process to get uniform monodisperse spherical lanthanide fluoride microcrystals in large scale. Homogeneous precipitation in a biphasic system of ethanol solution of lanthanide nitrates and ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate [C{sub 4}mim][PF{sub 6}] led to the uniform LnF{sub 3} microcrystals. The method was applied to the preparation of pure LnF{sub 3} (Ln = La, Ce, Pr, Nd) and Eu{sup 3+}-doped LaF{sub 3}, Tb{sup 3+}-doped CeF{sub 3}. SEM images indicated highly uniform cotton-like spherical microcrystals were obtained. HRTEM image indicated that the microcrystals were aggregated by nanocrystals of 6–10 nm due to agglomeration effect of the ionic liquid. The uniformity and dispersility of LaF{sub 3} decreased with the increasing of the molar ratio of [C{sub 4}mim][PF{sub 6}] to La(NO{sub 3}){sub 3}·6H{sub 2}O. Diameter of the microcrystal decreased from La to Nd. Photoluminescence properties of Eu{sup 3+}-doped LaF{sub 3} and Tb{sup 3+}-doped CeF{sub 3} were also studied.

  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. 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).

  9. 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.

  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. Integrated ionic liquid-based electrofluidic circuits for pressure sensing within polydimethylsiloxane microfluidic systems.

    Science.gov (United States)

    Wu, Chueh-Yu; Liao, Wei-Hao; Tung, Yi-Chung

    2011-05-21

    This paper reports a novel pressure sensor with an electrical readout based on electrofluidic circuits constructed by ionic liquid (IL)-filled microfluidic channels. The developed pressure sensor can be seamlessly fabricated into polydimethylsiloxane (PDMS) microfluidic systems using the well-developed multilayer soft lithography (MSL) technique without additional assembly or sophisticated cleanroom microfabrication processes. Therefore, the device can be easily scaled up and is fully disposable. The pressure sensing is achieved by measuring the pressure-induced electrical resistance variation of the constructed electrofluidic resistor. In addition, an electrofluidic Wheatstone bridge circuit is designed for accurate and stable resistance measurements. The pressure sensor is characterized using pressurized nitrogen gas and various liquids which flow into the microfluidic channels. The experimental results demonstrate the great long-term stability (more than a week), temperature stability (up to 100 °C), and linear characteristics of the developed pressure sensing scheme. Consequently, the integrated microfluidic pressure sensor developed in this paper is promising for better monitoring and for characterizing the flow conditions and liquid properties inside the PDMS microfluidic systems in an easier manner for various lab on a chip applications.

  12. Ionic-Liquid-Based CO2 Capture Systems: Structure, Interaction and Process.

    Science.gov (United States)

    Zeng, Shaojuan; Zhang, Xiangping; Bai, Lu; Zhang, Xiaochun; Wang, Hui; Wang, Jianji; Bao, Di; Li, Mengdie; Liu, Xinyan; Zhang, Suojiang

    2017-07-26

    The inherent structure tunability, good affinity with CO2, and nonvolatility of ionic liquids (ILs) drive their exploration and exploitation in CO2 separation field, and has attracted remarkable interest from both industries and academia. The aim of this Review is to give a detailed overview on the recent advances on IL-based materials, including pure ILs, IL-based solvents, and IL-based membranes for CO2 capture and separation from the viewpoint of molecule to engineering. The effects of anions, cations and functional groups on CO2 solubility and selectivity of ILs, as well as the studies on degradability of ILs are reviewed, and the recent developments on functionalized ILs, IL-based solvents, and IL-based membranes are also discussed. CO2 separation mechanism with IL-based solvents and IL-based membranes are explained by combining molecular simulation and experimental characterization. Taking into consideration of the applications and industrialization, the recent achievements and developments on the transport properties of IL fluids and the process design of IL-based processes are highlighted. Finally, the future research challenges and perspectives of the commercialization of CO2 capture and separation with IL-based materials are posed.

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

    Directory of Open Access Journals (Sweden)

    Wei Xu

    2012-12-01

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

  14. Ionic Liquid-Based Non-Aqueous Electrolytes for Nickel/Metal Hydride Batteries

    Directory of Open Access Journals (Sweden)

    Tiejun Meng

    2017-02-01

    Full Text Available The voltage of an alkaline electrolyte-based battery is often limited by the narrow electrochemical stability window of water (1.23 V. As an alternative to water, ionic liquid (IL-based electrolyte has been shown to exhibit excellent proton conducting properties and a wide electrochemical stability window, and can be used in proton conducting batteries. In this study, we used IL/acid mixtures to replace the 30 wt % KOH aqueous electrolyte in nickel/metal hydride (Ni/MH batteries, and verified the proton conducting character of these mixtures through electrochemical charge/discharge experiments. Dilution of ILs with acetic acid was found to effectively increase proton conductivity. By using 2 M acetic acid in 1-ethyl-3-methylimidazolium acetate, stable charge/discharge characteristics were obtained, including low charge/discharge overpotentials, a discharge voltage plateau at ~1.2 V, a specific capacity of 161.9 mAh·g−1, and a stable cycling performance for an AB5 metal hydride anode with a (Ni,Co,Zn(OH2 cathode.

  15. 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%.

  16. Ionic liquid-based aqueous biphasic systems as a versatile tool for the recovery of antioxidant compounds.

    Science.gov (United States)

    Santos, João H; e Silva, Francisca A; Ventura, Sónia P M; Coutinho, João A P; de Souza, Ranyere L; Soares, Cleide M F; Lima, Álvaro S

    2015-01-01

    The comparative evaluation of distinct types of ionic liquid-based aqueous biphasic systems (IL-ABS) and more conventional polymer/salt-based ABS to the extraction of two antioxidants, eugenol and propyl gallate, is focused. In a first approach, IL-ABS composed of ILs and potassium citrate (C6H5K3O7/C6H8O7) buffer at pH 7 were applied to the extraction of two antioxidants, enabling the assessment of the impact of IL cation core on the extraction. The second approach uses ABS composed of polyethylene glycol (PEG) and potassium phosphate (K2HPO4/KH2PO4) buffer at pH 7 with imidazolium-based ILs as adjuvants. Their application to the extraction of the compounds allowed the investigation of the impact of the presence/absence of IL, the PEG molecular weight, and the alkyl side chain length of the imidazolium cation on the partition. It is possible to maximize the extractive performance of both antioxidants up to 100% using both types of IL-ABS. The IL enhances the performance of ABS technology. The data puts in evidence the pivotal role of the appropriate selection of the ABS components and design to develop a successful extractive process, from both environmental and performance points of view.

  17. 3-V Solid-State Flexible Supercapacitors with Ionic-Liquid-Based Polymer Gel Electrolyte for AC Line Filtering.

    Science.gov (United States)

    Kang, Yu Jin; Yoo, Yongju; Kim, Woong

    2016-06-08

    State-of-the-art solid-state flexible supercapacitors with sufficiently fast response speed for AC line filtering application suffer from limited energy density. One of the main causes of the low energy density is the low cell voltage (1 V), which is limited by aqueous-solution-based gel electrolytes. In this work, we demonstrate for the first time a 3-V flexible supercapacitor for AC line filtering based on an ionic-liquid-based polymer gel electrolyte and carbon nanotube electrode material. The flexible supercapacitor exhibits an areal energy density that is more than 20 times higher than that of the previously demonstrated 1-V flexible supercapacitor (0.66 vs 0.03 μWh/cm(2)) while maintaining excellent capacitive behavior at 120 Hz. The supercapacitor shows a maximum areal power density of 1.5 W/cm(2) and a time constant of 1 ms. The improvement of the cell voltage while maintaining the fast-response capability greatly improves the potential of supercapacitors for high-frequency applications in wearable and/or portable electronics.

  18. Ultrasound assisted phytosynthesis of iron oxide nanoparticle.

    Science.gov (United States)

    Sathya, K; Saravanathamizhan, R; Baskar, G

    2017-11-01

    The present work deals with the ultrasound assisted green synthesis of iron oxide nano particle using Coriandrum sativum leaf extract as a reducing agent. The synthesized iron oxide nanoparticle was confirmed by UV spectra. The characterization was done to know more about morphology and size of the particle by SEM analysis which shows spherical particles with size ranging from 20 to 90nm. The antimicrobial activity of the leaf extract and the synthesized nanoparticles was studied against the pathogens Micrococcus luteus, Staphylococcus aureus and Aspergillus niger. The ultrasound assisted iron oxide nanoparticle shows higher scavenging activity and antimicrobial activity compared with iron oxide nanoparticle synthesized by magnetic stirrer and Coriandrum sativum leaf extract. Copyright © 2017. Published by Elsevier B.V.

  19. Ultrasound assisted engineering of lactose crystals.

    Science.gov (United States)

    Dhumal, Ravindra S; Biradar, Shailesh V; Paradkar, Anant R; York, Peter

    2008-12-01

    To engineer lactose crystals of desired size, shape, surface and particle size distribution (PSD) as a carrier for dry powder inhalers (DPI) by ultrasound assisted in-situ seeding. Lactose crystals were obtained from solution by ultrasound assisted in-situ seeding, followed by growth in viscous glycerin solution. The crystals were characterized for physical properties and 63-90 mum size fractions of different batches were mixed with salbutamol sulphate (SS) and compared for in-vitro deposition. Cooling crystallization with stirring for 10-20 h resulted in crystals with wide PSD and varied shape. Application of ultrasound resulted in rapid and complete crystallization in 5 min with rod-shaped fine crystals (15-30 microm) and narrow PSD. In-situ seeded batches yielded micro-fine rod-shaped seed crystals. Seeding followed by growth in glycerin showed desirable size, high elongation ratio, smooth surface and narrow PSD, while growth under stirring showed high elongation ratio with rough surface. Crystals grown in glycerin showed highest dispersibility and fine particle fraction (FPF) of SS. Ultrasound assisted in-situ seeding, followed by ordered growth in glycerin offers rapid technique for separation of nuclei induction from crystal growth yielding desirable characteristics for better dispersion and in-vitro deposition when employed as DPI carrier.

  20. Discharge products of ionic liquid-based Li-O2 batteries observed by energy dependent soft x-ray transmission microscopy

    Science.gov (United States)

    Olivares-Marín, Mara; Sorrentino, Andrea; Pereiro, Eva; Tonti, Dino

    2017-08-01

    Products deposited on an O2-cathode discharged in ionic liquid electrolytes are analyzed by transmission soft X-ray microscopy (TXM) and compared to ether-based electrolytes, showing differences in morphology and chemical compositions. With both solvents we observe Li2O2 and LiO2 primary products in similar proportions. However, while as previously observed in tetraglyme an important reactivity takes place producing significant amount of carbonates, in ionic liquid-based electrolytes the formation of carbonates was almost negligible, confirming higher stability. Only when sample is intentionally air exposed before analysis, significant amounts of carbonates came up. However, LiOH crystallites are clearly recognized with the ionic liquid electrolyte. The abundance of these crystallites depends on both the LiTFSI concentration and the storage time of discharged electrodes, suggesting that they result from the reaction of water trace with primary discharge products.

  1. Preparation of Ionic Liquid-based Vilsmier Reagent from Novel Multi-purpose Dimethyl Formamide-like Ionic Liquid and Its Application

    Institute of Scientific and Technical Information of China (English)

    Hullio, Ahmed Ali; Mastoi, G. M.

    2012-01-01

    In continuation of research to explore the applied potential of DMF-like ionic liquid, the ionic liquid version of N,N-dimethyliminiumchloride (Vilsmier reagent) has been synthesized from DMF-like ionic liquid and tested effectively for its capacity to achieve more useful organic transformations. The results show that DMF-like ionic liquid is world's first task specific ionic liquid which has catalyzed numerous diverse type of reaction and is multipurpose in its application. Thus a new term for this DMF-like ionic liquid has been coined that is DMF-like "multipurpose" ionic liquid.

  2. Ionic liquid-based extraction followed by graphite-furnace atomic absorption spectrometry for the determination of trace heavy metals in high-purity iron metal.

    Science.gov (United States)

    Matsumiya, Hiroaki; Kato, Tatsuya; Hiraide, Masataka

    2014-02-01

    The analysis of high-purity materials for trace impurities is an important and challenging task. The present paper describes a facile and sensitive method for the determination of trace heavy metals in high-purity iron metal. Trace heavy metals in an iron sample solution were rapidly and selectively preconcentrated by the extraction into a tiny volume of an ionic liquid [1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide] for the determination by graphite-furnace atomic absorption spectrometry (GFAAS). A nitrogen-donating neutral ligand, 2,4,6-tris(2-pyridyl)-1,3,5-triazine (TPTZ), was found to be effective in the ionic liquid-based selective extraction, allowing the nearly complete (~99.8%) elimination of the iron matrix. The combination with the optimized GFAAS was successful. The detectability reached sub-μg g(-1) levels in iron metal. The novel use of TPTZ in ionic liquid-based extraction followed by GFAAS was successfully applied to the determination of traces of Co, Ni, Cu, Cd, and Pb in certified reference materials for high-purity iron metal. © 2013 Published by Elsevier B.V.

  3. 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.

  4. Ionic liquid-based ultrasonic/microwave-assisted extraction combined with UPLC-MS-MS for the determination of tannins in Galla chinensis.

    Science.gov (United States)

    Lu, Chunxia; Wang, Hongxin; Lv, Wenping; Ma, Chaoyang; Lou, Zaixiang; Xie, Jun; Liu, Bo

    2012-01-01

    Ionic liquid was used as extraction solvents and applied to the extraction of tannins from Galla chinensis in the simultaneous ultrasonic- and microwave-assisted extraction (UMAE) technique. Several parameters of UMAE were optimised, and the results were compared with of the conventional extraction techniques. Under optimal conditions, the content of tannins was 630.2 ± 12.1 mg g⁻¹. Compared with the conventional heat-reflux extraction, maceration extraction, regular ultrasound- and microwave-assisted extraction, the proposed approach exhibited higher efficiency (11.7-22.0% enhanced) and shorter extraction time (from 6 h to 1 min). The tannins were then identified by ultraperformance liquid chromatography tandem mass spectrometry. This study suggests that ionic liquid-based UMAE is an efficient, rapid, simple and green sample preparation technique.

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

    Science.gov (United States)

    Tan, Zhi-Jian; Wang, Chao-Yun; Yang, Zi-Zhen; Yi, Yong-Jian; Wang, Hong-Ying; Zhou, Wan-Lai; Li, Fen-Fang

    2015-09-30

    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.

  6. Interfacial interactions in aprotic ionic liquid based protonic membrane and its correlation with high temperature conductivity and thermal properties.

    Science.gov (United States)

    Mistry, Mayur K; Subianto, Surya; Choudhury, Namita Roy; Dutta, Naba K

    2009-08-18

    Novel supported liquid membranes (SLMs) have been developed by impregnating Nafion and Hyflon membranes with ionic liquid 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide (BMI-BTSI). These supported liquid membranes were characterized in terms of their ionic liquid uptake behavior, leaching of ionic liquid by water, thermal stability, mechanical properties, glass transition temperature, ion exchange capacity, and proton conductivity. In general, modified membranes are more flexible than unmodified samples due to the plasticization effects of the ionic liquid. However, these supported liquid membranes exhibit a significant increase in their operational stability and proton conductivity over unmodified membranes. We also demonstrate that proton conductivity of these supported liquid membranes allows conduction of protons in anhydrous conditions with conductivity increasing with temperature. Conductivity of up to 3.58 mS cm(-1) has been achieved at 160 degrees C in dry conditions, making these materials promising for various electrochemical applications.

  7. Electrochemistry of poly(3,4-ethylenedioxythiophene)-polyaniline/ Prussian blue electrochromic devices containing an ionic liquid based gel electrolyte film.

    Science.gov (United States)

    Deepa, Melepurath; Awadhia, Arvind; Bhandari, Shweta

    2009-07-21

    Electrochromic devices based on poly(3,4-ethylenedioxythiophene) (PEDOT) as the cathodic coloring electrode and polyaniline (PANI) or Prussian blue (PB) as the counter electrode containing a highly conductive, self-supporting, distensible and transparent polymer-gel electrolyte film encapsulating an ionic liquid, 1-butyl-1-methylpyrrolidiniumbis-(trifluoromethylsulfonyl)imide, have been fabricated. Polarization, charge transfer and diffusion processes control the electrochemistry of the functional electrodes during coloration and bleaching and these phenomena differ when PEDOT and PANI/PB were employed alternately as working electrodes. While the electrochemical impedance response shows good similitude for PEDOT and PANI electrodes, the responses of PEDOT and PB were significantly different in the PEDOT-PB device, especially during reduction of PB, wherein the overall amplitude of the impedance response is enormous. Large values of the coloration efficiency maxima of 281 cm2 C(-1) (lambda = 583 nm) and 274 cm2 C(-1) (lambda = 602 nm), achieved at -1.0 and -1.5 V for the PEDOT PANI and PEDOT-PB devices have been correlated to the particularly low magnitude of charge transfer resistance and high polarization capacitance operative at the PEDOT ionic liquid based electrolyte interface at these dc potentials, thus allowing facile ion-transport and consequently resulting in enhanced absorption modulation. Moderately fast switching kinetics and the ability of these devices to sustain about 2500 cycles of clear-to-dark and dark-to-clear without incurring major losses in the optical contrast, along with the ease of construction of these cells in terms of high scalability and reproducibility of the synthetic procedure for fabrication of the electrochromic films and the ionic liquid based gel electrolyte film, are indicators of the promise these devices hold for practical applications like electrochromic windows and displays.

  8. Application of ionic liquids based microwave-assisted simultaneous extraction of carnosic acid, rosmarinic acid and essential oil from Rosmarinus officinalis.

    Science.gov (United States)

    Liu, Tingting; Sui, Xiaoyu; Zhang, Rongrui; Yang, Lei; Zu, Yuangang; Zhang, Lin; Zhang, Ying; Zhang, Zhonghua

    2011-11-25

    An ionic liquid based microwave-assisted simultaneous extraction and distillation (ILMSED) method has been developed for the effective extraction of carnosic acid (CA), rosmarinic acid (RA) and essential oil (EO) from Rosmarinus officinalis. A series of 1-alkyl-3-methylimidazolium ionic liquids differing in composition of anion and cation were evaluated for extraction yield in this work. The results obtained indicated that the anions and cations of ionic liquids had influences on the extraction of CA and RA, 1.0M 1-octyl-3-methylimidazolium bromide ([C8mim]Br) solution was selected as solvent. In addition, the ILMSED procedures for the three target ingredients were optimized and compared with other conventional extraction techniques. ILMSED gave the best result due to the highest extraction yield within the shortest extraction time for CA and RA. The novel process developed offered advantages in term of yield and selectivity of EO and shorter isolation time (20 min in comparison of 4h of hydrodistillation), and provides a more valuable EO (with high amount of oxygenated compounds). The microstructures and chemical structures of rosemary samples before and after extraction were also investigated. Moreover, the proposed method was validated by the stability, repeatability and recovery experiments. The results indicated that the developed ILMSED method provided a good alternative for the both extraction of non-volatile compounds (CA and RA) and EO from rosemary as well as other herbs.

  9. New types of Brönsted acid-base ionic liquids-based membranes for applications in PEMFCs.

    Science.gov (United States)

    Fernicola, Alessandra; Panero, Stefania; Scrosati, Bruno; Tamada, Masahiro; Ohno, Hiroyuki

    2007-05-14

    A series of ionic liquids (ILs) are prepared by neutralizing tertiary amines with N,N-bis(trifluoromethanesulfonyl)imide (HTFSI). As demonstrated by thermal and electrochemical characterizations, these ILs have very good temperature stability and a high ionic conductivity, that is, of the order of 10(-2) S cm-1. By incorporating these ILs into a poly(vinylidenfluoride-co-hexafluoropropylene) polymer matrix, membranes with a high melting temperature, high decomposition point and with an ionic conductivity of about 10(-2) S cm-1 at 140 degrees C, are obtained. These IL-based, proton-conducting membranes are proposed as new polymer electrolytes for high-temperature polymer electrolyte membrane fuel cells (PEMFCs).

  10. Towards Li(Ni0.33Mn0.33Co0.33)O2/graphite batteries with ionic liquid-based electrolytes. I. Electrodes' behavior in lithium half-cells

    Science.gov (United States)

    Simonetti, E.; Maresca, G.; Appetecchi, G. B.; Kim, G.-T.; Loeffler, N.; Passerini, S.

    2016-11-01

    Lithium cells based on NMC cathodes or graphite anodes and ionic liquid-based electrolyte mixtures are investigated. The electrode tapes, using water-soluble natural binders, as well as the ionic liquid materials, are prepared through eco-friendly routes involving H2O as the only processing solvent. The Li/NMC and Li/graphite half-cells are studied by cyclic voltammetry, impedance spectroscopy and galvanostatic cycling tests at different temperatures. The results herein reported, demonstrate the performance improvement in terms of cycling behavior and ageing resistance, granted by the ionic liquid mixtures with respect to the electrolytes reported in literature based on a single ionic liquid.

  11. 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.

  12. Fluid phase behaviour of ionic liquid-based systems of interest for green processes: measurements and modelling

    NARCIS (Netherlands)

    Kühne, E.

    2008-01-01

    In the last decades a large number of applications with ionic liquids (IL) have emerged, and since the discovery that carbon dioxide can tune the miscibility of IL+organic mixtures, special attention has been drawn to the use of IL and CO2 as combined solvents for synthesis and extractions. To evalu

  13. 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.

  14. 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.

  15. Ionic liquid-based dispersive liquid-liquid microextraction and enhanced spectrophotometric determination of molybdenum (VI) in water and plant leaves samples by FO-LADS.

    Science.gov (United States)

    Gharehbaghi, Maysam; Shemirani, Farzaneh

    2011-02-01

    A new simple and rapid ionic liquid-based dispersive liquid-liquid microextraction (IL-DLLME) has been applied to preconcentrate trace levels of molybdenum (VI) as a prior step to its enhanced determination by fiber optic-linear array detection spectrophotometry (FO-LADS). In this method, a small amount of [Hmim][Tf(2)N] (1-hexyl-3-methylimmidazolium bis (trifluormethylsulfonyl) imid) as an extraction solvent was applied to extract molybdenum - pyrogallol red complex, which was formed in an aqueous solution in the presence of N-cetyl-N-N-N-trimethyl ammonium chloride as a sensitizing agent. Under optimum conditions, enhancement factor, detection limit and relative standard deviation (n=5, for 30 μg L(-1) of molybdenum (VI)) in 10 mL water sample were 72.6, 1.43 μg L(-1) and 2.8%, respectively.

  16. 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 ZrO2 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 ZrO2 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.

  17. 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.

  18. Development of an ionic liquid-based microwave-assisted method for simultaneous extraction and distillation for determination of proanthocyanidins and essential oil in Cortex cinnamomi.

    Science.gov (United States)

    Liu, Ye; Yang, Lei; Zu, Yuangang; Zhao, Chunjian; Zhang, Lin; Zhang, Ying; Zhang, Zhonghua; Wang, Wenjie

    2012-12-15

    Cortex cinnamomi is associated with many health benefits and is used in the food and pharmaceutical industries. In this study, an efficient ionic liquid-based microwave-assisted simultaneous extraction and distillation (ILMSED) technique was used to extract cassia oil and proanthocyanidins from Cortex cinnamomi; these were quantified by gas chromatography/mass spectrometry (GC-MS) and the vanillin-HCl colorimetric method, respectively. 0.5M 1-butyl-3-methylimidazolium bromide ionic liquid was selected as solvent. The optimum parameters of dealing with 20.0 g sample were 230 W microwave irradiation power, 15 min microwave extraction time and 10 liquid-solid ratio. The yields of essential oil and proanthocyanidins were 1.24 ± 0.04% and 4.58 ± 0.21% under the optimum conditions. The composition of the essential oil was analysed by GC-MS. Using the ILMSED method, the energy consumption was reduced and the extraction yields were improved. The proposed method was validated using stability, repeatability, and recovery experiments. The results indicated that the developed ILMSED method provided a good alternative for the extraction of both the essential oil and proanthocyanidins from Cortex cinnamomi.

  19. Determination of Anilines in Water Samplse by Ultrasound-Assisted Ionic Liquid Dispersive Liquid-liquid micro-extraction combined with high performance liquid chromatography%超声辅助离子液体-分散液液微萃取-高效液相色谱法测定水中苯胺类化合物

    Institute of Scientific and Technical Information of China (English)

    马莹; 张奇; 李媛; 张海霞

    2016-01-01

    本研究建立了超声辅助离子液体-分散液液微萃取-高效液相色谱测定环境水样中苯胺( AN)、对氟苯胺(4-FA)、对硝基苯胺(4-NA)、对氯苯胺(4-CA)四种苯胺化合物的方法。以最常用的烷基咪唑六氟磷酸盐类离子液体为萃取剂,通过超声加速萃取剂的分散程度,提高了萃取效率。该方法的检测限达到0.1~73 ng/ml,对黄河水和自来水中的加标回收率均在90.5%~113%之间,回收效果良好。与传统的液液萃取相比,该萃取方法具有绿色、快速、富集效果好、有机溶剂消耗小的优点,可以满足环境水体中苯胺类化合物的测定。%Ultrasound-assisted ionic liquid dispersive liquid -liquid microextraction combined with high performance liquid chromatography ( HPLC) method for preconcentration and determination of trace amounts of anilines in water samples was es -tablished .1-butyl-3-methylmidazolium hexafluoro -phosphate ( [ C4 MIM] [PF 6 ] ) is selected because it can simultane-ously extract aniline compounds from water .The limits of detection is in the range of 0.1~73 ng/ml.The developed method showed high relative recoveries for Aniline (AN),4-Fluoroaniline (4-FA),4-Nitroaniline (4-NA),4-Chloroaniline (4-CA) at different concentrations from 90.5%to 113%,which ensured the accuracy of method using to detect the amount of anilines in environmental water samples .

  20. Coarse-grained simulations of an ionic liquid-based capacitor: I. Density, ion size, and valency effects.

    Science.gov (United States)

    Breitsprecher, Konrad; Košovan, Peter; Holm, Christian

    2014-07-16

    We introduce a hierarchy of generic coarse-grained models of ionic liquids of increasing complexity. We use them in molecular dynamics simulations to study the differential capacitance of a capacitor consisting of an ionic liquid between two planar electrodes. The primary goal is to explain the complex dependence of the differential capacitance Cd on the electrode potential U in simple terms, e.g. in terms of the size and valency of the ions. For this purpose we introduce the symmetric model A, which qualitatively reproduces the Cd(U) dependence predicted by the mean-field theory but also reveals strong quantitative deviations. We further introduce size asymmetry in model A by increasing the cation size. In model B we vary the cation valency, keeping the sizes of both ions constant. We show that simultaneous increases in size and valency may compensate for each other, leading to a Cd(U) very similar to that for the symmetric case. We interpret distinct features in Cd(U) on the basis of the density profiles of the ions and charge density profiles. We focus on the first two ion layers at the electrode, and demonstrate that the polarization of the ionic liquid proceeds through replacement of one ion type by the other, in contrast to the simple increase in ion concentrations typical for dilute systems. The understanding gained for the simple models serves as a reference for interpretation of complex effects of ion size, valency and shape. This is carried through in part II (a separate article) where we show how the planar shape of ions in model C brings new features to the Cd(U) curve and also to the polarization mechanism.

  1. A Novel Category of Ionic Liquids Based on Diacetone Acrylamide Cation and Their Use as Esterification Catalysts

    Institute of Scientific and Technical Information of China (English)

    CAI Qing-Hai; LU Bin; LI Jiang; YANG Xin; SHAN Yong-Kui

    2006-01-01

    A novel category of salts based on diacetone acrylamide cation (DA+) and the anions such as acetate (Ac-),trifluoroacetate (TF-), tetrafluoroborate (BF-), hexafluorophosphate (PF-), sulfate (SO-) and chloride (Cl-) were synthesized by usual neutralization of acids and bases at room temperature and characterized by IR, 1H NMR and elemental analysis (EA). The results show that these compounds possess the characteristic of ionic liquids. In addition, four of them, DABF, DACl, DASO and DAPF, were efficient catalysts for esterication of acetic acid with C1C6 alcohols and octanol.

  2. 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

  3. Ionic Liquid-Based Polymer Electrolytes via Surfactant-Assisted Polymerization at the Plasma-Liquid Interface.

    Science.gov (United States)

    Tran, Quoc Chinh; Bui, Van-Tien; Dao, Van-Duong; Lee, Joong-Kee; Choi, Ho-Suk

    2016-06-29

    We first report an innovative method, which we refer to as interfacial liquid plasma polymerization, to chemically cross-link ionic liquids (ILs). By this method, a series of all-solid state, free-standing polymer electrolytes is successfully fabricated where ILs are used as building blocks and ethylene oxide-based surfactants are employed as an assisted-cross-linking agent. The thickness of the films is controlled by the plasma exposure time or the ratio of surfactant to ILs. The chemical structure and properties of the polymer electrolyte are characterized by scanning electron microscopy (SEM), Fourier transformation infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR) spectroscopy, X-ray photoelectron spectroscopy (XPS), differential scanning calorimetry (DSC), and electrochemical impedance spectroscopy (EIS). Importantly, the underlying polymerization mechanism of the cross-linked IL-based polymer electrolyte is studied to show that fluoroborate or halide anions of ILs together with the aid of a small amount of surfactants having ethylene oxide groups are necessary to form cross-linked network structures of the polymer electrolyte. The ionic conductivity of the obtained polymer electrolyte is 2.28 × 10(-3) S·cm(-1), which is a relatively high value for solid polymer electrolytes synthesized at room temperature. This study can serve as a cornerstone for developing all-solid state polymer electrolytes with promising properties for next-generation electrochemical devices.

  4. Isolation of natural red colorants from fermented broth using ionic liquid-based aqueous two-phase systems.

    Science.gov (United States)

    Ventura, Sónia P M; Santos-Ebinuma, Valéria C; Pereira, Jorge F B; Teixeira, Maria F S; Pessoa, Adalberto; Coutinho, João A P

    2013-05-01

    There is a growing demand for natural colorants. This is prompting the search for new alternative and "benign" separation systems allowing higher recoveries, extraction yields, and selectivities. This work investigates the use of aqueous two-phase systems (ATPS) based on ionic liquids as extraction processes for the recovery of red colorants from the fermented broth of Penicillium purpurogenum DPUA 1275. Several ATPS based on quaternary ammonium and imidazolium were studied in this work aiming at separating the red colorants produced from the remaining colorants and contaminant proteins present in the fermented broth. The results suggest that the red colorants can be isolated by an appropriate manipulation of some of the process conditions, such as the use of quaternary ammonium with short alkyl chains, alkaline media, and short tie-line lengths (extraction point systems with lower concentrations of ionic liquid). These conditions allow large partition coefficients for the red colorants (K red = 24.4 ± 2.3), high protein removal (60.7 ± 2.8 %) and selectivity parameters (S red/prot = 10.05).

  5. Highly selective ionic liquid-based microextraction method for sensitive trace cobalt determination in environmental and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Berton, Paula [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); Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gov.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)

    2010-03-10

    A simple and rapid dispersive liquid-liquid microextraction procedure based on an ionic liquid (IL-DLLME) was developed for selective determination of cobalt (Co) with electrothermal atomic absorption spectrometry (ETAAS) detection. Cobalt was initially complexed with 1-nitroso-2-naphtol (1N2N) reagent at pH 4.0. The IL-DLLME procedure was then performed by using a few microliters of the room temperature ionic liquid (RTIL) 1-hexyl-3-methylimidazolium hexafluorophosphate [C{sub 6}mim][PF{sub 6}] as extractant while methanol was the dispersant solvent. After microextraction procedure, the Co-enriched RTIL phase was solubilized in methanol and directly injected into the graphite furnace. The effect of several variables on Co-1N2N complex formation, extraction with the dispersed RTIL phase, and analyte detection with ETAAS, was carefully studied in this work. An enrichment factor of 120 was obtained with only 6 mL of sample solution and under optimal experimental conditions. The resultant limit of detection (LOD) was 3.8 ng L{sup -1}, while the relative standard deviation (RSD) was 3.4% (at 1 {mu}g L{sup -1} Co level and n = 10), calculated from the peak height of absorbance signals. The accuracy of the proposed methodology was tested by analysis of a certified reference material. The method was successfully applied for the determination of Co in environmental and biological samples.

  6. Study of ion diffusional motion in ionic liquid-based polymer electrolytes by simultaneous solid state NMR and DTA.

    Science.gov (United States)

    Rajput, Dushyant Singh; Yamada, Koji; Sekhon, S S

    2013-02-28

    Polymer electrolytes containing ionic liquid (IL), 2-methyl-1,3-dipropylimidazolium dihydrogenphosphate (MDPImH2PO4) have been studied by (1)H solid state NMR and differential thermal analysis (DTA) simultaneously by using a specially designed probe. To the best of our knowledge, this is the first report of its kind for IL based polymer electrolytes. The variation of NMR line width with temperature for the IL and polymer electrolytes shows line narrowing at the glass transition and melting temperature. The onset of long-range ion diffusional motion also takes place at these temperatures and is accompanied by a sudden increase in ionic conductivity value by 2-3 orders of magnitude. The presence of amorphous and crystalline phases in IL-based polymer electrolytes has been observed from X-ray diffraction (XRD) studies, and the amorphous phase is the high conducting phase in these polymer electrolytes. The IL-based polymer electrolytes have been observed to be thermally stable up to 200 °C. The results obtained from ion transport studies have also been supported by Fourier transform infrared (FTIR), XRD, and cyclic voltammetry (CV) studies.

  7. Fabrication of a polymeric ionic liquid-based adsorbent for multiple monolithic fiber solid-phase microextraction of endocrine disrupting chemicals in complicated samples.

    Science.gov (United States)

    Pei, Miao; Zhang, Zirui; Huang, Xiaojia; Wu, Yuanfei

    2017-04-01

    A multiple monolithic fiber solid-phase microextraction (MMF-SPME) utilizing polymeric ionic liquid-based adsorbent was prepared. The adsorbent was obtained by in situ copolymerization of an ionic liquid, 1-trimethyl-(4-vinylbenzyl) aminium chloride and dual cross-linkers (divinylbenzene and ethylenedimethacrylate). The effect of preparation conditions including the content of ionic liquid and porogen in the polymerization mixture on extraction performance was studied in detail. Infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry were used to inspect the physicochemical properties of the new adsorbent. The applicability of the new MMF-SPME was demonstrated by the extraction of trace endocrine disrupting chemicals (EDCs). Results indicated that the prepared MMF-SPME could extract EDCs effectively through multi-interactions such as ion-exchange, π-π and hydrophobic interactions. After optimization of extraction parameters, a method of MMF-SPME coupled to high performance liquid chromatography/diode array detection was conducted to detect trace EDCs in complicated samples including environmental water and human urine. The limits of detection (S/N=3) and quantification (S/N=10) for targeted compounds were 0.011-0.065μg/L and 0.036-0.21μg/L, respectively. Satisfactory precision was also achieved by evaluating the repeatability and intermediate precision with relative standard deviations (RSDs) of less than 9% and 10%, respectively. At the same time, the proposed method was successfully applied for the determination of EDCs in water and human urine with spiking recoveries ranged from 70.6% to 119%.

  8. Preparation of a new polymeric ionic liquid-based monolith for stir cake sorptive extraction and its application in the extraction of inorganic anions.

    Science.gov (United States)

    Huang, Xiaojia; Chen, Linli; Yuan, Dongxing; Bi, Shangshang

    2012-07-27

    In this study, a novel stir cake sorptive extraction (SCSE) sorbent based on polymeric ionic liquid-based monolith (PILM) for the extraction of inorganic anions was prepared. In the presence of a porogen solvent containing 1-propanol and dimethylformamid, an ionic liquid, 1-ally-3-methylimidazolium chloride was used as monomer to copolymerize in situ with ethylene dimethacrylate to form PILM. The effect of preparation conditions such as ratio of functional monomer to cross-linker, content of porogenic solvent on the extraction efficiencies were investigated in detail. The PILM was characterized by elemental analysis, scanning electron microscopy, mercury intrusion porosimetry and infrared spectroscopy. In order to investigate the extraction capacity of PILM-SCSE for inorganic anions, the SCSE was combined with ion chromatography with conductivity detection, F(-), Cl(-), NO(2)(-), Br(-), NO(3)(-), PO(4)(3-) and SO(4)(2-) were selected as detected solutes. Several extractive parameters, including pH values in sample matrix, desorption solvent, extraction and desorption time were optimized. The results showed that under the optimum experimental conditions, low detection limits (S/N=3) and quantification limits (S/N=10) of the proposed method for the target anions were achieved within the range of 0.11-2.08 and 0.37-6.88 μg/L, respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction inorganic anions. Finally, the proposed method was successfully used to detect different water samples include commercial purified water, tab water and river water. Acceptable recoveries and satisfactory repeatability were obtained. To the best of our knowledge, this is the first to use polymeric ionic liquid to enrich inorganic anions.

  9. Multiple functional ionic liquids based dispersive liquid-liquid microextraction combined with high performance chromatography for the determination of phenolic compounds in water samples.

    Science.gov (United States)

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

    2014-07-01

    A new mode of ionic liquid based dispersive liquid-liquid microextraction (IL-DLLME) is developed. In this work, [C6MIm][PF6] was chosen as the extraction solvent, and two kinds of hydrophilic ionic liquids, [EMIm][BF4] and [BSO3HMIm][OTf], functioned as the dispersive solvent. So in the whole extraction procedure, no organic solvent was used. With the aid of SO3H group, the acidic compound was extracted from the sample solution without pH adjustment. Two phenolic compounds, namely, 2-naphthol and 4-nitrophenol were chosen as the target analytes. Important parameters affecting the extraction efficiency, such as the type of hydrophilic ionic liquids, the volume ratio of [EMIm][BF4] to [BSO3HMIm][OTf], type and volume of extraction solvent, pH value of sample solution, sonication time, extraction time and centrifugation time were investigated and optimized. Under the optimized extraction conditions, the method exhibited good sensitivity with the limits of detection (LODs) at 5.5 μg L(-1)and 10.0 μg L(-1) for 4-nitrophenol and 2-naphthol, respectively. Good linearity over the concentration ranges of 24-384 μg L(-1) for 4-nitrophenol and 28-336 μg L(-1) for 2-naphthol was obtained with correlation coefficients of 0.9998 and 0.9961, respectively. The proposed method can directly extract acidic compound from environmental sample or even more complex sample matrix without any pH adjustment procedure.

  10. Extraction and Determination of Quercetin and Myricetin from Chamaecyparis obtusa by Ionic Liquids-based Monolithic Cartridge%Extraction and Determination of Quercetin and Myricetin from Chamaecyparis obtusa by Ionic Liquids-based Monolithic Cartridge

    Institute of Scientific and Technical Information of China (English)

    朱涛; 毕文韬; 卢敬昊

    2011-01-01

    A short ionic liquids (ILs)-based monolithic cartridge was prepared and used as the selective extraction sorbent. After the material was evaluated by field emission-scanning electron microscopy (FE-SEM), a new approach for the extraction and determination of quercetin and myricetin from Chamaecyparis obtusa (C. obtusa) by using ILs-based, monolithic cartridge system was developed. Chromatographic analysis was conducted on a C18 column with UV detection at 372 nm, an eluting solution consisting of acetonitrile-water (25/75, V/V) as the mobile phase, and a flow rate of 0.7 mLomin 1. A good linear relationship was demonstrated when the concentrations of quercetin and myricetin were in the range of 0.5--100.0 ggomL-1. The recoveries ranged from 101.6% to 104.6% and the inter- and intra-day relative standard deviations (RSD) were less than 5.0%. This method effectively removed the impurities and avoided tedious pretreatment. It provided a fast, economic and effective method for assaying trace drugs from natural plants.

  11. Determination of Four Pesticides in Soil by Homogeneous Ionic Liquid-based Microextraction Coupled with High-performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    YAN Rui; SHAO Ming-yuan; LIANG Zhen-fen; ZHANG Han-qi; YU Ai-min

    2013-01-01

    Homogeneous ionic liquid microextraction was developed for the simultaneceus extraction of dimethomorph,mefenacet,isoprothiolane and oxadiazon from soil.1-Butyl-3-methylimidazolium tetrafluoroborate was used as extraction solvent,and ammonium hexafluorophosphate was used as ion-pairing agent.High-performance liquid chromatography(HPLC) was employed for separation and determination of the analytes.The calibration curves show good linear relationship(r>0.9988).The recoveries are between 74.2% and 97.9% with relative standard deviations(RSDs) lower than 5.97%.The present method is free of volatile organic solvents,and expenditures of sample,extraction time and solvent are lower,compared with ultrasonic and Soxhlet extraction.There was no obvious difference in the extraction recoveries of pesticides obtained by the three extraction methods.

  12. The influence of pore size and surface area of activated carbons on the performance of ionic liquid based supercapacitors.

    Science.gov (United States)

    Pohlmann, Sebastian; Lobato, Belén; Centeno, Teresa A; Balducci, Andrea

    2013-10-28

    This study analyses and compares the behaviour of 5 commercial porous carbons in the ionic liquid N-butyl-N-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide (PYR14TFSI) and its mixture with propylene carbonate (PC) as electrolytes. The results of this investigation show that the existence of a distribution of pore sizes and/or constrictions at the entrance of the pores leads to significant changes in the specific capacitance of the investigated materials. The use of PYR14TFSI as an electrolyte has a positive effect on the EDLC energy storage, but its high viscosity limits the power density. The mixture 50 : 50 wt% propylene carbonate-PYR14TFSI provides high operative voltage as well as low viscosity and thus notably enhances EDLC operation.

  13. 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.

  14. Evaluation of Two Ionic Liquid-Based Epoxies from the MISSE-8 (Materials International Space Station Experiment-8) Sample Carrier

    Science.gov (United States)

    Rabenberg, Ellen; Kaukler, William; Grugel, Richard

    2015-01-01

    Two sets of epoxy mixtures, both containing the same ionic liquid (IL) based resin but utilizing two different curing agents, were evaluated after spending more than two years of continual space exposure outside of the International Space Station on the MISSE-8 sample rack. During this period the samples, positioned on nadir side, also experienced some 12,500 thermal cycles between approximately -40?C and +40 C. Initial examination showed some color change, a miniscule weight variance, and no cracks or de-bonding from the sample substrate. Microscopic examination of the surface reveled some slight deformities and pitting. These observations, and others, are discussed in view of the ground-based control samples. Finally, the impetus of this study in terms of space applications is presented.

  15. Alkyl imidazolium ionic liquid based sweeping-micellar electrokinetic chromatography for simultaneous determination of seven tea catechins in human plasma.

    Science.gov (United States)

    El-Hady, Deia Abd; Albishri, Hassan M

    2014-10-15

    Determination of tea catechins in human plasma might provide a means of better evaluation of their benefits. The main difficulty in their analysis is the low catechins concentrations in plasma and their susceptible to oxidation during sample pretreatment. In the current work, a sweeping-micellar electrokinetic chromatography (sweeping-MEKC) by long alkyl chain ionic liquid was investigated for the simultaneous determination of seven principal naturally-occurring tea catechins in human plasma under acidic conditions after the intake of green tea beverage. The effects of type and concentration of three 1-tetradecyl-3-methylimidazolium ionic liquids, namely bromide, acetate and hydrogen sulfate salts were studied. The seven catechins were successfully separated within 5min by micellar running buffer of 5mmolL(-1) 1-tetradecyl-3-methylimidazolium bromide and 15mmolL(-1) phosphate buffer at pH 4.5 under optimal parameters of 50mbar injection for 150s, 10kV, 25°C and 200nm. To prevent the possibility of IL adsorption, an appropriate rinsing protocol was established. The method has analytical ranges from 0.5, 1, 0.5, 1, 2, 1 and 1 to 500ngmL(-1) for GC, C, EC, EGCG, GCG, ECG and EGC, respectively (r ranged from 0.995 to 0.999). The intraday precision and accuracy were 0.1-0.9% RSD (n=10) and 97-106% recovery, respectively. Limits of detections of analytes were ranged from 0.2 to 1.2ngmL(-1). The current sweeping-MEKC achieved sensitivity enhancement factor (SEF) up to 183-fold of analytes concentrations compared to other hitherto published CE reports that is suitable to find out the trace amounts of catechins in plasma.

  16. Ionic-liquid-based dispersive liquid-liquid microextraction for high-throughput multiple food contaminant screening.

    Science.gov (United States)

    Ho, Yee-Man; Tsoi, Yeuk-Ki; Leung, Kelvin Sze-Yin

    2013-12-01

    This paper describes an innovation of dispersive liquid-liquid microextraction enabling multiple-component analysis of eight high-priority food contaminants in two chemically distinctive families: Sudan dyes and phthalate plasticizers. To provide convenient sample handling for solid and solid-containing matrices, a modified dispersive liquid-liquid microextraction procedure used an extractant precoated frit to perform simultaneous filtration, solvent mixing, and phase dispersion in one simple step. A binary ionic liquid extractant system was carefully tuned to deliver high quality analysis based only on affordable LC with diode array detector instrumentation. The method is comprehensively validated for robust quantification with good precision (6.9-9.8% RSD) in a linear 2-1000 μg/L range. Having accomplished enrichment factors up to 451, the treatment enables sensitive detection at 0.09-1.01 μg/L levels. Analysis of six high-risk solid condiments and sauces further verified its practical applicability within a 70-120% recovery range. Compared to other approaches, the current dispersive liquid-liquid microextraction treatment offers major advantages in terms of minimal solvent (1.5 mL) and sample (0.1 g) consumption, ultra-high analytical throughput (6 min), and the ability to handle complex solid matrices. The idea of performing simultaneous analysis for multiple contaminants presented here fosters a more effective mode of operation in food control routines.

  17. Extraction of tetra-oxo anions into a hydrophobic, ionic liquid-based solvent without concomitant ion exchange.

    Energy Technology Data Exchange (ETDEWEB)

    Stepinski, D. C.; Vandegrift, G. F.; Shkrob, I. A.; Wishart, J. F.; Kerr, K.; Dietz, M. L.; Qadah, D. T. D.; Garvey, S. L.; BNL; Univ. of Wisconsin at Milwaukee

    2010-06-16

    Hydrophobic ionic liquids (IL) have the potential to simplify certain separations by serving as both an extraction solvent and an electrolyte for subsequent electrochemical reductions. While IL-based solvents are known to be efficient media for metal ion extraction, separations employing these solvents are frequently complicated by the loss of constituent IL ions to the aqueous phase, resulting in deteriorating performance. In this study, we have examined the extraction of pertechnetate and related tetra-oxo anions from aqueous solutions into IL-based solvents incorporating tetraalkylphosphonium bis[(trifluoromethyl)sulfonyl]imide and a crown ether. In contrast to various previously studied IL-based cation extraction systems, facile anion extraction without significant transfer of the IL ions to the aqueous phase has been observed. In addition, the solvents exhibit high distribution ratios (100-500 for pertechnetate), significant electrical conductivity (>100 ?S/cm), and a wide (4 V) electrochemical window. The results suggest that these solvents may provide the basis for improved approaches to the extraction and recovery of a variety of anions.

  18. Extraction of Tetra-oxo Anions into a Hydrophobic, Ionic Liquid-Based Solvent Without Concomitant Ion Exchange

    Energy Technology Data Exchange (ETDEWEB)

    Stepinski, D.C.; Wishart, J.; Vandegrift, III, G.F.; Shkrob, I.A.; Kerr, K.; Dietz, M.L.; Qadah, D.T.D.; Garvey, S.L.

    2010-06-10

    Hydrophobic ionic liquids (IL) have the potential to simplify certain separations by serving as both an extraction solvent and an electrolyte for subsequent electrochemical reductions. While IL-based solvents are known to be efficient media for metal ion extraction, separations employing these solvents are frequently complicated by the loss of constituent IL ions to the aqueous phase, resulting in deteriorating performance. In this study, we have examined the extraction of pertechnetate and related tetra-oxo anions from aqueous solutions into IL-based solvents incorporating tetraalkylphosphonium bis[(trifluoromethyl)sulfonyl]imide and a crown ether. In contrast to various previously studied IL-based cation extraction systems, facile anion extraction without significant transfer of the IL ions to the aqueous phase has been observed. In addition, the solvents exhibit high distribution ratios (100-500 for pertechnetate), significant electrical conductivity (>100 {micro}S/cm), and a wide ({approx}4 V) electrochemical window. The results suggest that these solvents may provide the basis for improved approaches to the extraction and recovery of a variety of anions.

  19. 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.

  20. 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.

  1. A new polymeric ionic liquid-based magnetic adsorbent for the extraction of inorganic anions in water samples.

    Science.gov (United States)

    Chen, Lei; Huang, Xiaojia; Zhang, Yong; Yuan, Dongxing

    2015-07-17

    In this work, a novel type of polymeric ionic liquid (PIL)-based magnetic adsorbent was successfully synthesized and applied for the extraction and determination of seven inorganic anions in water samples by coupling with ion chromatography. The new adsorbent was synthesized by simple free radical copolymerization of 1-ally-3-vinylimidazolium chloride, ethylene glycol dimethacrylate and silica-coated magnetite. The adsorbent exhibited well-defined core-shell structure and good magnetic response ability. Furthermore, due to the presence of abundant anion-exchange groups in the PIL, the adsorbent displayed expected extraction performance for anions including F(-), Cl(-), Br(-), NO2(-), NO3(-), PO4(3-) and SO4(2-). Various experimental parameters that could affect the extraction performance, such as the amount of adsorbent, desorption solvent, extraction and desorption time, the pH value of sample solution were investigated in detail. Under the optimized conditions, low limits of detection (S/N=3) and quantification limits (S/N=10) of the proposed method for the target anions were achieved within the range of 0.061-0.73μg/L and 0.19-2.41μg/L, respectively. The repeatability was investigated by evaluating the intra-day, inter-day precisions and batch-to-batch reproducibility with relative standard deviations (RSDs) lower than 11%. At the same time, the method also showed high extraction speed, simplicity, practicality and low cost for the extraction inorganic anions. Finally, the proposed method was used to detect anions in different water samples successfully. The recoveries were in the range of 71.0-111%, and the RSDs were below 12% in the all cases.

  2. Theoretical Study on Ionic Liquid Based on 1-Ethyl-3-Methyl- Imidazolium Cation and Hexafluorophosphate or Tetrafluoroborate

    Institute of Scientific and Technical Information of China (English)

    Renqing Lü; Zuogang Cao; Guoping Shen

    2007-01-01

    The Hartree-Fock and DFT/B3LYP methods have been employed to investigate the electronic structures of l-ethyl-3-methyl-imidazolium cation (EMIM+), BF-4 , PF-6, EMIM+-BF-4, and EMIM+-PF6-using the Gaussian-94 soft-package at 6-31+G(d,p) basis set level for hydrogen, carbon, nitrogen, boron, phosphorus, and fluorine atoms. Comparison of the electronic structures of the lowest energy of EMIM+-BF4- and EMIM+-PF6- pairs, and single EMIM+, BF-4 and PF-6 showed that the optimized EMIM+-BF-4 and EMIM+-PF-6 pair conformers were BF-4 and PF-6 outside the 5-ring plane between the ethyl group and the methyl group. The cohesion of C-H…F hydrogen bond between cation and anion is reinforced by charge assistance. The interaction energy between EMIM+ and PF-6 is 328.8 kJ/mol at the B3LYP level and 326.6 kj/mol at the Hartree-Fock level, whereas that between EMIM+ and BFJ is 353.5 kj/mol at the B3LYP level and 350.5 kj/mol at the Hartree-Fock level. The low energy interactions caused by bulky asymmetric EMIM+, and charge dispersion of cation and anion give rise to the low melting point of ionic liquid EMIM+-BF-4 and EMIM+-PF-6. The two hydrogen bonding models of single hydrogen bond formation, and the hydrogen transfer between C2 in EMIM+ and F in BF-4 or PF-6 were principally depicted.

  3. 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.

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

    Science.gov (United States)

    Chen, Lei; Huang, Xiaojia

    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.

  5. EPR Study of Radicals in Irradiated Ionic Liquids and Implications for the Radiation Stability of Ionic Liquid-Based Extraction Systems

    CERN Document Server

    Shkrob, I A; Wishart, J F; Chemerisov, Sergey D.; Shkrob, Ilya A.; Wishart, James F.

    2007-01-01

    The radiation- and photo- chemistry of room temperature ionic liquids (ILs) composed of ammonium, phosphonium, pyrrolidinium, and imidazolium cations and bis(triflyl)amide, dicyanamide, and bis(oxalato)borate anions, have been studied using low-temperature Electron Paramagnetic Resonance (EPR). Several classes of radicals have been identified and related to reactions of the primary radiolytically generated electrons and holes. Large yields of terminal and penultimate C-centered radicals are observed in the aliphatic chains of the phosphonium, ammonium and pyrrolidinium cations, but not for imidazolium cation. This pattern can be accounted for by efficient deprotonation of a hole trapped on the cation (the radical dication) that competes with rapid charge transfer to a nearby anion. The latter leads to the formation of stable N- or O-centered radicals. The electrons either react with the protic impurity (for nonaromatic cations) yielding H atoms or the aromatic moiety (for imidazolium cations). Excitation of b...

  6. 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.

  7. 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.

  8. Ionic Liquid-based Microwave-assisted Liquid-liquid Microextraction and High Performance Liquid Chromatography Determination of Sulfonamides from Animal Oils

    Institute of Scientific and Technical Information of China (English)

    FENG Xu-dong; LIANG Fang-hui; SU Rui; WU Li-jie; LI Xue-yuan; WANG Xing-hua; ZHANG Han-qi

    2013-01-01

    The authors performed ionic liquid-based microwave-assisted liquid-liquid microextraction(IL-based MALLME) coupled with high performance liquid chromatographic separation for the determination of 6 sulfonamides (SAs) from animal oils.The target analytes were extracted from animal oil samples with sodium hydroxide solution containing 1-butyl-3-methylimidazolium tetrafluoroborateand as the extraction solvent under microwave irradiation.The experimental parameters of the IL-based MALLME,including types of ILs,volume of IL,amount of ion-pairing agent(NH4PF6),pH value of sample solution,and extraction temperature and time were evaluated.The limits of detection and quantification obtained were in a range of 0.4-0.5 μg/kg and a range of 1.2-1.8 μg/kg,respectively.The accuracy of the method was evaluated by analyzing five spiked animal oil samples at two fortified levels(5 and 50 μg/kg),and the recoveries of SAs varied from 81.4% to 114.5% with relative standard deviations ranging from 0.8% to 9.0%.

  9. ULTRASOUND-ASSISTED ORGANIC SYNTHESIS: ALCOHOL OXIDATION AND OLEFIN EPOXIDATION

    Science.gov (United States)

    Ultrasound-assisted Organic Synthesis: Alcohol Oxidation and Olefin EpoxidationUnnikrishnan R Pillai, Endalkachew Sahle-Demessie , Vasudevan Namboodiri, Quiming Zhao, Juluis EnriquezU.S. EPA , 26 W. Martin Luther King Dr. , Cincinnati, OH 45268 Phone: 513-569-773...

  10. 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.

  11. 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

    OpenAIRE

    Saha Sanjoy; Brahman Dhiraj; Sinha Biswajit

    2015-01-01

    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) sal...

  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 waters from PTP only galaxolide was found at a concentration higher than MQL.

  13. Estimation of lead in biological samples of oral cancer patients chewing smokeless tobacco products by ionic liquid-based microextraction in a single syringe system.

    Science.gov (United States)

    Arain, Sadaf S; Kazi, Tasneem G; Arain, Asma J; Afridi, Hassan I; Arain, Muhammad B; Brahman, Kapil D; Naeemullah; Panhwar, Abdul H; Arain, Mariam S

    2015-08-01

    Several studies have reported that the chewing habit of smokeless tobacco (SLT) has been associated with oral cancer. The aim of the present study was to evaluate the trace levels of lead (Pb) in biological samples (blood, scalp hair) of oral cancer patients and referents of the same age group (range 30-60 years). As the concentrations of Pb are very low in biological samples, so a simple and efficient ionic liquid-based microextraction in a single syringe system has been developed, as a prior step to determination by flame atomic absorption spectrometry. In this procedure, the hydrophobic chelates of Pb with ammonium pyrrolidinedithiocarbamate (APDC) were extracted into fine droplets of 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6] within a syringe while using Triton X-114 as a dispersant. Factors influencing the microextraction efficiency and determination, such as pH of the sample, volume of [C4MIM][PF6] and Triton X-114, ligand concentration, and incubation time, were studied. To validate the proposed method, certified reference materials were analyzed and the results of Pb(2+) were in good agreement with certified values. At optimum experimental values of significant variables, detection limit and enhancement factor were found to be 0.412 μg/L and 80, respectively. The coexisting ions showed no obvious negative outcome on Pb preconcentration. The proposed method was applied satisfactorily for the preconcentration of Pb(2+) in acid-digested SLT and biological samples of the study population. It was observed that oral cancer patients who consumed different SLT products have 2-3-fold higher levels of Pb in scalp hair and blood samples as compared to healthy referents (p < 0.001). While 31.4-50.8% higher levels of Pb were observed in referents chewing different SLT products as compared to nonconsumers (p < 0.01).

  14. Separation performance of cucurbit[7]uril in ionic liquid-based sol-gel coating as stationary phase for capillary gas chromatography.

    Science.gov (United States)

    Wang, Xiaogang; Qi, Meiling; Fu, Ruonong

    2014-12-05

    Here we report the separation performance of a new stationary phase of cucurbit[7]uril (CB7) incorporated into an ionic liquid-based sol-gel coating (CB7-SG) for capillary gas chromatography (GC). The CB7-SG stationary phase showed an average polarity of 455, suggesting its polar nature. Abraham system constants revealed that its major interactions with analytes include H-bond basicity (a), dipole-dipole (s) and dispersive (l) interactions. The CB7-SG stationary phase achieved baseline separation for a wide range of analytes with symmetrical peak shapes and showed advantages over the conventional polar stationary phase that failed to resolve some critical analytes. Also, it exhibited different retention behaviors from the conventional stationary phase in terms of retention times and elution order. Most interestingly, in contrast to the conventional polar phase, the CB7-SG stationary phase exhibited longer retentions for analytes of lower polarity but relatively comparable retentions for polar analytes such as alcohols and phenols. The high resolving ability and unique retention behaviors of the CB7-SG stationary phase may stem from the comprehensive interactions of the aforementioned interactions and shape selectivity. Moreover, the CB7-SG column showed good peak shapes for analytes prone to peak tailing, good thermal stability up to 280°C and separation repeatability with RSD values in the range of 0.01-0.11% for intra-day, 0.04-0.41% for inter-day and 2.5-6.0% for column-to-column, respectively. As demonstrated, the proposed coating method can simultaneously address the solubility problem with CBs for the intended purpose and achieve outstanding GC separation performance.

  15. Ultrasound-assisted extraction of pectin from sisal waste.

    Science.gov (United States)

    Maran, J Prakash; Priya, B

    2015-01-22

    In this study, an efficient ultrasound-assisted extraction (UAE) of pectin from sisal waste was investigated and optimized. Response surface methodology (RSM) based on a three-level four-factor Box-Behnken response surface design (BBD) was employed to optimize the extraction conditions (ultrasonic power, extraction temperature, extraction time and solid-liquid ratio). Analysis of variance showed that the contribution of a quadratic model was significant for the pectin extraction yield. The experimental yield (29.32%) was obtained under the optimal condition (ultrasonic power of 61 W, temperature of 50°C, time of 26 min and SL ratio of 1:28 g/ml) was well agreement with predicted values. Therefore, ultrasound-assisted extraction could be used as an alternative method to extract pectin from sisal waste with the advantages of lower extraction temperatures, shorter extraction time and reduced energy consumption. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

    Directory of Open Access Journals (Sweden)

    Fengli Chen

    2014-01-01

    Full Text Available 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.

  17. 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.

  18. New Method for the Estimation of Viscosity of Pure and Mixtures of Ionic Liquids Based on the UNIFAC–VISCO Model

    OpenAIRE

    Zhao, Nan; Jacquemin, Johan; Oozeerally, Ryan; Degirmenci, Volkan

    2016-01-01

    A modified UNIFAC–VISCO group contribution method was developed for the correlation and prediction of viscosity of ionic liquids as a function of temperature at 0.1 MPa. In this original approach, cations and anions were regarded as peculiar molecular groups. The significance of this approach comes from the ability to calculate the viscosity of mixtures of ionic liquids as well as pure ionic liquids. Binary interaction parameters for selected cations and anions were determined by fitting the ...

  19. Ultrasound assisted intensification of biodiesel production using enzymatic interesterification.

    Science.gov (United States)

    Subhedar, Preeti B; Gogate, Parag R

    2016-03-01

    Ultrasound assisted intensification of synthesis of biodiesel from waste cooking oil using methyl acetate and immobilized lipase obtained from Thermomyces lanuginosus (Lipozyme TLIM) as a catalyst has been investigated in the present work. The reaction has also been investigated using the conventional approach based on stirring so as to establish the beneficial effects obtained due to the use of ultrasound. Effect of operating conditions such as reactant molar ratio (oil and methyl acetate), temperature and enzyme loading on the yield of biodiesel has been investigated. Optimum conditions for the conventional approach (without ultrasound) were established as reactant molar ratio of 1:12 (oil:methyl acetate), enzyme loading of 6% (w/v), temperature of 40 °C and reaction time of 24 h and under these conditions, 90.1% biodiesel yield was obtained. The optimum conditions for the ultrasound assisted approach were oil to methyl acetate molar ratio of 1:9, enzyme loading of 3% (w/v), and reaction time of 3 h and the biodiesel yield obtained under these conditions was 96.1%. Use of ultrasound resulted in significant reduction in the reaction time with higher yields and lower requirement of the enzyme loading. The obtained results have clearly established that ultrasound assisted interesterification was a fast and efficient approach for biodiesel production giving significant benefits, which can help in reducing the costs of production. Reusability studies for the enzyme were also performed but it was observed that reuse of the catalyst under the optimum experimental condition resulted in reduced enzyme activity and biodiesel yield.

  20. Dynamic ultrasound-assisted extraction of polyphenols in tobacco.

    Science.gov (United States)

    Gu, Xungang; Cai, Jibao; Zhu, Xiaolan; Su, Qingde

    2005-12-01

    A novel extraction method, namely dynamic ultrasound-assisted extraction, is investigated. This technique is efficient with respect to both time and solvent consumption because it utilizes ultrasonic energy in dynamic mode during extraction. Polyphenols (chlorogenic acid, esculetin, rutin, scopoletin, and quercitrin) are extracted from a tobacco (Nicotina tobaccum L.) sample for 10 min with 6 mL of solvent. Fresh solvent is continuously pumped through the sample, with which the analytes can be rapidly extracted, and the possibility of degradation efficiently avoided. Methanol involving 0.5% w/v ascorbic acid was used as extraction solvent; optimal flow rate and extraction time were investigated. The extract was cleaned up by C18 disposable cartridge. The spiked and nonspiked tobacco samples were used for the evaluation of the proposed method. Recoveries obtained were varied from 96 to 108% and RSDs from 2.0 to 4.6%. This extraction technique was revealed to recover larger amounts of polyphenols from tobacco, compared to the static ultrasound-assisted extraction method.

  1. Ultrasound-assisted CO2 flooding to improve oil recovery.

    Science.gov (United States)

    Hamidi, Hossein; Sharifi Haddad, Amin; Mohammadian, Erfan; Rafati, Roozbeh; Azdarpour, Amin; Ghahri, Panteha; Ombewa, Peter; Neuert, Tobias; Zink, Aaron

    2017-03-01

    CO2 flooding process as a common enhanced oil recovery method may suffer from interface instability due to fingering and gravity override, therefore, in this study a method to improve the performance of CO2 flooding through an integrated ultraosund-CO2 flooding process is presented. Ultrasonic waves can deliver energy from a generator to oil and affect its properties such as internal energy and viscosity. Thus, a series of CO2 flooding experiments in the presence of ultrasonic waves were performed for controlled and uncontrolled temperature conditions. Results indicate that oil recovery was improved by using ultrasound-assisted CO2 flooding compared to conventional CO2 flooding. However, the changes were more pronounced for uncontrolled temperature conditions of ultrasound-assisted CO2 flooding. It was found that ultrasonic waves create a more stable interface between displacing and displaced fluids that could be due to the reductions in viscosity, capillary pressure and interfacial tension. In addition, higher CO2 injection rates, increases the recovery factor in all the experiments which highlights the importance of injection rate as another factor on reduction of the fingering effects and improvement of the sweep efficiency.

  2. 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.

  3. Simultaneous determination of cork taint and Brett character responsible compounds in wine using ultrasound-assisted emulsification microextraction with solidification of floating organic drop.

    Science.gov (United States)

    Pizarro, C; Sáenz-González, C; Pérez-del-Notario, N; González-Sáiz, J M

    2012-08-03

    In this study, ultrasound-assisted emulsification microextraction combined with solidification of floating organic drop method (USAEME-SFOD) has been proposed as a novel approach for the sensitive determination of haloanisoles and volatile phenols in wines. For this purpose, the influence of the different parameters affecting the procedure (type and volume of extraction solvent, temperature, time and ionic strength) was evaluated in order to optimise the efficiency of the process. Subsequently, the linearity, detection and quantification limits, precision, recoveries and applicability to real samples were studied, obtaining excellent method performance results. Moreover, USAEME-SFOD was compared with other liquid-liquid microextraction methods such as dispersive liquid-liquid microextraction (DLLME) and ultrasound-assisted emulsification microextraction (USAEME). This comparison study proved the suitability of USAEME-SFOD as an alternative to previously reported methods for the simultaneous determination of cork taint and Brett character responsible compounds in wines.

  4. Design and development of single stage purification of papain using Ionic Liquid based aqueous two phase extraction system and its Partition coefficient studies

    Directory of Open Access Journals (Sweden)

    Senthilkumar Rathnasamy

    2013-04-01

    Full Text Available As an emerging trend in bioseparation, aqueous two phase extractions based on phosponium ionic liquid have been utilized in this work to extract papain from Carica papaya fruit latex and the same wascompared with conventional aqueous two phase extraction system. Factors affecting the partition coefficient of papain such as ionic liquid concentration, pH of the extraction system and temperature have been investigated. The optimization studies show that ionic liquid concentrations and pH are majorly influencing the phaseformations and papain partitioning. It reveals the importance of electrostatic and hydrophobic interactions in the papain partitioning. Purification studies performed on Gel Filtration Chromatography shows that 96% of the papain enzyme could be extracted with the phosponium based ionic liquid in a single stage extraction. The final fraction containing papain enzyme was confirmed by SDS Page analysis.

  5. First principles molecular dynamics simulation of a task-specific ionic liquid based on silver-olefin complex: atomistic insight into separation process

    CERN Document Server

    Jiang, De-en

    2008-01-01

    First principles molecular dynamics based on density functional theory is applied to a hypothetical ionic liquid whose cations and anions are silver-ethylene complex [Ag(C2H4)2+] and tetrafluoroborate [BF4-], respectively. This ionic liquid represents a group of task-specific silver complex-based ionic liquids synthesized recently. Molecular dynamics simulations at two temperatures are performed for five picoseconds. Events of association, dissociation, exchange, and recombination of ethylene with silver cation are observed. A mechanism of ethylene transfer similar to the Grotthus type of proton transfer in water is identified, where a silver cation accepts one ethylene molecule and donates another to a neighboring silver cation. This mechanism may contribute to fast transport of olefins through ionic liquid membranes based on silver complexes for olefin/paraffin separation.

  6. First principles molecular dynamics simulation of a task-specific ionic liquid based on silver-olefin complex: atomistic insights into a separation process.

    Science.gov (United States)

    Jiang, De-en; Dai, Sheng

    2008-08-21

    First principles molecular dynamics based on density functional theory is applied to a hypothetical ionic liquid whose cations and anions are silver-ethylene complex [Ag(C2H4)2+] and tetrafluoroborate [BF4-], respectively. This ionic liquid represents a group of task-specific silver complex-based ionic liquids synthesized recently. Molecular dynamics simulations at two temperatures are performed for five picoseconds. Events of association, dissociation, exchange, and recombination of ethylene with silver cation are found. A mechanism of ethylene transfer similar to the Grotthus type of proton transfer in water is identified, where a silver cation accepts one ethylene molecule and donates another to a neighboring silver cation. This mechanism may contribute to fast transport of olefins through ionic liquid membranes based on silver complexes for olefin/paraffin separation.

  7. Extending the role of liposuction in body contouring with ultrasound-assisted liposuction.

    Science.gov (United States)

    Rohrich, R J; Beran, S J; Kenkel, J M; Adams, W P; DiSpaltro, F

    1998-04-01

    The initial experience with ultrasound-assisted liposuction in treating difficult fibrous areas, such as gynecomastia, hitherto not uniformly responsive to traditional suction-assisted lipoplasty, has led to the evolution and improvement of ultrasound-assisted liposuction techniques. This prospective study examined 114 consecutive patients treated with ultrasound-assisted liposuction over a 13-month period, from September of 1996 to September of 1997. The means by which this procedure helps achieve fat contouring differs from that of suction-assisted lipoplasty. Ultrasound-assisted liposuction removes fat through a fat emulsification process termed "cavitation," whereas suction-assisted lipoplasty achieves contouring through the mechanical avulsion of fat. The technique for the use of ultrasound-assisted liposuction has changed significantly from our initial series of patients to our current technique. To optimize the benefits of both ultrasound-assisted and traditional suction-assisted lipoplasty, we use a three-stage technique consisting of infiltration, ultrasound-assisted sculpturing, and suction-assisted lipoplasty for evacuation and final contouring. This has decreased our operative time, minimized complications, and optimized our body contouring results. Data were collected intraoperatively, including treatment times, treatment volumes, and treatment areas for both suction-assisted and ultrasound-assisted lipoplasty. A total of 114 patients were treated with ultrasound-assisted liposuction between September of 1996 and September of 1997. There were 23 male patients and 91 female patients. In general, the average total volume removed with this procedure decreased by about 50 percent throughout the series, whereas the suction-assisted lipoplasty volume increased correspondingly by 50 percent. Overall, suction-assisted lipoplasty volume was approximately two times ultrasound-assisted liposuction volume in the same area. Exceptions to this include the dense

  8. Ionic liquid-based totally organic solvent-free emulsification microextraction coupled with high performance liquid chromatography for the determination of three acaricides in fruit juice.

    Science.gov (United States)

    Zhang, Jiaheng; Liang, Zhe; Guo, Hao; Gao, Peng; Lu, Runhua; Zhou, Wenfeng; Zhang, Sanbing; Gao, Haixiang

    2013-10-15

    A novel, totally organic solvent-free emulsification microextraction (TEME) technique using ionic liquids (ILs) is proposed in this study. Seven bis(trifluoromethylsulfonyl)imide ionic liquids were synthesized. After comparing the physicochemical properties of the ionic liquids and their application to microextraction experiments, 1-hexyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([C6MIM][NTf2]), which has moderate surface tension and viscosity, was selected as the extraction solvent. The dispersion of ILs and mass transfer were accelerated by ultrasound irradiation and temperature control processes. Therefore, no dispersive organic solvent was needed. Several variables, such as ionic liquid volume, duration of the ultrasound extraction, dispersion temperature, ionic strength and centrifugation time were investigated and optimized. Under the optimum conditions, the calibration curve was linear in the range of 0.1-600 μg L(-1) for chlorfenapyr and fenpyroximate and 0.5-600 μg L(-1) for spirodiclofen, with correlation coefficients of 0.9994-0.9999. The enrichment factors were between 261 and 285. The limits of detection (LODs) were 0.02-0.06 μg L(-1). Real fruit juice samples (at fortified levels of 10 μg L(-1) and 30 μg L(-1)) were successfully analyzed using the proposed method. The relative recoveries and enrichment factors were in the range of 92-104%. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Development of a robust ionic liquid-based dispersive liquid-liquid microextraction against high concentration of salt for preconcentration of trace metals in saline aqueous samples: Application to the determination of Pb and Cd

    Energy Technology Data Exchange (ETDEWEB)

    Yousefi, Seyed Reza [School of Chemistry, University College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Shemirani, Farzaneh, E-mail: shemiran@khayam.ut.ac.ir [School of Chemistry, University College of Science, University of Tehran, Tehran (Iran, Islamic Republic of)

    2010-06-11

    A new ionic liquid-based dispersive liquid-liquid microextraction method was developed for preconcentration and determination of compounds in aqueous samples containing very high salt concentrations. This method can solve the problems associated with the limited application of the conventional IL-based DLLME in these samples. This is believed to arise from dissolving of the ionic liquids in aqueous samples with high salt content. In this method, the robustness of microextraction system against high salt concentration (up to 40%, w/v) is increased by introducing a common ion of the ionic liquid into the sample solution. The proposed method was applied satisfactorily to the preconcentration of lead and cadmium in saline samples. After preconcentration, the settled IL-phase was dissolved in 100 {mu}L ethanol and aspirated into the flame atomic absorption spectrometer (FAAS) using a home-made microsample introduction system. Several variables affecting the microextraction efficiency were investigated and optimized. Under the optimized conditions and preconcentration of only 10 mL of sample, the enhancement factors of 273 and 311 and the detection limits of 0.6 {mu}g L{sup -1} and 0.03 {mu}g L{sup -1} were obtained for lead and cadmium, respectively. Validation of the method was performed by both an analysis of a certified reference material (CRM) and comparison of results with those obtained by ISO standard method.

  10. Biodiesel Production from Bulk Frying Oil with Ultrasound Assisted

    Directory of Open Access Journals (Sweden)

    Widayat

    2013-07-01

    Full Text Available The objective of this research is to optimize of biodiesel production with ultrasound assisted. Optimization was used central composite design methods. Biodiesel was produced from frying oil with KOH catalyst and ultrasonic assisted. The variables were investigated temperature, catalyst concentration and ratio of methanol to oil. Biodiesel was separated from reactant and impurities with decantation process and distillation process. The results of research obtained optimum conversion 85.95% in operation condition are methanol/oil 5.05:1, catalyst concentration 1.65% and temperature reaction 50°C. Mathematic modeling for describe in this process like expressed; Y = 86.2107 - 7.4287X1 + 1.0661X2 + 0.6289X3 - 2.5319X12 - 2.0603X22 - 1.0618X32.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. SO3H-functionalized organic-inorganic ionic liquids based on polyoxometalates characterization and their application in Csbnd C coupling reaction

    Science.gov (United States)

    Rafiee, Ezzat; Mirnezami, Fakhrosadat; Kahrizi, Masoud

    2016-09-01

    Different ionic liquids (ILs) with SO3H as functional group were achieved by combining SO3H-functionalized organic cations and polyoxometalates (POM). The obtained salts were characterized and their catalytic activities investigated in Csbnd C coupling between benzhydrol and aromatic compounds at neat conditions, including the effect of organic cations, influence of POMs, optimization of reaction conditions, and reusability of the catalyst. Furthermore, Recovery, reusability and activity of ILs as heterogeneous catalysts were studied at least four times.

  16. Novel Brφnsted Acidic Ionic Liquid Based on a Cyclic Guanidinium Cation: a Green, Efficient, and Recyclable Dual Slovent-catalyst System for Fisher Esterification

    Institute of Scientific and Technical Information of China (English)

    GUO Xu; DUAN Hai-feng; SUN Hai; CAO Jun-gang; LIN Ying-jie

    2007-01-01

    A novel Brφnsted acidic ionic liquid(IL) based on the cyclic guanidinium cation has been synthesized. This IL,as a strong Brφnsted acid catalyst or solvent, shows high catalytic activity and biphsaic behavor in the esterifications of carboxylic acids and alcohols. The produced esters as a separate phase can be conveniently decanted out from the IL and the IL is recyclable without any loss of catalytic activity.

  17. Enzyme-assisted extraction and ionic liquid-based dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for determination of patulin in apple juice and method optimization using central composite design.

    Science.gov (United States)

    Mohammadi, Abdorreza; Tavakoli, Rouya; Kamankesh, Marzieh; Rashedi, Hamid; Attaran, Abdolmohammad; Delavar, Mostafa

    2013-12-01

    A simple and highly sensitive analytical methodology for isolation and determination of patulin in apple-juice samples, based on enzyme-assisted extraction (EAE) and ionic liquid-based dispersive liquid-liquid microextraction (IL-DLLME) was developed and optimized. Enzymes play essential roles in eliminating interference and increasing the extraction efficiency of patulin. Apple-juice samples were treated with pectinase and amylase. A mixture of 80 μL ionic liquid and 600 μL methanol (disperser solvent) was used for the IL-DLLME process. The sedimented phase was analyzed by high-performance liquid chromatography (HPLC). Experimental parameters controlling the performance of DLLME, were optimized using response surface methodology (RSM) based on central composite design (CCD). Under optimum conditions, the calibration curves showed high levels of linearity (R(2)>0.99) for patulin in the range of 1-200 ng g(-1). The relative standard deviation (RSD) for the seven analyses was 7.5%. The limits of detection (LOD) and limits of quantification (LOQ) were 0.15 ng g(-1) and 0.5 ng g(-1), respectively. The merit figures, compared with other methods, showed that new proposed method is an accurate, precise and reliable sample-pretreatment method that substantially reduces sample matrix interference and gives very good enrichment factors and detection limits for investigation trace amount of patulin in apple-juice samples.

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

    Science.gov (United States)

    Jalbani, Nusrat; Soylak, Mustafa

    2015-01-01

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

  19. LiFePO 4 and graphite electrodes with ionic liquids based on bis(fluorosulfonyl)imide (FSI) - for Li-ion batteries

    Science.gov (United States)

    Guerfi, A.; Duchesne, S.; Kobayashi, Y.; Vijh, A.; Zaghib, K.

    Ambient-temperature ionic liquids (IL) based on bis(fluorosulfonyl)imide (FSI) as anion and 1-ethyl-3-methyleimidazolium (EMI) or N-methyl- N-propylpyrrolidinium (Py13) as cations have been investigated with natural graphite anode and LiFePO 4 cathode in lithium cells. The electrochemical performance was compared to the conventional solvent EC/DEC with 1 M LiPF 6 or 1 M LiFSI. The ionic liquid showed lower first coulombic efficiency (CE) at 80% compared to EC-DEC at 93%. The impedance spectroscopy measurements showed higher resistance of the diffusion part and it increases in the following order: EC-DEC-LiFSI < EC-DEC-LiPF 6 < Py13(FSI)-LiFSIE = MI(FSI)-LiFSI. On the cathode side, the lower reversible capacity at 143 mAh g -1 was obtained with Py13(FSI)-LiFSI; however, a comparable reversible capacity was found in EC-DEC and EMI(FSI)-LiFSI. The high viscosity of the ionic liquids suggests that different conditions such as vacuum and 60 °C are needed to improve impregnation of IL in the electrodes. With these conditions, the reversible capacity improved to 160 mAh g -1 at C/24. The high-rate capability of LiFePO 4 was evaluated in polymer-IL and compared to the pure IL cells. The reversible capacity at C/10 decreased from 155 to only 126 mAh g -1 when the polymer was present.

  20. LiFePO{sub 4} and graphite electrodes with ionic liquids based on bis(fluorosulfonyl)imide (FSI){sup -} for Li-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Guerfi, A.; Duchesne, S.; Vijh, A.; Zaghib, K. [Institut de Recherche d' Hydro-Quebec, Varennes, QC (Canada); Kobayashi, Y. [Institut de Recherche d' Hydro-Quebec, Varennes, QC (Canada); Central Research Institute of Electric Power Industry, 2-11-1, Iwado Kita, Komae-shi, Tokyo 201-8511 Japan

    2008-01-10

    Ambient-temperature ionic liquids (IL) based on bis(fluorosulfonyl)imide (FSI) as anion and 1-ethyl-3-methyleimidazolium (EMI) or N-methyl-N-propylpyrrolidinium (Py13) as cations have been investigated with natural graphite anode and LiFePO{sub 4} cathode in lithium cells. The electrochemical performance was compared to the conventional solvent EC/DEC with 1 M LiPF{sub 6} or 1 M LiFSI. The ionic liquid showed lower first coulombic efficiency (CE) at 80% compared to EC-DEC at 93%. The impedance spectroscopy measurements showed higher resistance of the diffusion part and it increases in the following order: EC-DEC-LiFSI < EC-DEC-LiPF{sub 6} < Py13(FSI)-LiFSIE = MI(FSI)-LiFSI. On the cathode side, the lower reversible capacity at 143 mAh g{sup -1} was obtained with Py13(FSI)-LiFSI; however, a comparable reversible capacity was found in EC-DEC and EMI(FSI)-LiFSI. The high viscosity of the ionic liquids suggests that different conditions such as vacuum and 60 C are needed to improve impregnation of IL in the electrodes. With these conditions, the reversible capacity improved to 160 mAh g{sup -1} at C/24. The high-rate capability of LiFePO{sub 4} was evaluated in polymer-IL and compared to the pure IL cells. The reversible capacity at C/10 decreased from 155 to only 126 mAh g{sup -1} when the polymer was present. (author)

  1. A new dispersive liquid-liquid microextraction using ionic liquid based microemulsion coupled with cloud point extraction for determination of copper in serum and water samples.

    Science.gov (United States)

    Arain, Salma Aslam; Kazi, Tasneem Gul; Afridi, Hassan Imran; Arain, Mariam Shahzadi; Panhwar, Abdul Haleem; Khan, Naeemullah; Baig, Jameel Ahmed; Shah, Faheem

    2016-04-01

    A simple and rapid dispersive liquid-liquid microextraction procedure based on ionic liquid assisted microemulsion (IL-µE-DLLME) combined with cloud point extraction has been developed for preconcentration copper (Cu(2+)) in drinking water and serum samples of adolescent female hepatitits C (HCV) patients. In this method a ternary system was developed to form microemulsion (µE) by phase inversion method (PIM), using ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C4mim][PF6]) and nonionic surfactant, TX-100 (as a stabilizer in aqueous media). The Ionic liquid microemulsion (IL-µE) was evaluated through visual assessment, optical light microscope and spectrophotometrically. The Cu(2+) in real water and aqueous acid digested serum samples were complexed with 8-hydroxyquinoline (oxine) and extracted into IL-µE medium. The phase separation of stable IL-µE was carried out by the micellar cloud point extraction approach. The influence of of different parameters such as pH, oxine concentration, centrifugation time and rate were investigated. At optimized experimental conditions, the limit of detection and enhancement factor were found to be 0.132 µg/L and 70 respectively, with relative standard deviation <5%. In order to validate the developed method, certified reference materials (SLRS-4 Riverine water) and human serum (Sero-M10181) were analyzed. The resulting data indicated a non-significant difference in obtained and certified values of Cu(2+). The developed procedure was successfully applied for the preconcentration and determination of trace levels of Cu(2+) in environmental and biological samples.

  2. Ionic Liquid Based Electrolyte with Mesoporous Silica SBA-15 as Framework for Quasi-solid-state Dye-sensitized Solar Cells

    Institute of Scientific and Technical Information of China (English)

    YANG, Hong; CHENG, Yun-Fei; ZHOU, Zhi-Guo; CHEN, Zhi-Gang; LI, Fu-You; YI, Tao; HUANG, Chun-Hui

    2006-01-01

    Quasi-solid-state electrolytes were fabricated with mesoporous silica SBA-15 as a framework material. Ionic conductivity measurements revealed that SBA-15 can enhance the conductivity of the quasi-solid-state electrolyte.The diffusion coefficients of polyiodide ions such as I-3 and I-5 which were confirmed by Raman spectroscopic measurement, were about twice larger than that of I-. The optimized photoenergy conversion efficiency of dye-sensitized solar cells (DSSC) with the quasi-solid-state electrolyte was 4.3% under AM 1.5 irradiation at 75 mW·cm-2 light intensity.

  3. Comparison of ultrasound-assisted cloud point extraction and ultrasound-assisted dispersive liquid liquid microextraction for copper coupled with spectrophotometric determination.

    Science.gov (United States)

    Yang, Shengchun; Fang, Xiang; Duan, Liju; Yang, Shu; Lei, Zirong; Wen, Xiaodong

    2015-09-01

    In this work, ultrasound-assisted cloud point extraction (UA-CPE) and ultrasound-assisted dispersive liquid liquid microextraction (UA-DLLME) were investigated and compared firstly as ultrasound-assisted liquid phase microextraction methods, which were coupled with spectrophotometer for copper preconcentration and detection. Compared to conventional CPE and DLLME, the extraction patterns were changed and improved by the effect of ultrasound. As novel methods, their applications were expanded and the analytical performance of spectrophotometric determination for copper was considerably improved. The influence factors of UA-CPE and UA-DLLME were studied in detail. Under the optimal conditions, the limits of detection (LODs) for copper were 0.7 μg L(-1) of UA-CPE and 0.8 μg L(-1) of UA-DLLME with sensitivity enhancement factors (EFs) of 17 and 16. The developed methods were applied to the determination of trace copper in real water samples with satisfactory analytical results.

  4. Comparison of ultrasound-assisted cloud point extraction and ultrasound-assisted dispersive liquid liquid microextraction for copper coupled with spectrophotometric determination

    Science.gov (United States)

    Yang, Shengchun; Fang, Xiang; Duan, Liju; Yang, Shu; Lei, Zirong; Wen, Xiaodong

    2015-09-01

    In this work, ultrasound-assisted cloud point extraction (UA-CPE) and ultrasound-assisted dispersive liquid liquid microextraction (UA-DLLME) were investigated and compared firstly as ultrasound-assisted liquid phase microextraction methods, which were coupled with spectrophotometer for copper preconcentration and detection. Compared to conventional CPE and DLLME, the extraction patterns were changed and improved by the effect of ultrasound. As novel methods, their applications were expanded and the analytical performance of spectrophotometric determination for copper was considerably improved. The influence factors of UA-CPE and UA-DLLME were studied in detail. Under the optimal conditions, the limits of detection (LODs) for copper were 0.7 μg L-1 of UA-CPE and 0.8 μg L-1 of UA-DLLME with sensitivity enhancement factors (EFs) of 17 and 16. The developed methods were applied to the determination of trace copper in real water samples with satisfactory analytical results.

  5. 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.

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

    Science.gov (United States)

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

    2012-04-01

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

  7. 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.

  8. 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.

  9. 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

    2013-09-01

    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.

  10. Ultrasound-assisted synthesis of aliphatic acid esters at room temperature.

    Science.gov (United States)

    Hobuss, Cristiane B; Venzke, Dalila; Pacheco, Bruna S; Souza, Alexander O; Santos, Marco A Z; Moura, Sidnei; Quina, Frank H; Fiametti, Karina G; Vladimir Oliveira, J; Pereira, Claudio M P

    2012-05-01

    This work describes the ultrasound-assisted synthesis of saturated aliphatic esters from synthetic aliphatic acids and either methanol or ethanol. The products were isolated in good yields after short reaction times under mild conditions.

  11. Antimicrobial activity of ultrasound-assisted solvent-extracted spices.

    Science.gov (United States)

    Thongson, C; Davidson, P M; Mahakarnchanakul, W; Weiss, J

    2004-01-01

    The objective of this research was to determine the antimicrobial activity of conventional and high-intensity ultrasound-assisted (HI-US) solvent-extracted Thai spices, including ginger (Zingiber officinale Rose), fingerroot (Bosenbergia pandurata Holtt) and turmeric (Curouma longa Linn). Extracts were obtained using hexane, isopropanol and a 7 : 3 isopropanol : hexane mixture as solvents with and without HI-US. The antimicrobial activity of the extracts was assayed against four strains each of Listeria monocytogenes and Salmonella Typhimurium DT 104 using an agar dilution assay. Application of HI-US did not alter antibacterial activity against S. Typhimurium, but antilisterial activity of some HI-US spice extracts decreased. Solvent type affected antimicrobial efficacy of extracts with hexane producing the least antimicrobial activity. Fingerroot extracted with isopropanol-hexane and without HI-US had the best antilisterial effect while HI-US-isopropanol fingerroot extract had the greatest antimicrobial efficacy against S. Typhimurium. Application of HI-US reduced time of extraction to 5 min, compared with the 24 h required for conventional extraction and maintained antimicrobial activity against Salmonella but slightly reduced activity against Listeria. HI-US in combination with proper solvent selection may offer a new tool to optimize extraction of spice essential oil for use as antimicrobial agents, and reduce processing time and costs.

  12. Ultrasound assisted extraction of polysaccharides from hazelnut skin.

    Science.gov (United States)

    Yılmaz, Tuncay; Tavman, Şebnem

    2016-03-01

    In this study ultrasound assisted extraction (UAE) of polysaccharides from hazelnut skin has been studied. Optimum sonication time has been evaluated depending on responses such as amount of carbohydrate and dried sample and thermogravimetric analysis. Chemical and structural properties of extracted material have been determined by Fourier transform spectroscopy attenuated-total reflectance (FTIR-ATR) spectroscopy. Pretreated hazelnut skin powders were extracted in distilled water. Mixture was sonicated by ultrasonic processor probe for 15, 30, 45, 60, 90, and 120 min. The results of UAE showed that maximum ethanol insoluble extracts in 60 min and the highest dry matter content could be obtained in 120 min extraction. Although total carbohydrate content of ethanol insoluble dry extract decreased with time, total carbohydrate in ethanol soluble fraction increased. Polysaccharides extracted from hazelnut skin were assumed to be pectic polysaccharide according to the literature survey of FTIR analysis result. Application time of UAE has an important effect on extraction of polysaccharide from hazelnut skin. This affect could be summarized by enhancing extraction yield up to critical level. Decrease of the yield in ethanol insoluble part could be explained by polymer decomposition. Most suitable model was hyperbolic model by having the lowest root mean square error and the highest R(2) values.

  13. Ultrasound assisted extraction and characterization of pectin from tomato waste.

    Science.gov (United States)

    Grassino, Antonela Ninčević; Brnčić, Mladen; Vikić-Topić, Dražen; Roca, Sunčica; Dent, Maja; Brnčić, Suzana Rimac

    2016-05-01

    Pectin was extracted from tomato waste using two different extraction methods to assess its potential utilization as an alternative source of commercial pectin production. Tomato waste was treated with ammonium oxalate/oxalic acid by conventional extraction (CE), under reflux and ultrasound assisted extraction (UAE) at 37 kHz and temperatures of 60 °C and 80 °C. The pectin obtained from these methods was analysed and compared in terms of yield, chemical properties and structure. Among examined methods, CE at 60 °C resulted with the highest yield, but UAE during 15 min of sonication produced the pectin of better quality (anhydrouronic acid, methoxy and calcium pectate contents and degree of esterification). NMR and FTIR spectroscopy of isolated pectins revealed predominantly esterified structure, irrespective of extraction conditions. The comparison of the pectin yields obtained after extraction at 80 °C, indicate that similar values were found at times of 24h and 15 min for CE and UAE, respectively. According to obtained results it can be concluded that main advantage of UAE is considerable shortening of extraction procedure with strong emphasis on environmental friendly processing approach. Therefore, these results suggested that UAE could be used as an efficient technique for the extraction of pectin from tomato waste and by-products. Copyright © 2015 Elsevier Ltd. All rights reserved.

  14. Ultrasound-assisted bioethanol production from waste newspaper.

    Science.gov (United States)

    Subhedar, Preeti B; Gogate, Parag R

    2015-11-01

    The present work deals with intensification of bioethanol production from waste newspaper using Saccharomyces cerevisiae using ultrasonic irradiations. The effect of different process parameters such as application of ultrasonic irradiation at different growth phases, irradiation time, ultrasonic power and duty cycle on the bioethanol production has been investigated. The favorable conditions for the maximum yield were established as application of ultrasonic irradiation (duration of 10 min) to fermentation broth at 12 h of growth phase with 25 kHz frequency, 160 W power and 20% duty cycle. The bioethanol productivity was increased by 1.8 times from 7.8 to 14.1 g/L compared with the non-sonicated control fermentation. Decrease in glucose concentration from 0.63% to 0.2% w/v in ultrasound-assisted fermentation confirmed the improved substrate uptake of the microbial cell due to the application of ultrasound. ESEM analysis also confirmed the changes in the cell morphology leading to improved cell permeability. Results were fitted to an unstructured kinetic model comprising of the kinetic and physiological parameters. Overall, the work has demonstrated an intensified approach for the bioethanol production based on the use of ultrasound.

  15. Recent developments on ultrasound assisted catalyst-free organic synthesis.

    Science.gov (United States)

    Banerjee, Bubun

    2017-03-01

    Mother Nature needs to be protected from ever increasing chemical pollutions associated with synthetic organic processes. The fundamental challenge for today's methodologists is to make their protocols more environmentally benign and sustainable by avoiding the extensive use of hazardous reagents and solvents, harsh reaction conditions, and toxic metal catalysts. However, the people of the twenty-first century are well aware about the side effects of those hazardous substances used and generated by the chemical processes. As a result, the last decade has seen a tremendous outburst in modifying chemical processes to make them 'sustainable' for the betterment of our environment. Catalysts play a crucial role in organic synthesis and thus they find huge applications and uses. Scientists' continuously trying to modify the catalysts to reduce their toxicity level, but the most benign way is to design an organic reaction without catalyst(s), if possible. It is worthy to mention that the involvement of ultrasound in organic synthesis is sometimes fulfilling this goal. In many occasions the applications of ultrasound can avoid the use of catalysts in organic reactions. Such beneficial features as a whole have motivated the organic chemists to apply ultrasonic irradiation in more heights and as a results, in recent past, there were immense applications of ultrasound in organic reactions for the synthesis of diverse organic scaffolds under catalyst-free condition. The present review summarizes the latest developments on ultrasound assisted catalyst-free organic synthesis reported so far. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. 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.

  17. 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

    2015-02-25

    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 (Al(3+)) in scalp hair samples of Alzheimer's (AD) patients, prior to analyzing by flame atomic absorption spectrometry (FAAS). The Al(3+) 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 (3s) 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) Al(3+) 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 Al(3+) 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.

  18. One-pot synthesis of SnO{sub 2}/reduced graphene oxide nanocomposite in ionic liquid-based solution and its application for lithium ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Gu, Changdong, E-mail: cdgu@zju.edu.cn; Zhang, Heng; Wang, Xiuli; Tu, Jiangping

    2013-10-15

    Graphical abstract: - Highlights: • A facile and low-temperature method is developed for SnO{sub 2}/graphene composite. • Synthesis performed in a choline chloride-based ionic liquid. • The composite shows an enhanced cycling stability as anode for Li-ion batteries. • 4 nm SnO{sub 2} nanoparticles mono-dispersed on the surface of reduced graphene oxide. - Abstract: A facile and low-temperature method is developed for SnO{sub 2}/graphene composite which involves an ultrasonic-assistant oxidation–reduction reaction between Sn{sup 2+} and graphene oxide in a choline chloride–ethylene glycol based ionic liquid under ambient conditions. The reaction solution is non-corrosive and environmental-friendly. Moreover, the proposed technique does not require complicated infrastructures and heat treatment. The SnO{sub 2}/graphene composite consists of about 4 nm sized SnO{sub 2} nanoparticles with cassiterite structure mono-dispersed on the surface of reduced graphene oxide. As anode for lithium-ion batteries, the SnO{sub 2}/graphene composite shows a satisfying cycling stability (535 mAh g{sup −1} after 50 cycles @100 mA g{sup −1}), which is significantly prior to the bare 4 nm sized SnO{sub 2} nanocrsytals. The graphene sheets in the hybrid nanostructure could provide a segmentation effect to alleviate the volume expansion of the SnO{sub 2} and restrain the small and active Sn-based particles aggregating into larger and inactive clusters during cycling.

  19. 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).

  20. A Computational Exploration of H2S and CO2 Capture by Ionic Liquids Based on α-Amino Acid Anion and N7,N9-Dimethyladeninium Cation.

    Science.gov (United States)

    Seyedhosseini, Badrosadat; Izadyar, Mohammad; Housaindokht, Mohammad Reza

    2017-06-08

    Hydrogen sulfide (H2S) and carbon dioxide (CO2) adsorption on a series of the aliphatic amino acid ionic liquids (AAILs) composed of N7,N9- dimethyladeninium cation with amino acid anions (AA = Gly, Ala, Val, Leu, and Ile) as the functionalized ILs with dual groups of amine have been investigated. On the basis of the obtained data, the possible sites of H2S adsorption are twice those of CO2 on the ionic liquids, and also the average adsorption energy of H2S (ΔE = -51.5 kJ mol(-1)) in the most stable region of adsorption is twice greater than that of CO2 (ΔE = -25.5 kJ mol(-1)). An increase in the length of the side chain of the amino acids increases the interaction energy of the H2S and CO2 capture (on the amine group of the [AA](-) anions). Quantum theory of atoms in molecules analysis confirmed the noncovalent nature of the N···C bond formed between CO2 and N atom in both of the amine groups and S-H···O and S-H···N bond critical points of H2S on [dMA][AA]. Natural bond orbital analysis indicates that charge transfer in H2S adsorption is more important than CO2 capture. Finally, a correlation between the adsorption energy and the sum of stability energies (∑E(2)) in the most stable region has been obtained and discussed.

  1. 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.

  2. In situ SEM observation of the Si negative electrode reaction in an ionic-liquid-based lithium-ion secondary battery.

    Science.gov (United States)

    Tsuda, Tetsuya; Kanetsuku, Tsukasa; Sano, Teruki; Oshima, Yoshifumi; Ui, Koichi; Yamagata, Masaki; Ishikawa, Masashi; Kuwabata, Susumu

    2015-06-01

    By exploiting characteristics such as negligible vapour pressure and ion-conductive nature of an ionic liquid (IL), we established an in situ scanning electron microscope (SEM) method to observe the electrode reaction in the IL-based Li-ion secondary battery (LIB). When 1-ethyl-3-methylimidazolium bis(fluorosulfonyl)amide ([C2mim][FSA]) with lithium bis(trifluoromethanesulfonyl)amide (Li[TFSA]) was used as the electrolyte, the Si negative electrode exhibited a clear morphology change during the charge process, without any solid electrolyte interphase (SEI) layer formation, while in the discharge process, the appearance was slightly changed, suggesting that a morphology change is irreversible in the charge-discharge process. On the other hand, the use of 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide ([C2mim][TFSA]) with Li[TFSA] did not induce a change in the Si negative electrode. It is interesting to note this distinct contrast, which could be attributed to SEI layer formation from the electrochemical breakdown of [C2mim](+) at the Si negative electrode|separator interface in the [C2mim][TFSA]-based LIB. This in situ SEM observation technique could reveal the effect of the IL species electron-microscopically on the Si negative electrode reaction.

  3. Arsenic speciation analysis in mono-varietal wines by on-line ionic liquid-based dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Escudero, Leticia B; Martinis, Estefanía M; Olsina, Roberto A; Wuilloud, Rodolfo G

    2013-05-01

    A highly efficient separation and pre-concentration method for arsenic species determination, based on ionic liquid (IL) dispersive microextraction technique implemented in a flow analysis system, is proposed. Highly selective separation of arsenite species [As(III)] was achieved by chelation with sodium diethyldithiocarbamate (DDTC) followed by dispersion with 40 mg of 1-octyl-3-methylimidazolium hexafluorophosphate ([C(8)mim][PF(6)]) IL. Analyte extraction, retention and separation of IL phase were achieved with a packed microcolumn and As(III) was determined in eluent solution by electrothermal atomic absorption spectrometry (ETAAS). Concentration of As(V) was deduced by the difference between total inorganic arsenic and As(III). Thus, determination of total arsenic was performed by previous degradation of organo-arsenic species, followed by a reduction. Under optimal conditions, As(III) extraction efficiency was 100% and a sensitivity enhancement factor of 46 was obtained with only 4.0 ml of sample The method was successfully applied for arsenic speciation studies in mono-varietal wines.

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

    Science.gov (United States)

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

    2016-12-01

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

  5. Application of ionic liquid-based dispersive liquid phase microextraction for highly sensitive simultaneous determination of three endocrine disrupting compounds in food packaging.

    Science.gov (United States)

    Wang, Lingling; Zhang, Danfeng; Xu, Xu; Zhang, Lei

    2016-04-15

    Ionic liquid (IL) dispersive liquid-liquid microextraction (DLLME) method was successfully developed for extracting three endocrine disrupting compounds (EDCs) (bisphenol A, bisphenol AF and bisphenol AP) from the food packaging. 1-Octyl-3-methylimidazoliumhexafluorophosphate ([C8MIM][PF6]) was selected as extraction solution. The extraction procedure did not require a dispersive solvent. Three EDCs extraction kinetics were found to be very fast and the equilibrium was attained within 3.0 min following the pseudo-first-order model. The H-bonding and hydrophobic interactions play an important role in the partitioning of EDCs into IL from aqueous solution. The recovered IL could be reused for three runs without significant loss of extraction efficiencies. The spiked recoveries of three targets in food packaging were in the range of 97.8-103.1%. The limits of detection ranged from 0.50 to 1.50 ng mL(-1) (S/N=3). As a result, this method has been successfully applied for the sensitive detection of three EDCs in real samples.

  6. [Determination of five triazine herbicides in infant milk powder by high performance liquid chromatography coupled with ionic liquid-based homogeneous liquid-liquid microextraction].

    Science.gov (United States)

    Zhang, Liyuan; Yao, Di; Li, Na; Zhang, Hanqi; Yu, Aimin

    2015-07-01

    A high performance liquid chromatography coupled with homogeneous liquid-liquid microextraction was developed for the determination of five triazine herbicides in infant milk powders. The ionic liquid was used as microextraction solvent. The separation of the herbicides was performed on an Eclipse XDB-C18 column using acetonitrile and water as mobile phases in gradient mode. The effects of homogeneous liquid-liquid extraction conditions on the experimental results were investigated in detail. Under the optimized experimental conditions, the calibration curves for determining the analytes were linear and the correlation coefficients were ≥ 0.9992. The limits of detection for cyanazine, desmetryn, terbumeton, terbuthylazine and dimethametryn were 12.1, 13.8, 11.8, 14.6 and 13.7 μg/kg, respectively. The recoveries of the analytes spiked in four infant milk powders ranged from 92.2% to 103.2% and the relative standard deviations were lower than 6%. This method is sensitive, simple, and suitable for the determination of triazine herbicides in milk powder samples.

  7. Final Technical Report: SISGR: The Influence of Electrolyte Structure and Electrode Morphology on the Performance of Ionic-Liquid Based Supercapacitors: A Combined Experimental and Simulation Study

    Energy Technology Data Exchange (ETDEWEB)

    Bedrov, Dmitry [University of Utah

    2013-08-15

    Obtaining fundamental understanding and developing predictive modeling capabilities of electrochemical interfaces can significantly shorten the development cycles of electrical double layer capacitors (EDLCs). A notable improvement in EDLC performance has been achieved due to recent advances in understanding charge storage mechanisms, development of advanced nanostructured electrodes and electrochemically stable electrolytes. The development of new generation of EDLCs is intimately linked to that of nanostructured carbon materials which have large surface area, good adsorption/desorption properties, good electrical conductivity and are relatively inexpensive. To address these scientific challenges the efforts of an interdisciplinary team of modelers and experimentalists were combined to enhance our understanding of molecular level mechanisms controlling the performance of EDLCs comprised of room temperature ionic liquid (RTIL) electrolytes and nanostructured carbon-based electrodes and to utilize these knowledge in the design of a new generation of materials and devices for this energy storage application. Specifically our team efforts included: atomistic molecular dynamics simulations, materials science and electrode/device assembly, and synthesis and characterization of RTIL electrolytes.

  8. 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.

  9. 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).

  10. Ultrasound assisted enzymatic depolymerization of aqueous guar gum solution.

    Science.gov (United States)

    Prajapat, Amrutlal L; Subhedar, Preeti B; Gogate, Parag R

    2016-03-01

    The present work investigates the effectiveness of application of low intensity ultrasonic irradiation for the intensification of enzymatic depolymerization of aqueous guar gum solution. The extent of depolymerization of guar gum has been analyzed in terms of intrinsic viscosity reduction. The effect of ultrasonic irradiation on the kinetic and thermodynamic parameters related to the enzyme activity as well as the intrinsic viscosity reduction of guar gum using enzymatic approach has been evaluated. The kinetic rate constant has been found to increase with an increase in the temperature and cellulase loading. It has been observed that application of ultrasound not only enhances the extent of depolymerization but also reduces the time of depolymerization as compared to conventional enzymatic degradation technique. In the presence of cellulase enzyme, the maximum extent of depolymerization of guar gum has been observed at 60 W of ultrasonic rated power and ultrasonic treatment time of 30 min. The effect of ultrasound on the kinetic and thermodynamic parameters as well as the molecular structure of cellulase enzyme was evaluated with the help of the chemical reaction kinetics model and fluorescence spectroscopy. Application of ultrasound resulted in a reduction in the thermodynamic parameters of activation energy (Ea), enthalpy (ΔH), entropy (ΔS) and free energy (ΔG) by 47%, 50%, 65% and 1.97%, respectively. The changes in the chemical structure of guar gum treated using ultrasound assisted enzymatic approach in comparison to the native guar gum were also characterized by FTIR. The results revealed that enzymatic depolymerization of guar gum resulted in a polysaccharide with low degree of polymerization, viscosity and consistency index without any change in the core chemical structure which could make it useful for incorporation in food products.

  11. Ultrasound assisted extraction of lycopene from tomato processing wastes.

    Science.gov (United States)

    Kumcuoglu, Seher; Yilmaz, Tuncay; Tavman, Sebnem

    2014-12-01

    Tomato paste processing wastes, an important by-product of the paste industry, is rich in potentially health-promoting compounds such as lycopene. In this study, extraction yield of lycopene from tomato paste processing wastes by application of ultrasound assisted extraction (UAE) was compared with conventional organic solvent extraction (COSE) method. BHT (butylated hydroxytoluene) 0.05 % (w/v) added hexane:acetone:ethanol (2:1:1) mixture was used as solvent. Three different solvent solid ratios; 50:1, 35:1 and 20:1, (v/w) were used in both COSE and UAE. COSE experiments were performed at 20 °C, 40 °C and 60 °C for 10, 20, 30 and 40 min. 50, 65 and 90 W of ultrasonic power were applied in UAE for 1, 2, 5, 10, 15, 20 and 30 min. Lycopene contents of the samples were determined by spectrophotometric method. The effects of different factors, including the temperature, solvent solid ratio and ultrasonic power on lycopene yield were investigated. It was determined that the most efficient application for COSE was extracting samples by 50:1 solvent solid ratio at 60 °C for 40 min run, for UAE, 35:1 (v/w) solvent solid ratio, 90 W ultrasonic power for 30 min run. It was showed that UAE of lycopene requires less time, lower temperature and lower solvent than COSE.

  12. 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.

  13. 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.

  14. 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.

  15. Ionic liquid based model catalysis: interaction of [BMIM][Tf2N] with Pd nanoparticles supported on an ordered alumina film.

    Science.gov (United States)

    Sobota, Marek; Schmid, Martin; Happel, Markus; Amende, Max; Maier, Florian; Steinrück, Hans-Peter; Paape, Natalia; Wasserscheid, Peter; Laurin, Mathias; Gottfried, J Michael; Libuda, Jörg

    2010-09-21

    Towards a better understanding of novel catalytic materials consisting of supported noble metal catalysts modified by an ionic liquid (IL) film, we have performed a study under ultrahigh-vacuum (UHV) conditions. The model surface consists of Pd nanoparticles grown in UHV on an ordered alumina film on NiAl(110). Thin films of the room temperature IL 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide [BMIM][Tf(2)N] are deposited onto this surface by means of physical vapor deposition (PVD). The interaction of the IL with clean and CO-covered Pd/Al(2)O(3)/NiAl(110) at 300 K and the thermal behavior of the deposited IL films on Pd/Al(2)O(3)/NiAl(110) are investigated by time-resolved infrared reflection absorption spectroscopy (TR-IRAS) and X-ray photoelectron spectroscopy (XPS). At 300 K, the IL adsorbs molecularly both onto the Pd particles and onto the alumina. The IR spectra suggest that the [Tf(2)N](-) anions interact with Pd sites preferentially via the sulfonyl groups. CO pre-adsorbed on the Pd particles is partially displaced by the IL, even at 300 K, and only the part of CO adsorbed onto hollow sites on (111) facets of the Pd particles remains in place. Upon heating to temperatures higher than the desorption temperature of the IL (>400 K), molecular desorption of the IL competes with decomposition. The decomposition products, atomic species and small fragments, remain preferentially adsorbed onto the Pd nanoparticles and strongly modify their surface properties. Most of the decomposition products originate from the [BMIM](+) cations, whereas the [Tf(2)N](-) anions desorb for the most part.

  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.

  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 (C8Gu-Cl) was designed and synthetized with the purpose of obtaining a less harmful surfactant: containing guanidinium as core cation and a relatively short alkyl chain. Its interfacial and aggregation behavior was evaluated through conductivity and fluorescence measurements, presenting a critical micelle concentration value of 42.5 and 44.6mmolL(-1), respectively. Cytotoxicity studies were carried out with C8Gu-Cl and other IL-based and conventional surfactants, specifically the analogue 1-octyl-3-methylimidazolium chloride (C8MIm-Cl), and other imidazolium- (C16MIm-Br) and pyridinium- (C16Py-Cl) based surfactants, together with the conventional cationic CTAB and the conventional anionic SDS. From these studies, C8Gu-Cl was the only one to achieve the classification of low cytotoxicity. An in situ dispersive liquid-liquid microextraction (DLLME) method based on transforming the water-soluble C8Gu-Cl IL-based surfactant into a water-insoluble IL microdroplet via a simple metathesis reaction was then selected as the extraction/preconcentration method for a group of 6 personal care products (PCPs) present in cosmetic samples. The method was carried out in combination with high-performance liquid chromatography (HPLC) and diode array detection (DAD). The method was properly optimized, requiring the use of only 30μL of C8Gu-Cl for 10mL of aqueous sample with a NaCl content of 8% (w/v) to adjust the ionic strength and pH value of 5. The metathesis reaction required the addition of the anion exchange reagent (bis[(trifluoromethyl)sulfonyl]imide - 1:1 molar ratio), followed by vortex and centrifugation, and dilution of the final microdroplet up to 60μL with acetonitrile before the injection in the HPLC-DAD system. The optimum in situ DLLME-HPLC-DAD method takes ∼10min for the extraction step and ∼22min for the chromatographic separation, with analytical features of low detection limits: down to 0.4μgL(-1); high

  18. Hybrid flow analyzer for automatic hollow-fiber-assisted ionic liquid-based liquid-phase microextraction with in-line membrane regeneration.

    Science.gov (United States)

    Nitiyanontakit, Sira; Varanusupakul, Pakorn; Miró, Manuel

    2013-04-01

    The proof-of-concept of a new methodology for in-line hollow-fiber (HF)-assisted three-phase liquid-phase microextraction (LPME) allowing for handling of the feed and acceptor aqueous solutions and of minute volumes of the organic extracting phase in a programmable flow mode is reported in this paper. The flow analyzer fosters in-line anchoring of ionic-liquid-laden extracting solution (10 % (v/v) methyltrioctyl ammonium chloride in kerosene) in the pores of a single-strand microporous polypropylene HF, and regeneration of the liquid-phase membrane itself for each individual analysis cycle in a fully automated mode. Using hexavalent chromium as a model analyte and 1,5-diphenylcarbazide as a chromogenic probe in the acceptor solution, the flow-based HF-LPME hyphenated system was harnessed to the clean-up of troublesome samples (viz., domestic wastewater and soil leachates) with concomitant enrichment of target species. Distinct extraction modes and chemistries were assessed for enhanced Cr(VI) permeability. A single sample plug was subjected to a twofold backward-forward flow extraction so as to decrease the thickness of the boundary layer at the HF shell side for improved extraction efficiency. Under the optimized physicochemical variables, a limit of detection of 4.6 μg L(-1) Cr(VI), a dynamic linear range of up to 500 μg L(-1) and intermediate precision better than 10 % were obtained for a sample volume of 2.8 mL buffered at pH 4 and a volume of organic extractant of 120 μL, with an enrichment factor of ca. 11 for a sample residence time in the donor compartment of merely 4.5 min. Analyte recoveries in domestic wastewaters were ≥83 % using external calibration with relative standard deviations better than 14 %, thereby demonstrating the expedient clean-up of samples with elevated content of dissolved organic carbon. The automatic HF-LPME method was validated in terms of bias against the SRM 2701 (NIST soil) preceded by the EPA alkaline digestion method 3060A

  19. Efficient anti-Prelog enantioselective reduction of acetyltrimethylsilane to (R-1-trimethylsilylethanol by immobilized Candida parapsilosis CCTCC M203011 cells in ionic liquid-based biphasic systems

    Directory of Open Access Journals (Sweden)

    Zhang Bo-Bo

    2012-08-01

    Full Text Available Abstract Background Biocatalytic asymmetric reductions with whole cells can offer high enantioselectivity, environmentally benign processes and energy-effective operations and thus are of great interest. The application of whole cell-mediated bioreduction is often restricted if substrate and product have low water solubility and/or high toxicity to the biocatalyst. Many studies have shown that a biphasic system is often useful in this instance. Hence, we developed efficient biphasic reaction systems with biocompatible water-immiscible ionic liquids (ILs, to improve the biocatalytic anti-Prelog enantioselective reduction of acetyltrimethylsilane (ATMS to (R-1-trimethylsilylethanol {(R-1-TMSE}, which is key synthon for a large number of silicon-containing drugs, using immobilized Candida parapsilosis CCTCC M203011 cells as the biocatalyst. Results It was found that the substrate ATMS and the product 1-TMSE exerted pronounced toxicity to immobilized Candida parapsilosis CCTCC M203011 cells. The biocompatible water-immiscible ILs can be applied as a substrate reservoir and in situ extractant for the product, thus greatly enhancing the efficiency of the biocatalytic process and the operational stability of the cells as compared to the IL-free aqueous system. Various ILs exerted significant but different effects on the bioreduction and the performances of biocatalysts were closely related to the kinds and combination of cation and anion of ILs. Among all the water-immiscible ILs investigated, the best results were observed in 1-butyl-3-methylimidazolium hexafluorophosphate (C4mim·PF6/buffer biphasic system. Furthermore, it was shown that the optimum substrate concentration, volume ratio of buffer to IL, buffer pH, reaction temperature and shaking rate for the bioreduction were 120 mM, 8/1 (v/v, 6.0, 30°C and 180 r/min, respectively. Under these optimized conditions, the initial reaction rate, the maximum yield and the product e.e. were 8.1

  20. Ultrasound assisted extraction of food and natural products. Mechanisms, techniques, combinations, protocols and applications. A review.

    Science.gov (United States)

    Chemat, Farid; Rombaut, Natacha; Sicaire, Anne-Gaëlle; Meullemiestre, Alice; Fabiano-Tixier, Anne-Sylvie; Abert-Vian, Maryline

    2017-01-01

    This review presents a complete picture of current knowledge on ultrasound-assisted extraction (UAE) in food ingredients and products, nutraceutics, cosmetic, pharmaceutical and bioenergy applications. It provides the necessary theoretical background and some details about extraction by ultrasound, the techniques and their combinations, the mechanisms (fragmentation, erosion, capillarity, detexturation, and sonoporation), applications from laboratory to industry, security, and environmental impacts. In addition, the ultrasound extraction procedures and the important parameters influencing its performance are also included, together with the advantages and the drawbacks of each UAE techniques. Ultrasound-assisted extraction is a research topic, which affects several fields of modern plant-based chemistry. All the reported applications have shown that ultrasound-assisted extraction is a green and economically viable alternative to conventional techniques for food and natural products. The main benefits are decrease of extraction and processing time, the amount of energy and solvents used, unit operations, and CO2 emissions.

  1. Ultrasound-assisted synthesis and processing of carbon materials

    Science.gov (United States)

    Fortunato, Maria E.

    2011-12-01

    -liquid slurries, surface erosion and particle fracture occur due to the shockwaves and microjets formed from asymmetric bubble collapse at extended surfaces. The chemical and physical effects of ultrasound have been studied as an adjunct to the traditional chemical pretreatment of lignocellulosic biomass for ethanol production. Lignocellulosic biomass consists of cellulose, hemicellulose, and lignin. The surface effects of ultrasound were used in this work to increase the accessibility of the cellulose, which can be converted to glucose and then fermented into ethanol. The lignocellulosic biomass used in this work was Miscanthus x giganteus (Mxg) which was grown at the University of Illinois at Urbana-Champaign. The chemical effects of NaOH pretreatment on Mxg were enhanced by ultrasound: greater delignification and a significant increase in the amount of pores >5 nm were observed. ˜ 70% of the theoretical glucose yield was obtained by enzymatic saccharification of the ultrasound-assisted NaOH-pretreated Mxg; this is comparable to the yields that can be obtained by traditional alkaline pretreatments, but it was achieved in a shorter time and at a lower temperature. Because the apparatus used for laboratory studies is not a likely device for scale-up, the economics of ultrasound with regards to energy balance are not yet resolved.

  2. 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.

  3. 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…

  4. 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…

  5. Simultaneous determination of acrylamide, asparagine and glucose in food using short chain methyl imidazolium ionic liquid based ultrasonic assisted extraction coupled with analyte focusing by ionic liquid micelle collapse capillary electrophoresis.

    Science.gov (United States)

    Abd El-Hady, Deia; Albishri, Hassan M

    2015-12-01

    Acrylamide (AA) is a known lethal neurotoxin and carcinogen. AA is formed in foods during the browning process by the Maillard reaction of glucose (GL) with asparagine (AS). For the first time, the simultaneous online preconcentration and separation of AA, AS and GL using analyte focusing by ionic liquid micelle collapse capillary electrophoresis (AFILMC) was presented. Samples were prepared in a 1-butyl-3-methylimidazolium bromide (BMIMBr) micellar matrix with a conductivity 4 times greater than that of the running buffer (12.5 mmol L(-1) phosphate buffer at pH 8.5). Samples were hydrodynamically injected into a fused silica capillary at 25.0 mbar for 25.0 s. Separations were performed by applying a voltage of 25.0 kV and a detection at 200.0 nm. To sufficiently reduce BMIMBr adsorption on the interior surface of capillary, an appropriate rinsing procedure by hydrochloric acid and water was optimized. AFILMC measurements of analytes within the concentration range of 0.05-10.0 μmol L(-1) achieved adequate reproducibility and accuracy with RSD 1.14-3.42% (n=15) and recovery 98.0-110.0%, respectively. Limits of detections were 0.71 ng g(-1) AA, 1.06 ng g(-1) AS and 27.02 ng g(-1) GL with linearity ranged between 2.2 and 1800 ng g(-1). The coupling of AFILMC with IL based ultrasonic assisted extraction (ILUAE) was successfully applied to the efficient extraction and determination of AA, AS and GL in bread samples. The structure of ILs has significant effects on the extraction efficiency of analytes. The optimal extraction efficiency (97.8%) was achieved by an aqueous extraction with 4:14 ratio of sample: 3.0 mol L(-1) BMIMBr followed by sonication at 35 °C. The proposed combination of ILUAE and AFILMC was simple, ecofriendly, reliable and inexpensive to analyze a toxic compound and its precursors in bread which is applicable to food safety.

  6. Structure formation and properties of a copper-aluminum joint produced by ultrasound-assisted explosive welding

    Science.gov (United States)

    Kuz'min, E. V.; Peev, A. P.; Kuz'min, S. V.; Lysak, V. I.

    2017-08-01

    The effect of ultrasound-assisted explosive welding on the structure formation and the properties of copper-aluminum joints is studied. Ultrasound-assisted explosive welding improves the quality of formed copper-aluminum joints, i.e., enhances their strength and significantly reduces the amount of fused metal over the entire weldability range. It is shown that ultrasound-assisted explosive welding can noticeably extend the weldability range of the copper-aluminum pair to obtain equal-in-strength joints with minimum structural heterogeneity in the wide welding range.

  7. Ultrasound-assisted lipoplasty treatment for axillary bromidrosis: clinical experience of 375 cases.

    Science.gov (United States)

    Hong, Joon Pio; Shin, Hyun Woo; Yoo, Sung-Chul; Chang, Hak; Park, Sang Hoon; Koh, Kyung Suck; Hur, Jae Young; Lee, Taik Jong

    2004-04-01

    Bromidrosis is a condition of abnormal offensive body odor caused mostly by apocrine gland secretion from the axilla. Although no morbid sequelae are known, the odor can be disturbing enough to cause social impairment and psychological distress. Medical care is available but is temporary and yields limited clinical benefit. Surgical treatment may provide a more definite remedy through reduction of the apocrine gland. However, there are risks for complication following surgical treatment such as subdermal excision, subcutaneous shaving, en bloc excision, and liposuction. The search for a less invasive but still effective procedure has led the authors to use ultrasound-assisted liposuction, which has reduced the risk of complication and recurrence. The purpose of this article was to evaluate the long-term outcome of ultrasound-assisted liposuction for the treatment of bromidrosis. From August 1998 to September 2002, 375 consecutive patients underwent ultrasound-assisted liposuction for bromidrosis of the axilla. The average age of the patients was 25.7 years (range, 15 to 55 years) and the average follow-up period was 18.8 months (range, 7 to 56 months). Subjective complaints of recurrences were noted in 22 patients (5.9 percent) and secondary ultrasound-assisted liposuction was performed, resulting in no further complaints. Complications other than recurrences were mild skin sloughing (3.2 percent), hematoma (1.3 percent), subcutaneous band (0.3 percent), and hypesthesia of the hand (0.3 percent), all of which healed spontaneously. Through a questionnaire that was answered by 264 patients, a subjective satisfaction rate was measured. Among the completed questionnaires, 91.7 percent reported satisfactory reduction of odor. Ultrasound-assisted liposuction to treat bromidrosis of the axilla provides advantages such as rapid recovery, less restriction of movement, unnoticeable scars, and a low rate of recurrence. The long-term outcome supports the benefits of this

  8. 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.

  9. Surgical treatment of multiple symmetric lipomatosis with ultrasound-assisted liposuction.

    Science.gov (United States)

    Bassetto, Franco; Scarpa, Carlotta; De Stefano, Fabio; Busetto, Luca

    2014-11-01

    Multiple symmetric lipomatosis (MSL) is a rare disease of unknown etiology, characterized by the presence of multiple, symmetrical, noncapsulated lipomas, mostly in the neck and upper trunk. To date, there is no effective medical treatment of MSL. Surgical treatment is based on 2 options, namely, lipectomy and/or liposuction. In this retrospective study, we compare traditional lipectomy with ultrasound-assisted liposuction. Our initial experience demonstrates that the ultrasound-assisted liposuction procedure can be applied to patients with MSL, allowing simultaneous treatment of multiple areas in a single session and the removal of a substantial amount of fat, thus improving aesthetic results. If lipomas are circumscribed and isolated, traditional lipectomy is probably to be preferred.

  10. 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.

  11. Drying characteristics of ultrasound assisted hot air drying of Flos Lonicerae

    OpenAIRE

    LIU, YUNHONG; Sun, Yue; Miao, Shuai; Li, Fang; Luo, Denglin

    2014-01-01

    Ultrasound assisted hot air drying of Flos Lonicerae was investigated in this study. The effects of drying parameters such as ultrasonic radiation distance, ultrasonic power and drying temperature on drying characteristics were discussed. The results showed that ultrasound application has positive and significant effects on hot air drying. Shortening ultrasonic radiation distance is beneficial to improve both ultrasonic energy efficiency and drying rate. Higher ultrasonic power had more posit...

  12. Ultrasound-Assisted Extraction of Antioxidants in Misai Kucing (Orthosiphon stamineus)

    OpenAIRE

    2014-01-01

    Ultrasound-assisted extraction (UAE) with ethanol was used to extract the compounds responsible for the antioxidant activities of Misai Kucing (Orthosiphon stamineus). Response surface methodology (RSM) was used to optimize four independent variables: ethanol concentration (%), amplitude (%), duty cycle (W/s) and extraction time (min). Antioxidant compounds were determined by total phenolic content and total flavonoid content to be 1.4 g gallic acid equivalent/100 g DW and 45 g catechin equiv...

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

    OpenAIRE

    Ling-Li Zheng; Guan Wen; Min-Yong Yuan; Feng Gao

    2016-01-01

    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 we...

  14. Enhanced decomposition of reactive blue 19 dye in ultrasound assisted electrochemical reactor.

    Science.gov (United States)

    Siddique, Maria; Farooq, Robina; Khan, Zahid Mehmood; Khan, Zarsher; Shaukat, S F

    2011-01-01

    Textile industry effluents contain reactive dyes that may harm our receiving waters. A typical reactive blue (RB) 19 dye is frequently detected in significant concentrations in textile industry effluents. Such dyes have generally shown resistance to decomposition and tend to persist in the environment for long periods and multiply the impacts to water and environment. Therefore, the present investigation focused on high-rate decomposition of a typical reactive dye RB 19 under various ultrasound and electrochemical process conditions. The decomposition of un-hydrolyzed and hydrolyzed forms of reactive blue (RB) 19 dye by ultrasound assisted electrochemical process was investigated using various parameters including dye concentration, pH, ultrasonic frequency and reaction time. Reaction kinetics, organic carbon and mechanism for dye decomposition were determined using UV-Visible spectrophotometry, TOC (total organic carbon) analysis and gas chromatography-mass spectrometry (GC-MS). Almost complete 90% color removal and a maximum of 56% TOC removal for 50 mg L(-1) dye concentration of un-hydrolyzed RB 19 dye was achieved at an ultrasonic frequency of 80 kHz, pH of 8 after 120 min. GC-MS analysis showed that a sonoelectrochemical treatment of un-hydrolyzed RB 19 dye for 30 min resulted in the formation of products e.g. acetic acid, benzoic acid etc. with the complete removal of dye. For hydrolyzed dye, a treatment of 10 min was enough and the results were comparable with 30 min treatment of un-hydrolyzed dye. Kinetics of ultrasound assisted electrolysis showed that the dye decomposition followed 1st order. The ultrasound assisted electrolysis for dye decomposition and hence decolorization proved to be more effective and the total energy consumption reduced to half as compared with simple electrolysis/sonochemical decomposition. Therefore, ultrasound assisted electrolysis was found to be more effective technique for dye decomposition of an otherwise environmentally

  15. Antioxidant Capacity of Rapeseed Extracts Obtained by Conventional and Ultrasound-Assisted Extraction

    OpenAIRE

    2014-01-01

    Ultrasound-assisted extraction (UAE) and conventional solid–liquid extraction were applied to extract total antioxidants from two rapeseed varieties. The antioxidant capacities (AC) of winter and spring rapeseed cultivars were determined by four different analytical methods: ferric reducing antioxidant power (FRAP), cupric reducing antioxidant capacity (CUPRAC), 2,2′-diphenyl-1-picrylhydrazyl (DPPH), 2,2′-azino-bis-3-ethylbenzothiazoline-6-sulfonic acid (ABTS). The average AC of the studied r...

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

    OpenAIRE

    Javed Ahamad; Saima Amin; Showkat R. Mir

    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-leve...

  17. Comparison of Conventional and Ultrasound-assisted Extraction Techniques on Mass Fraction of Phenolic Compounds from Sage (Salvia officinalis L.)

    OpenAIRE

    2015-01-01

    An innovative ultrasound-assisted extraction (UAE) is the rapid non-thermal extraction technique, which in comparison to conventional extraction (CE), offers high reproducibility in a short time with simplified manipulation, reduced solvent consumption and lower energy. Optimization of ultrasonic conditions was conducted for devices with nominal output power of 100 and 400 W, including the influence of geometrical parameters of probes regarding ultrasound-assisted extraction. The results show...

  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.

  19. Ultrasound assisted extraction in quantifying lutein from chicken liver using high-performance liquid chromatography.

    Science.gov (United States)

    Sun, Ting; Xu, Zhimin; Godber, J Samuel

    2006-01-01

    Four sample preparation methods, (1) solvent (SOL), (2) saponification and solvent (SP), (3) ultrasound assisted solvent (UA), and (4) saponification and ultrasound assisted solvent (SP-UA), were used for quantifying lutein in chicken liver samples by HPLC. The lutein concentrations obtained by using SOL, UA, SP, and SP-UA were significantly different with values from 10.4 microg/g (UA) to undetected (SOL). Efficiency of the four different methods for extracting lutein from high to low were the UA, SP, SP-UA, and SOL method. The measured value of lutein in the liver sample using the UA method was approximately two and three times higher than that obtained from the SP and SP-UA method, respectively. The methods with saponification significantly affected the stabilities of lutein in liver samples. The lutein concentration measured with the solvent only method was either much lower than any of the other extraction methods or undetectable. This indicated that little lutein in those samples was in a form that could be extracted directly by solvent. Compared with the saponification method, the ultrasound assisted solvent method could effectively extract lutein from sample matrix and thus avoid chemical degradation reactions, which would be especially important for complex biological tissue such as liver.

  20. Improved sensitivity gas chromatography-mass spectrometry determination of parabens in waters using ionic liquids.

    Science.gov (United States)

    Cacho, Juan Ignacio; Campillo, Natalia; Viñas, Pilar; Hernández-Córdoba, Manuel

    2016-01-01

    A new procedure for the introduction of ionic liquid samples in gas chromatography (GC) is proposed. This procedure, based on microvial insert thermal desorption, allows the direct analysis of the compounds preconcentrated by ionic liquid based liquid-liquid microextraction (IL-LLME) using the combination of a thermal desorption unit (TDU) and a programmed temperature vaporization injector (PTV). Two different IL-LLME methodologies, one based on the formation of a microdroplet emulsion by dispersive liquid-liquid microextraction (DLLME) and other through ultrasound-assisted emulsification microextraction (USAEME) were studied and evaluated. IL-DLLME proved advantageous and consequently, it was adopted for preconcentration purposes. This easy to apply approach was used for the determination of five parabens (methyl-, ethyl-, propyl-, butyl- and isobutyl paraben) in swimming pool waters, after in situ acetylation. The optimized conditions of TDU/PTV allowed the analytes contained in 20 µL of the enriched IL to be transferred to the capillary column. Quantification of the samples was carried out against aqueous standards, and quantification limits of between 4.3 and 8.1 ng L(-1) were obtained, depending on the compound. Concentrations of between 9 and 47 ng L(-1) for some analytes were obtained in the analysis of ten samples.

  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. OPTIMIZATION OF ULTRASOUND-ASSISTED EXTRACTION CONDITIONS OF FLAVONOIDS FROM TARTARY BUCKWHEAT

    Directory of Open Access Journals (Sweden)

    Zhang Zhong

    2012-12-01

    Full Text Available The objective of this study was to establish the optimum ultrasound-assisted extraction (UAE conditions for flavonoids from tartary buckwheat (FTB. Single factor experiments were performed to determine the appropriate range of extraction conditions and orthogonal experiment were performed to obtain the optimum extraction conditions. The results showed that the optimum UAE conditions for FTB were as followings: ethanol concentration of 65%, solid:liquid ratio of 1:40 g/ml, extraction time of 35 min and extraction temperature of 65 °C. UAE method is an alternative extraction technique for fast extraction of FTB.

  3. Determination of selected polychlorinated biphenyls in water samples by ultrasound-assisted emulsification-microextraction and gas chromatography-mass-selective detection.

    Science.gov (United States)

    Ozcan, Senar; Tor, Ali; Aydin, Mehmet Emin

    2009-08-11

    Ultrasound-assisted emulsification-microextraction (USAEME) procedure was developed for the determination of selected polychlorinated biphenyls (PCBs) in 10 mL of water samples by gas chromatography-mass-selective detection. After determination of the most suitable solvent and extraction time, several other parameters including solvent volume, centrifugation time and ionic strength of the sample were optimized using a 2(3) factorial experimental design. The optimized USAEME procedure used 200 microL of chloroform as extraction solvent, 10 min of extraction with no ionic strength adjustment at 25 degrees C and 5 min of centrifugation at 4000 rpm. The limits of detection ranged from 14 ngL(-1) (for PCB153) to 30 ngL(-1) (for PCB101). Recoveries of PCBs from fortified distilled water are over 80% for three different fortification levels between 0.1 and 5 microgL(-1) and relative standard deviations of the recoveries are below 10%. The performance of the proposed method was compared with those involving traditional liquid-liquid extraction (LLE) and solid phase extraction (SPE) on the real water samples (i.e., tap and well water as well as domestic and industrial wastewaters, etc.) and comparable efficiencies were obtained. The proposed USAEME procedure has been demonstrated to be viable, simple, rapid and easy to use for residue analysis of PCBs in water samples.

  4. Optimization of ultrasound-assisted extraction of bioactive compounds from wild garlic (Allium ursinum L.).

    Science.gov (United States)

    Tomšik, Alena; Pavlić, Branimir; Vladić, Jelena; Ramić, Milica; Brindza, Ján; Vidović, Senka

    2016-03-01

    Ultrasound-assisted extraction was used for extraction of bioactive compounds and for production of Allium ursinum liquid extract. The experiments were carried out according to tree level, four variables, face-centered cubic experimental design (FDC) combined with response surface methodology (RSM). Temperature (from 40 to 80 °C), ethanol concentration (from 30% to 70%), extraction time (from 40 to 80 min) and ultrasonic power (from 19.2 to 38.4 W/L) were investigated as independent variables in order to obtain the optimal conditions for extraction and to maximize the yield of total phenols (TP), flavonoids (TF) and antioxidant activity of obtained extracts. Experimental results were fitted to the second order polynomial model where multiple regression and analysis of variance were used to determine the fitness of the model and optimal condition for investigated responses. The predicted values of the TP (1.60 g GAE/100 g DW), TF (0.35 g CE/100 g DW), antioxidant activity, IC50 (0.71 mg/ml) and EY (38.1%) were determined at the optimal conditions for ultrasound assisted extraction: 80 °C temperature, 70% ethanol, 79.8 min and 20.06 W/L ultrasonic power. The predicted results matched well with the experimental results obtained using optimal extraction conditions which validated the RSM model with a good correlation.

  5. Ultrasound-assisted extraction of phenolic compounds from Laurus nobilis L. and their antioxidant activity.

    Science.gov (United States)

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

    2013-09-01

    Bay leaves (BL) (Laurus nobilis L., Family: Laureceae) are traditionally used to treat some symptoms of gastrointestinal problems, such as epigastric bloating, impaired digestion, eructing and flatulence. These biological properties are mainly attributed to its phenolic compounds. In this paper, ultrasound-assisted extraction of phenolic compounds from Laurus nobilis L. (Laureceae) was studied. Effects of several experimental factors, such as sonication time, solid/liquid ratio and concentration of solvent on extraction of phenolic compounds were evaluated through a randomized complete block design with factorial treatment arrangement (3(3)). The best extraction conditions were: 1g plant sample with 12 mL of 35% ethanol, for 40 min, obtaining a yield of phenolic compounds of 17.32±1.52 mg g(-1) of plant. In addition, free radical-scavenging potential of DPPH and lipid oxidation inhibition, by linoleic acid peroxidation of the selected extract was measured in order to evidence their antioxidant properties. Results indicated that high amounts of phenolic compounds can be extracted from L. nobilis by ultrasound-assisted extraction technology.

  6. Ultrasound-assisted extraction of D-pinitol from carob pods using Response Surface Methodology.

    Science.gov (United States)

    Tetik, Nedim; Yüksel, Esra

    2014-03-01

    This study reports on the optimization of the conditions of extraction of D-pinitol compound from carob pods by using ultrasonication. For this purpose, the Box-Behnken design, which is a widely used form of Response Surface Methodology, was used to investigate the effects of parameters on the ultrasound-assisted extraction. Four independent variables, temperature (°C), ultrasonic power (W), dilution rate (material:water ratio) and time (min), were studied. The results showed that the highest D-pinitol concentration of 11.98 g/L was obtained with an extraction temperature of 50 °C, ultrasonic power of 207 W, a dilution rate of 1:4 and an extraction time of 120 min. It was found that the D-pinitol concentration of carob extract increased with the effect of ultrasonication during the extraction process. Therefore, ultrasound-assisted extraction could be used as an alternative to conventional hot water extraction with respect to the recovery of D-pinitol from carob pods with the advantages of lower extraction temperatures, shorter extraction time and reduced energy consumption.

  7. 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.

  8. Process optimization of ultrasound-assisted curcumin nanoemulsions stabilized by OSA-modified starch.

    Science.gov (United States)

    Abbas, Shabbar; Bashari, Mohanad; Akhtar, Waseem; Li, Wei Wei; Zhang, Xiaoming

    2014-07-01

    This study reports on the process optimization of ultrasound-assisted, food-grade oil-water nanoemulsions stabilized by modified starches. In this work, effects of major emulsification process variables including applied power in terms of power density and sonication time, and formulation parameters, that is, surfactant type and concentration, bioactive concentration and dispersed-phase volume fraction were investigated on the mean droplet diameter, polydispersity index and charge on the emulsion droplets. Emulsifying properties of octenyl succinic anhydride modified starches, that is, Purity Gum 2000, Hi-Cap 100 and Purity Gum Ultra, and the size stability of corresponding emulsion droplets during the 1 month storage period were also investigated. Results revealed that the smallest and more stable nanoemulsion droplets were obtained when coarse emulsions treated at 40% of applied power (power density: 1.36 W/mL) for 7 min, stabilized by 1.5% (w/v) Purity Gum Ultra. Optimum volume fraction of oil (medium chain triglycerides) and the concentration of bioactive compound (curcumin) dispersed were 0.05 and 6 mg/mL oil, respectively. These results indicated that the ultrasound-assisted emulsification could be successfully used for the preparation of starch-stabilized nanoemulsions at lower temperatures (40-45 °C) and reduced energy consumption.

  9. 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.

  10. [Ultrasound assisted the enzymolysis of ginsenosides to prepare pare ginseng saponin Compound K].

    Science.gov (United States)

    Yu, Zhao-Hui; Liu, Qi-Yuan; Cui, Li; Jia, Xiao-Bin; Jin, Xin; Zhang, Zhen-Hai

    2014-08-01

    To prepare ginseng saponin Compound K with ultrasound-assisted total zymolytic ginseng saponins. The conversion rate was taken as the index to detect the pre-treatment factors such as ultrasonic power and ultrasonic time, as well as the impact of enzymatic factors, such as pH value, temperature, concentration of substrate, dosage of enzyme and reaction time, on the conversion rate. The response surface method was used to optimize the preparation conditions. The enzymolytic products were identified with MS, 1H-NMR and 13C-NMR. The results showed that the optimum conditions of the ultrasound-assisted enzymolysis were 250 W for ultrasonic power, 15 min for ultrasonic time, 5.5 for enzymolytic pH, 50 degrees C for enzymolytic temperature, 36 h for enzymolytic time, 4:5 for enzymolytic dosage: substrate and 1.0 g x L(-1) for concentration of substrate. The relative molecular mass of reaction products was 622.4. Therefore, the nuclear magnetic map verified that the reaction product was rare ginseng saponin Compound K. Under the above conditions, based on the total zymolytic ginseng saponins, the conversion rate of rare ginseng saponin Compound K was 6.91% in proportion to the total of ginsenosides. The process features gentle reaction conditions, high conversion rate and simple and reliable process, which is suitable for industrial production.

  11. Ultrasound-assisted extraction of volatile compounds from industrial Cannabis sativa L. inflorescences

    Directory of Open Access Journals (Sweden)

    C. Da Porto

    2014-02-01

    Full Text Available Summary. This study investigated the use of ultrasound-assisted extraction (UAE to recovery  volatile compounds from the inflorescences of a fiber type Cannabis sativa L. cultivar. The results show that ultrasonic treatment not longer than 5 min allows to obtain an enhanced concentration of terpenes in comparison with maceration. Instead, an ultrasonic treatment longer than 5 min increased  the concentration of δ-9-tetraidrocannabinol (THC. A preliminary screening of cannabis inflorescences scent was performed by headspace solid-phase microextraction (HS-SPME with gas chromatography-mass spectrometry (GC-MS avoiding the chemical modification and artifact formation that can occur in conventional methods . Industrial relevance. Inflorescences of fiber type Cannabis sativa cultivars are generally considered waste parts for fiber industry, although the inflorescences’ volatiles are pleasant to the human sensory system. Cannabis scent originate from volatile monoterpenes and sesquiterpenes . Traditionally, the recovery of floral fragrances from plants is by water distillation (hydro-distillation or steam distillation to produce essential oils. However, these techniques take at least several hours and require the application of heating, which can produce the degradation of thermo labile compounds present in the starting plant material. Ultrasound-assisted extraction can be use as alternative method to extract aroma compounds from inflorescences of fiber type  Cannabis sativa. The extracts so obtained could be used as ingredients for perfumes (cosmetic industry or flavorings for beverages (food industry.Keywords. Ultrasound; Extraction; Cannabis sativa L.; terpenes; THC; HS-SPME

  12. Production of cerium zinc molybdate nano pigment by innovative ultrasound assisted approach.

    Science.gov (United States)

    Patel, M A; Bhanvase, B A; Sonawane, S H

    2013-05-01

    Ultrasound assisted synthesis of yellow rare earth cerium zinc molybdate anticorrosion nanopigment is presented. This new class of pigment is eco-friendly alternatives to lead, cadmium and chromium pigment as these pigments contains carcinogenic species like Cr(6+) which is responsible for human disease. The synthesis of nanosized cerium zinc molybdate was carried out using cerium nitrate, sodium zinc molybdate as a precursor materials by conventional and ultrasound assisted chemical precipitation method without addition of emulsification agent. XRD, FTIR and elemental analysis confirm the formation of cerium zinc molybdate nanoparticles. The conductivity results indicate that conventional synthesis takes longer time, while in sonochemical technique (US), reaction completes within short period of time. Improved solute transfer rate, rapid nucleation, and formation of large number of nuclei are attributed to presence of cavitation. Saturation of the Ce(3+) ions reaches earlier in case of sonochemical technique which restricts the growth of particles hence smaller size is obtained. The crystallite size of cerium zinc molybdate was found to be 27nm from XRD analysis.

  13. Ultrasound-assisted emulsification of cosmetic samples prior to elemental analysis by different atomic spectrometric techniques.

    Science.gov (United States)

    Lavilla, I; Cabaleiro, N; Costas, M; de la Calle, I; Bendicho, C

    2009-11-15

    In this work, ultrasound-assisted emulsification with a probe system is proposed as a rapid and simple sample treatment for atomic spectrometric determinations (Electrothermal Atomic Absorption Spectrometry, Inductively Coupled Plasma Optical Emission Spectrometry, Flame Atomic Absorption Spectrometry and Cold Vapour Atomic Absorption Spectrometry) of trace elements (As, Cd, Cr, Cu, Hg, Mg, Mn, Ni, Sr and Zn) in cosmetic samples such as shampoos, gel (hair gel), crèmes (body milk, hair conditioner) and oil (body oil). The type of dispersion medium, the sample mass-to-dispersion medium volume ratio, as well as the parameters related to the ultrasound-assisted emulsification (sonication amplitude and treatment time) were exhaustively studied. Only 1 min of ultrasonic shaking and a dispersion medium containing 0.5% (w/v) of SDS+3% (v/v) of HNO(3) or HCl allows obtaining a stable emulsion at least for 3 months. Thermal programs, nebulization of emulsions, speed of pumps and concentration of reagents used in cold vapour generation were optimized. Calibration using aqueous standards was feasible in all cases. Calibration by the standard addition method and recovery studies was also applied for validation. Microwave-assisted digestion and Inductively Coupled Plasma Mass Spectrometry were used for comparison purposes. Relative standard deviations from analysis of five independent emulsions were less than 9% in all cases.

  14. Characterization and functional properties of mango peel pectin extracted by ultrasound assisted citric acid.

    Science.gov (United States)

    Wang, Miaomiao; Huang, Bohui; Fan, Chuanhui; Zhao, Kaili; Hu, Hao; Xu, Xiaoyun; Pan, Siyi; Liu, Fengxia

    2016-10-01

    Pectin was extracted from 'Tainong No. 1' mango peels, using a chelating agent-citric acid as extraction medium by ultrasound-assisted extraction (UAE) and conventional extraction (CE) at temperatures of 20 and 80°C. Chemical structures, rheological and emulsifying properties of mango peel pectins (MPPs) were comparatively studied with laboratory grade citrus pectin (CP). All MPPs exhibited higher protein content (4.74%-5.94%), degree of methoxylation (85.43-88.38%), average molecular weight (Mw, 378.4-2858kDa) than the CP, but lower galacuronic acid content (GalA, 52.21-53.35%). CE or UAE at 80°C resulted in significantly higher pectin yield than those at 20°C, while the extraction time for UAE-80°C (15min) was significantly shorter compared to CE-80°C (2h) with comparable pectin yield. Moreover, MPPs extracted at 80°C were observed with higher GalA and protein content, higher Mw, resulting in higher viscosity, better emulsifying capacity and stability, as compared to those extracted at 20°C and the CP. Therefore, these results suggested that MPPs from 'Tainong No. 1' may become a highly promising pectin with good thickening and emulsifying properties, using ultrasound-assisted citric acid as an efficient and eco-friendly extraction method.

  15. 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

  16. Simultaneous determination of 12 pharmaceuticals in water samples by ultrasound-assisted dispersive liquid-liquid microextraction coupled with ultra-high performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Guan, Jin; Zhang, Chi; Wang, Yang; Guo, Yiguang; Huang, Peiting; Zhao, Longshan

    2016-11-01

    A new analytical method was developed for simultaneous determination of 12 pharmaceuticals using ultrasound-assisted dispersive liquid-liquid microextraction (DLLME) followed by ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS). Six nonsteroidal anti-inflammatory drugs (NSAIDs, ketoprofen, mefenamic acid, tolfenamic acid, naproxen, sulindac, and piroxicam) and six antibiotics (tinidazole, cefuroxime axetil, ciprofloxacin, sulfamethoxazole, sulfadiazine, and chloramphenicol) were extracted by ultrasound-assisted DLLME using dichloromethane (800 μL) and methanol/acetonitrile (1:1, v/v, 1200 μL) as the extraction and dispersive solvents, respectively. The factors affecting the extraction efficiency, such as the type and volume of extraction and dispersive solvent, vortex and ultrasonic time, sample pH, and ionic strength, were optimized. The ultrasound-assisted process was applied to accelerate the formation of the fine cloudy solution by using a small volume of dispersive solvent, which increased the extraction efficiency and reduced the equilibrium time. Under the optimal conditions, the calibration curves showed good linearity in the range of 0.04-20 ng mL(-1) (ciprofloxacin and sulfadiazine), 0.2-100 ng mL(-1) (ketoprofen, tinidazole, cefuroxime axetil, naproxen, sulfamethoxazole, and sulindac), and 1-200 ng mL(-1) (mefenamic acid, tolfenamic acid, piroxicam, and chloramphenicol). The LODs and LOQs of the method were in the range of 0.006-0.091 and 0.018-0.281 ng mL(-1), respectively. The relative recoveries of the target analytes were in the range from 76.77 to 99.97 % with RSDs between 1.6 and 8.8 %. The developed method was successfully applied to the extraction and analysis of 12 pharmaceuticals in five kinds of water samples (drinking water, running water, river water, influent and effluent wastewater) with satisfactory results. Graphical Abstract Twelve pharmaceuticals in water samples analyted by UHPLC

  17. ULTRASOUND-ASSISTED EPOXIDATION OF OLEFINS AND A,B-UNSATURATED KETONES OVER HYDROTALCITES USING HYDROGEN PEROXIDE

    Science.gov (United States)

    An efficient ultrasound-assisted epoxidation of olefins and a,B-unsaturated ketones over hydrotacite catalysts in the presence of hydrogen peroxide and acetonitrile is described. This general and selective protocol is relatively fast and is applicable to a wide variety of substra...

  18. 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.

  19. Ultrasound-assisted extraction of ginseng saponins from ginseng roots and cultured ginseng cells.

    Science.gov (United States)

    Wu, J; Lin, L; Chau, F T

    2001-10-01

    Ultrasound-assisted extraction was evaluated as a simpler and more effective alternative to conventional extraction methods for the isolation of ginsenosides (saponins) from various types of ginseng. The ginseng samples were extracted with different solvents, under either direct sonication by an ultrasound probe horn or indirect sonication in an ultrasound cleaning bath. The ultrasonic extraction was compared with the conventional method of refluxing boiling solvents in a soxhlet extractor, on the yields of both the total saponin isolated by thin-layer chromatography and the individual ginsenosides by high performance liquid chromatography. It was found that the sonication-assisted extraction of ginseng saponins was about three times faster than the traditional extraction method. The ultrasonic extraction was not only more efficient but also convenient for the recovery and purification of the active ingredients of plant materials. In addition, the sonication-assisted extraction can be carried out at lower temperatures which are favorable for the thermally unstable compounds.

  20. 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.

  1. 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.

  2. Ultrasound-assisted extraction of bioactive compounds from lemon balm and peppermint leaves

    Science.gov (United States)

    Šic Žlabur, Jana; Voća, Sandra; Dobričević, Nadica; Pliestić, Stjepan; Galić, Ante; Boričević, Ana; Borić, Nataša

    2016-01-01

    The aim of this study was to investigate the influence of conventional and ultrasound-assisted extraction (frequency, time, temperature) on the content of bioactive compounds as well as on the antioxidant activity of aqueous extracts from fresh lemon balm and peppermint leaves. Total phenols, flavonoids, non-flavonoids, total chlorophylls, total carotenoids, and radical scavenging capacity were determined. Moreover, the relationship between bioactive compounds and antioxidant capacity was studied by linear regression. A significant increase in all studied bioactive compounds during ultrasonic extraction for 5 to 20 min was found. With the classical extraction method, the highest amounts of total phenols, flavonoids, and antioxidant activity were determined, and the maximum amounts of total chlorophylls and carotenoids were determined during 20 min ultrasonic extraction. The correlation analysis revealed a strong, positive relationship between antioxidant activity and total phenolic compounds.

  3. Extraction of Angelica sinensis polysaccharides using ultrasound-assisted way and its bioactivity.

    Science.gov (United States)

    Zhao, Ying; Shi, Yongyong; Yang, Huixin; Mao, Lijuan

    2016-07-01

    In the present article, ultrasound-assisted extraction (UAE) of polysaccharides from Angelica sinensis were investigated. The aim of the study is to examine the extraction parameters such as ultrasound power (140-180W), the ratio of liquid to solid (5-7), extraction time (40-50min) and extraction temperature (80-100°C) and to obtain the best possible combinations of these parameters through response surface methodology (RSM). Based on contour plots and variance analysis, optimum operational conditions for maximizing polysaccharides yield were found to be 180w, 7, 45min and 90°C. Under the optimum operating conditions determined, 6.96% polysaccharides were achieved. In addition, the results showed that A. sinensis polysaccharides (ASP) could increase antioxidant enzymes activities and decrease the MDA levels in the skeletal muscle of exhaustive exercise rats. This study provides strong evidence that A. sinensis polysaccharides supplementation possessed protective effects against exhaustive exercise-induced oxidative stress.

  4. Ultrasound assisted citric acid mediated pectin extraction from industrial waste of Musa balbisiana.

    Science.gov (United States)

    Maran, J Prakash; Priya, B; Al-Dhabi, Naif Abdullah; Ponmurugan, K; Moorthy, I Ganesh; Sivarajasekar, N

    2017-03-01

    The objectives of the present work are to extract pectin from industrial waste of Musa balbisiana by ultrasound assisted citric acid mediated extraction method and optimization was done through central composite statistical experimental design under response surface methodology. The outcomes of this study exhibited that, process variables (ultrasound power, pH and extraction time) had considerable influence on the pectin extraction. Second order mathematical equation was constructed to predict the data through regression analysis. The optimal extraction process condition was ultrasound power of 323w, pH of 3.2, extraction time of 27min and SL (solid-liquid) ratio of 1:15g/ml. The mean experimental yield of pectin (8.99±0.018%) was fine accord among predicted yield of pectin (9.02%). Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Ultrasound assisted extraction of pectin from waste Artocarpus heterophyllus fruit peel.

    Science.gov (United States)

    Moorthy, I Ganesh; Maran, J Prakash; Ilakya, S; Anitha, S L; Sabarima, S Pooja; Priya, B

    2017-01-01

    Four factors three level face centered central composite response surface design was employed in this study to investigate and optimize the effect of process variables (liquid-solid (LS) ratio (10:1-20:1ml/g), pH (1-2), sonication time (15-30min) and extraction temperature (50-70°C)) on the maximum extraction yield of pectin from waste Artocarpus heterophyllus (Jackfruit) peel by ultrasound assisted extraction method. Numerical optimization method was adapted in this study and the following optimal condition was obtained as follows: Liquid-solid ratio of 15:1ml/g, pH of 1.6, sonication time of 24min and temperature of 60°C. The optimal condition was validated through experiments and the observed value was interrelated with predicted value. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. 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.

  7. Ultrasound-assisted microwave preparation of Ag-doped CdS nanoparticles.

    Science.gov (United States)

    Ma, Jun; Tai, Guo'an; Guo, Wanlin

    2010-03-01

    Ag-doped CdS nanoparticles were synthesized by an ultrasound-assisted microwave synthesis method. The X-ray diffraction patterns reveal a structural evolution from cubic to hexagonal with increasing molar ratios of Ag(+)/Cd(2+) from 0% to 5%. It shows that the Ag-doped hexagonal CdS nanoparticles are polycrystal. The X-ray photoelectron spectroscopy of the CdS nanoparticles doping with 5% Ag(+) shows that the doped Ag in CdS is metallic. Simultaneously, the characteristic Raman peaks of the CdS nanoparticles enhance with increasing Ag(+) concentrations. The photocatalytic activity of different Ag-doped samples show a reasonable change due to different ratios of Ag which doped into CdS. Copyright 2009 Elsevier B.V. All rights reserved.

  8. Ultrasound-assisted osmotic dehydration and convective drying of apples: Process kinetics and quality issues

    Directory of Open Access Journals (Sweden)

    Mierzwa Dominik

    2016-09-01

    Full Text Available The aim of the present theme issue was to study the influence of ultrasound enhancement on the kinetics of osmotic dehydration and the effect of convective drying from the point of view of drying time and quality of dried products. Apple fruit was used as the experimental material. The kinetics of osmotic dehydration with (UAOD and without (OD ultrasound enhancement were examined for 40% fructose and sorbitol solutions. The effective dehydration time of osmotic process was determined. Preliminary dehydrated samples with OD and UAOD were next dried convectively with (CVUS and without (CV ultrasound assistance. The influence of OD and UAOD on the kinetics of CV and CVUS drying was analysed. The parameters of water activity and colour change were measured for the assessment of product quality after drying process.

  9. Recovery of squalene from wine lees using ultrasound assisted extraction-a feasibility study.

    Science.gov (United States)

    Naziri, Eleni; Mantzouridou, Fani; Tsimidou, Maria Z

    2012-09-12

    The present work is a systematic approach for valorization of wine lees regarding the recovery of squalene, a bioactive lipid. Such a study is presented for the first time in literature. Separate examination of squalene content in "light" and "heavy" lees from different vinification processes by RP-HPLC demonstrated that these waste streams can be used as a source for this lipid, despite variations due to technological or genetic effects. Next, ultrasound assisted extraction of squalene from the "industrial waste" (the mixture of wine lees generated from different wines) using n-hexane was optimized with the aid of response surface methodology (independent variables: sonication duration and duty cycles). Autolysis was monitored through optical microscopy. Squalene yield (0.6 ± 0.08 g SQ/kg dry lees) was comparable to that of recently examined potential sources (0.2-0.35 g SQ/kg dry olive pomace and 0.06 g SQ/kg olive leaves).

  10. Spherical nanocrystalline cellulose (NCC) from oil palm empty fruit bunch pulp via ultrasound assisted hydrolysis.

    Science.gov (United States)

    Zianor Azrina, Z A; Beg, M Dalour H; Rosli, M Y; Ramli, Ridzuan; Junadi, Norhafzan; Alam, A K M Moshiul

    2017-04-15

    Nanocrystalline cellulose (NCC) was isolated from oil palm empty fruit bunch pulp (EFBP) using ultrasound assisted acid hydrolysis. The obtained NCC was analysed using FESEM, XRD, FTIR, and TGA, and compared with raw empty fruit bunch fibre (REFB), empty fruit bunch pulp (EFBP), and treated empty fruit bunch pulp (TEFBP). Based on FESEM analysis, it was found that NCC has a spherical shaped after acid hydrolysis with the assistance of ultrasound. This situation was different compared to previous studies that obtained rod-like shaped of NCC. Furthermore, the crystallinity of NCC is higher compared to REFB and EFBP. According to thermal stability, the NCC obtained shows remarkable sign of high thermal stability compared to REFB and EFBP.

  11. 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.)

  12. Empirical modeling the ultrasound-assisted base-catalyzed sunflower oil methanolysis kinetics

    Directory of Open Access Journals (Sweden)

    Avramović Jelena M.

    2012-01-01

    Full Text Available The ultrasound-assisted sunflower oil methanolysis catalyzed by KOH was studied to define a simple empirical kinetic model useful for reactor design without complex computation. It was assumed that the neutralization of free fatty acids and the saponification reaction were negligible. The methanolysis process rate was observed to be controlled by the mass transfer limitation in the initial heterogeneous regime and by the chemical reaction in the later pseudo-homogeneous regime. The model involving the irreversible second-order kinetics was established and used for simulation of the triacylglycerol conversion and the fatty acid methyl esters formation in the latter regime. A good agreement between the proposed model and the experimental data in the chemically controlled regime was found.

  13. Extraction of polyphenols from black tea--conventional and ultrasound assisted extraction.

    Science.gov (United States)

    Both, Simon; Chemat, Farid; Strube, Jochen

    2014-05-01

    Products from plant raw materials gain increasing importance in food-, cosmetics and pharmaceutical industry. By way of contrast, due to lack of detailed physico-chemical fundamentals, existing production processes are economically not optimal designed. This leads to a need for deeper understanding of the processes and furthermore a systematic process and equipment design for the potentially applicable extraction techniques. Using the example of polyphenol extraction from black tea (Kenya), the conventional and ultrasound assisted extractions are investigated. Here, the state of the art as well as a comparison between the two techniques is in focus. Especially, resulting quasi-equilibria and mass transport kinetics serves as a criteria. The physico-chemical background is discussed taking particle size distributions and scanning electron microscope (SEM) measurements into account. Conclusively, process alternatives are projected and discussed. Hence, the present study makes influences of ultrasound technique on physico-chemical characteristics during extraction a subject of discussion.

  14. Surface characterization of adsorbents in ultrasound-assisted oxidative desulfurization process of fossil fuels.

    Science.gov (United States)

    Etemadi, Omid; Yen, Teh Fu

    2007-09-01

    Surface properties of two different phases of alumina were studied through SEM images. Characterization of amorphous acidic alumina and crystalline boehmite by XRD explains the differences in adsorption capacities of each sample. Data from small angle neutron scattering (SANS) provide further results regarding the ordering in amorphous and crystalline samples of alumina. Quantitative measurements from SANS are used for pore size calculations. Higher disorder provides more topological traps, irregularities, and hidden grooves for higher adsorption capacity. An isotherm model was derived for adsorption of dibenzothiophene sulfone (DBTO) by amorphous acidic alumina to predict and calculate the adsorption of sulfur compounds. The Langmuir-Freundlich model covers a wide range of sulfur concentrations. Experiments prove that amorphous acidic alumina is the adsorbent of choice for selective adsorption in the ultrasound-assisted oxidative desulfurization (UAOD) process to produce ultra-low-sulfur fuel (ULSF).

  15. 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.

  16. Bifunctional ultrasound assisted extraction and determination of Elettaria cardamomum Maton essential oil.

    Science.gov (United States)

    Sereshti, Hassan; Rohanifar, Ahmad; Bakhtiari, Sadjad; Samadi, Soheila

    2012-05-18

    A new hyphenated extraction method composed of ultrasound assisted extraction (UAE)-optimized ultrasound assisted emulsification microextraction (USAEME) was developed for the extraction and preconcentration of the essential oil of Elettaria cardamomum Maton. The essential oil was analyzed by gas chromatography-mass spectrometry (GC-MS) and optimization was performed using gas chromatography-flame ionization detection (GC-FID). Ultrasound played two different roles in the extraction of the essential oil. First, as a source of sufficient energy to break the oil-containing glands in order to release the oil, and second as an emulsifier to disperse the organic phase within water. The effective parameters (factors) of USAEME including volume of extraction solvent (C(2)H(4)Cl(2)), extraction temperature and ultrasonic time were optimized by using a central composite design (CCD). The optimal conditions were 120 μL for extraction solvent volume, 32.5 °C for temperature and 10.5 min for ultrasonic time. The linear dynamic ranges (LDRs) were 0.01-50 mg L(-1) with the determination coefficients in the range of 0.9990-0.9999. The limits of detection (LODs) and the relative standard deviations (RSDs) were 0.001-0.007 mg L(-1) and 3.6-6.3%, respectively. The enrichment factors were 93-98. The main components of the extracted essential oil were α-terpenyl acetate (46.0%), 1,8-cineole (27.7%), linalool (5.3%), α-terpineol (4.0%), linalyl acetate (3.5%).

  17. 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.

  18. A rapid ultrasound-assisted dispersive liquid-liquid microextraction followed by ultra-performance liquid chromatography for the simultaneous determination of seven benzodiazepines in human plasma samples.

    Science.gov (United States)

    Fernández, Purificación; González, Cristina; Pena, M Teresa; Carro, Antonia M; Lorenzo, Rosa A

    2013-03-12

    A simple and efficient ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) method has been developed for the determination of seven benzodiazepines (alprazolam, bromazepam, clonazepam, diazepam, lorazepam, lormetazepam and tetrazepam) in human plasma samples. Chloroform and methanol were used as extractant and disperser solvents, respectively. The influence of several variables (e.g., type and volume of dispersant and extraction solvents, pH, ultrasonic time and ionic strength) was carefully evaluated and optimized, using an asymmetric screening design 3(2)4(2)//16. Analysis of extracts was performed by ultra-performance liquid chromatography coupled with photodiode array detection (UPLC-PDA). Under the optimum conditions, two reversed-phases, Shield RP18 and C18 columns were successfully tested, obtaining good linearity in a range of 0.01-5μgmL(-1), with correlation coefficients r>0.996. Quantification limits ranged between 4.3-13.2ngmL(-1) and 4.0-14.8ngmL(-1), were obtained for C18 and Shield RP18 columns, respectively. The optimized method exhibited a good precision level, with relative standard deviation values lower than 8%. The recoveries studied at two spiked levels, ranged from 71 to 102% for all considered compounds. The proposed method was successfully applied to the analysis of seven benzodiazepines in real human plasma samples.

  19. Determination of acrylamide in brewed coffee and coffee powder using polymeric ionic liquid-based sorbent coatings in solid-phase microextraction coupled to gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cagliero, Cecilia; Ho, Tien D; Zhang, Cheng; Bicchi, Carlo; Anderson, Jared L

    2016-06-03

    This study describes a simple and rapid sampling method employing a polymeric ionic liquid (PIL) sorbent coating in direct immersion solid-phase microextraction (SPME) for the trace-level analysis of acrylamide in brewed coffee and coffee powder. The crosslinked PIL sorbent coating demonstrated superior sensitivity in the extraction of acrylamide compared to all commercially available SPME coatings. A spin coating method was developed to evenly distribute the PIL coating on the SPME support and reproducibly produce fibers with a large film thickness. Ninhydrin was employed as a quenching reagent during extraction to inhibit the production of interfering acrylamide. The PIL fiber produced a limit of quantitation for acrylamide of 10μgL(-1) and achieved comparable results to the ISO method in the analysis of six coffee powder samples.

  20. 离子液体-超声波辅助萃取火焰原子吸收法测定油画棒中的可迁移微量Cd2+%Ionic Liquid Based Ultrasonic-assisted Extraction Coupled with Flame Atomic Adsorption Spectrometry for the Determination of the Migration of Trace Cadmium in Oil Pastel

    Institute of Scientific and Technical Information of China (English)

    周先波; 江海亮; 周赛春; 钟勇

    2011-01-01

    以离子液体为萃取介质,超声波辅助萃取油画棒中的可迁移微量Cd2,以硝酸溶液反萃取后用火焰原子吸收法测定镉.考察了主要影响因素对萃取效果的影响.结果表明,以1-丁基-3-甲基咪唑六氟磷酸盐离子液体为萃取介质,溶液pH值为9.0、金属螯合剂用量为2.00 mL、离子液体的用量为2.00 mL、反萃剂为4.00 mL1.00mol·L-1硝酸、超声时间为5 min时,萃取率可达99%,富集倍数为25,除Cu2、pb2+外其它干扰离子对Cd2+的萃取影响不大.方法的加标回收率为96% ~ 103%,相对标准偏差(n=11)为1.7%,检出限为0.016 mg·L-1.%A flame atomic absorption spectrometric method coupled with ionic liquids based ultrasonic assisted extraction was developed for the determination of the migration of trace cadmium in oil pastel. The main factors affecting the extraction efficiency, such as pH value, amount of metal chelating, I-onic liquid and nitric acid, ultrasonic extraction time, metal ions interference and chain length of I-onic liquid were studied. The optimal conditions were as follows; pH value; 9.0, metal chelating amount; 2. 00 mL, amount of ionic liquid; 2. 00 mL, amount of nitric acid; 4. 00 mL 1. 00 mol ? L , ultrasonic extraction time; 5 min. Under the optimized conditions, the extraction efficiency of Cd reached up to 99% , and the enrichment times was 25. The other metal ions made no effects on the extraction efficiency of Cd2 + except for Cu2 + and Pb2 + . The recoveries for the method varied from 96% to 103% with relative standard deviation(/I = 11) of 1. 7% , and the detection limit was 0. 016 mg ? L -1.

  1. 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

  2. Rapid and sensitive analysis of polychlorinated biphenyls and acrylamide in food samples using ionic liquid-based in situ dispersive liquid-liquid microextraction coupled to headspace gas chromatography.

    Science.gov (United States)

    Zhang, Cheng; Cagliero, Cecilia; Pierson, Stephen A; Anderson, Jared L

    2017-01-20

    A simple and rapid ionic liquid (IL)-based in situ dispersive liquid-liquid microextraction (DLLME) method was developed and coupled to headspace gas chromatography (HS-GC) employing electron capture (ECD) and mass spectrometry (MS) detection for the analysis of polychlorinated biphenyls (PCBs) and acrylamide at trace levels from milk and coffee samples. The chemical structures of the halide-based ILs were tailored by introducing various functional groups to the cations to evaluate the effect of different structural features on the extraction efficiency of the target analytes. Extraction parameters including the molar ratio of IL to metathesis reagent and IL mass were optimized. The effects of HS oven temperature and the HS sample vial volume on the analyte response were also evaluated. The optimized in situ DLLME method exhibited good analytical precision, good linearity, and provided detection limits down to the low ppt level for PCBs and the low ppb level for acrylamide in aqueous samples. The matrix-compatibility of the developed method was also established by quantifying acrylamide in brewed coffee samples. This method is much simpler and faster compared to previously reported GC-MS methods using solid-phase microextraction (SPME) for the extraction/preconcentration of PCBs and acrylamide from complex food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Ionic liquid-based one-step micellar extraction of multiclass polar compounds from hawthorn fruits by ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Hu, Shuai-Shuai; Yi, Ling; Li, Xing-Ying; Cao, Jun; Ye, Li-Hong; Cao, Wan; Da, Jian-Hua; Dai, Han-Bin; Liu, Xiao-Juan

    2014-06-11

    An ionic liquid (IL)-based one-step micellar extraction procedure was developed for the extraction of multiclass polar analytes (protocatechuic acid, chlorogenic acid, epicatechin, hyperoside, isoquercitrin, quercetin) from hawthorn fruits and their determination using ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q-TOF/MS). Compared to conventional organic solvent extractions, this newly proposed method was much easier, more sensitive, environmentally friendly, and effective as well. Several important parameters influencing the micellar extraction efficiency are discussed, such as selection of ILs, surfactant concentration, and extraction time. Under the optimal conditions, good linearity was achieved for each analyte with correlation coefficients (r(2)) ranging from 0.9934 to 0.9999, and the recovery values ranged from 89.3 to 106% with relative standard deviations lower than 5.5%. Results suggest that the IL-based one-step micellar extraction could be an alternative and promising means in future food analysis.

  4. 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.

  5. 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).

  6. Sensitive determination of trace urinary 3-hydroxybenzo[a]pyrene using ionic liquids-based dispersive liquid-liquid microextraction followed by chemical derivatization and high performance liquid chromatography-high resolution tandem mass spectrometry.

    Science.gov (United States)

    Hu, Huan; Liu, Baizhan; Yang, Jun; Lin, Zuomin; Gan, Wuer

    2016-08-01

    3-Hydroxybenzo[a]pyrene (3-OHBaP) is widely used as a biomarker for assessing carcinogenic benzo[a]pyrene exposure risks. However, monitoring urinary 3-OHBaP suffers from an insufficient sensitivity due to the pg/mL level in urine excretion. In this study, a sensitive method for determination trace urinary 3-OHBaP was developed, involving enzymatic hydrolysis of the glucuronide and sulfate conjugates, ionic liquids dispersive liquid-liquid microextraction (IL-DLLME) enrichment, derivatization with dansyl chloride and HPLC-HRMS/MS analysis in the positive ion mode. Using IL-DLLME makes the enrichment of trace 3-OHBaP very simple, time-saving, efficiency and environmentally-friendly. To enhanced HPLC-HRMS/MS response, an MS-friendly dansyl group was introduced to increase the ionization and fragmentation efficiency. The optimal IL-DLLME extraction parameters and derivatization reaction conditions were investigated. Good linearity was obtained over a concentration range of 0.6-50.0pg/mL with correlation coefficients (r(2)) of 0.9918. The limit of detection (LOD) and limit of quantification (LOQ) values were 0.2pg/mL and 0.58pg/mL, respectively. The recoveries were 92.0±4.2% with the intra-day and inter-day RSD values ranged from 2.2% to 3.8% and from 3.3% to 6.8%, respectively. The proposed IL-DLLME-Dansylation-HPLC-HRMS/MS method was successfully applied to determine urinary 3-OHBaP of non-occupational exposed smokers and nonsmokers.

  7. Utilization of highly robust and selective crosslinked polymeric ionic liquid-based sorbent coatings in direct-immersion solid-phase microextraction and high-performance liquid chromatography for determining polar organic pollutants in waters.

    Science.gov (United States)

    Pacheco-Fernández, Idaira; Najafi, Ali; Pino, Verónica; Anderson, Jared L; Ayala, Juan H; Afonso, Ana M

    2016-09-01

    Several crosslinked polymeric ionic liquid (PIL)-based sorbent coatings of different nature were prepared by UV polymerization onto nitinol wires. They were evaluated in a direct-immersion solid-phase microextraction (DI-SPME) method in combination with high-performance liquid chromatography (HPLC) and diode array detection (DAD). The studied PIL coatings contained either vinyl alkyl or vinylbenzyl imidazolium-based (ViCnIm- or ViBCnIm-) IL monomers with different anions, as well as different dicationic IL crosslinkers. The analytical performance of these PIL-based SPME coatings was firstly evaluated for the extraction of a group of 10 different model analytes, including hydrocarbons and phenols, while exhaustively comparing the performance with commercial SPME fibers such as polydimethylsyloxane (PDMS), polyacrylate (PA) and polydimethylsiloxane/divinylbenzene (PDMS/DVB), and using all fibers under optimized conditions. Those fibers exhibiting a high selectivity for polar compounds were selected to carry out an analytical method for a group of 5 alkylphenols, including bisphenol-A (BPA) and nonylphenol (n-NP). Under optimum conditions, average relative recoveries of 108% and inter-day precision values (3 non-consecutive days) lower than 19% were obtained for a spiked level of 10µgL(-1). Correlations coefficients for the overall method ranged between 0.990 and 0.999, and limits of detection were down to 1µgL(-1). Tap water, river water, and bottled water were analyzed to evaluate matrix effects. Comparison with the PA fiber was also performed in terms of analytical performance. Partition coefficients (logKfs) of the alkylphenols to the SPME coating varied from 1.69 to 2.45 for the most efficient PIL-based fiber, and from 1.58 to 2.30 for the PA fiber. These results agree with those obtained by the normalized calibration slopes, pointing out the affinity of these PILs-based coatings.

  8. 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.

  9. Ultrasound-Assisted Extraction of Syringin from the Bark of Ilex rotunda Thumb Using Response Surface Methodology

    OpenAIRE

    Hui Wang; Li-Chun Zhao; Wei Li; Xin Deng; Xiang-Hua Xia; Jian Liang; Geng-Liang Yang; Ying He

    2012-01-01

    In this work, a rapid extraction method based on ultrasound-assisted extraction (UAE) of syringin from the bark of Ilex rotunda Thumb using response surface methodology (RSM) is described. The syringin was analyzed and quantified by high performance liquid chromatography coupled with UV detection (HPLC-UV). The extraction solvent, extraction temperature and extraction time, the three main factors for UAE, were optimized with Box-Behnken design (BBD) to obtain the highest ...

  10. Chemical composition and antioxidant activity of ultrasound-assisted extract of the endemic plant Haberlea rhodopensis Friv.

    OpenAIRE

    2013-01-01

    The antioxidant capacity of extracts from leaves of Haberlea rhodopensis Friv. obtained by a highly efficient and simple method of the ultrasound-assisted extraction was investigated. The total polyphenolic content was determined spectrophotometrically using the Folin − Ciocalteu’s phenol reagent and the polyphenols composition was analyzed by HPLC method. Antioxidant activity of the extract was evaluated as 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging activity, 2,2-azinobis-3 ethy...

  11. 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

  12. Ultrasound-Assisted Extraction May Not Be a Better Alternative Approach than Conventional Boiling for Extracting Polysaccharides from Herbal Medicines

    OpenAIRE

    Ka-Man Yip; Jun Xu; Wing-Sum Tong; Shan-Shan Zhou; Tao Yi; Zhong-Zhen Zhao; Hu-Biao Chen

    2016-01-01

    In clinical practice polysaccharides from herbal medicines are conventionally prepared by boiling water extraction (BWE), while ultrasound-assisted extraction (UAE) has often been used instead employed in laboratory research due to its strong extraction ability and efficiency. However, if and how the polysaccharides obtained by UAE and BWE are comparable, and hence whether the UAE-based research is instructive for the actual usage of herbal polysaccharides still requires further evaluation. T...

  13. 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.

  14. 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.

  15. Evaluation of ultrasound-assisted Menghini technique in liver graft biopsy

    Directory of Open Access Journals (Sweden)

    Marcel Vieira da Nóbrega

    2009-03-01

    Full Text Available Objective: To report on the experience of implementing ultrasound-assisted Menghini technique in the evaluation of liver transplant dysfunction. Methods: Menghini technique uses a suction needle, through percutaneous access, allowing a fast puncture (less than one second, which can help reduce the incidence of complications. Rresults: A total of 87 biopsies performed with 16-gauge suction needles were studied in a period of 15 months. Ultrasound was used to access the presence of perihepatic liquid or collections, biliary and vascular disorders, to mark a safe puncture site and for post-procedure control. The main biopsy indication was elevation of liver enzymes. In 81 cases, one fragment was collected and satisfactory samples were obtained in 85 procedures (97.7%. Minor complications occurred in six patients (6.9%, five with local pain and one with vagal reaction. There was a major complication (1.1%, hemothorax, which was diagnosed by clinical and radiological control examination and then treated. Cconclusions: Menghini technique to obtain liver tissue is quick, effective and safe, but it has always to follow the general care aspects of any intervention procedure. The ultrasound before and after the procedure helps marking an appropriate puncture site, may enhance the effectiveness of the method and is useful to identify possible early complications.

  16. Catalytic activity of copper (II) oxide prepared via ultrasound assisted Fenton-like reaction.

    Science.gov (United States)

    Angı, Arzu; Sanlı, Deniz; Erkey, Can; Birer, Özgür

    2014-03-01

    Copper (II) oxide nanoparticles were synthesized in an ultrasound assisted Fenton-like aqueous reaction between copper (II) cations and hydrogen peroxide. The reactions were initiated with the degradation of hydrogen peroxide by ultrasound induced cavitations at 0 °C or 5 °C and subsequent generation of the OH radical. The radical was converted into hydroxide anion in Fenton-like reactions and copper hydroxides were readily converted to oxides without the need of post annealing or aging of the samples. The products were characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and Brunauer-Emmett-Teller (BET) surface area analysis. Catalytic activity of the nanoparticles for the hydrogen peroxide assisted degradation of polycyclic aromatic hydrocarbons in the dark was tested by UV-visible spectroscopy with methylene blue as the model compound. The rate of the reaction was first order, however the rate constants changed after the initial hour. Initial rate constants as high as 0.030 min(-1) were associated with the high values of surface area, i.e. 70 m(2)/g. Annealing of the products at 150 °C under vacuum resulted in the decrease of the catalytic activity, underlying the significance of the cavitation induced surface defects in the catalytic process.

  17. Ultrasound-Assisted Extraction of Antioxidants in Misai Kucing (Orthosiphon stamineus

    Directory of Open Access Journals (Sweden)

    Swee Kheng Ho

    2014-08-01

    Full Text Available Ultrasound-assisted extraction (UAE with ethanol was used to extract the compounds responsible for the antioxidant activities of Misai Kucing (Orthosiphon stamineus. Response surface methodology (RSM was used to optimize four independent variables: ethanol concentration (%, amplitude (%, duty cycle (W/s and extraction time (min. Antioxidant compounds were determined by total phenolic content and total flavonoid content to be 1.4 g gallic acid equivalent/100 g DW and 45 g catechin equivalent/100 g DW, respectively. Antioxidant activities were evaluated using the 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid (ABTS•+ radical scavenging capacity assay and the 2,2-diphenyl-1-picrylhydrazyl (DPPH• radical scavenging capacity assay to be 1,961.3 and 2,423.3 µmol Trolox Equivalent Antioxidant Capacity (TEAC/100 g DW, respectively. Based on the optimal conditions, experimental values were reported to be close to the predicted value by RSM modeling (p > 0.05, indicating the suitability of UAE for extracting the antioxidants of Misai Kucing. Rosmarinic acid, kaempferol-rutinoside and sinesetine were identified by high performance liquid chromatography-mass spectrometry.

  18. Ultrasound-assisted extraction of antioxidants in Misai Kucing (Orthosiphon stamineus).

    Science.gov (United States)

    Ho, Swee Kheng; Tan, Chin Ping; Thoo, Yin Yin; Abas, Faridah; Ho, Chun Wai

    2014-08-19

    Ultrasound-assisted extraction (UAE) with ethanol was used to extract the compounds responsible for the antioxidant activities of Misai Kucing (Orthosiphon stamineus). Response surface methodology (RSM) was used to optimize four independent variables: ethanol concentration (%), amplitude (%), duty cycle (W/s) and extraction time (min). Antioxidant compounds were determined by total phenolic content and total flavonoid content to be 1.4 g gallic acid equivalent/100 g DW and 45 g catechin equivalent/100 g DW, respectively. Antioxidant activities were evaluated using the 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS•+) radical scavenging capacity assay and the 2,2-diphenyl-1-picrylhydrazyl (DPPH•) radical scavenging capacity assay to be 1,961.3 and 2,423.3 µmol Trolox Equivalent Antioxidant Capacity (TEAC)/100 g DW, respectively. Based on the optimal conditions, experimental values were reported to be close to the predicted value by RSM modeling (p>0.05), indicating the suitability of UAE for extracting the antioxidants of Misai Kucing. Rosmarinic acid, kaempferol-rutinoside and sinesetine were identified by high performance liquid chromatography-mass spectrometry.

  19. Value of Duplex Ultrasound Assistance for Thromboaspiration and Dilation of Thrombosed Native Arterio-Venous Fistulae

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Medina, J., E-mail: josegmedina57@gmail.com [Reina Sophia University Hospital, Vascular and Interventional Radiology Unit, Department of Radiology (Spain)

    2013-12-15

    Purpose: To evaluate the value of duplex ultrasound assistance during thromboaspiration of thrombosed arteriovenous fistulae for haemodialysis. Materials and Methods: We prospectively studied 54 thrombosed native fistulae (23 with total thrombosis and 31 with partial thrombosis), in which we performed manual thromboaspiration guided by ultrasonography associated with fluoroscopy. Results: The fistulae were located in the forearm (n = 39) or in the upper arm (n = 15) of 46 patients. Mean patient age was 65 years, and hypertension was the most common risk factor (74 %). Mean access age was 928 days (range 69-2,290), and most fistulae were on the left side (41 cases, 75.92 %). The success rate was 83 % in the total thrombosis group and 100 % in the partial thrombosis group. Including initial failures, the respective primary patency rates in the total thrombosis group and the partial thrombosis group were, respectively, 83 {+-} 8 % (n = 20) and 87 {+-} 6 % (n = 28) at 1 month, 39 {+-} 10 % (n = 10) and 61 {+-} 8 % (n = 20) at 6 months, and 17 {+-} 8 % (n = 5) and 26 {+-} 8 % (n = 9) at 1 year. The mean decrease of fluoroscopy time with ultrasound was 3 min (range 1-5). The mean decrease of radiation dose was 2.6 Gy cm Superscript-Two (range 0.9-4.3]. Conclusion: Ultrasound is a feasible and useful tool in the management of thrombosed native fistulae, thus decreasing radiation exposure, and has no detrimental effect on success rates.

  20. Modeling and optimization of ultrasound-assisted extraction of polysaccharide from Cucurbita moschata.

    Science.gov (United States)

    Prakash Maran, J; Mekala, V; Manikandan, S

    2013-02-15

    Polysaccharides from pumpkin were extracted by ultrasound-assisted extraction technology using four factors at five levels central composite rotatable response surface design (CCRD). On using single factor analysis, process variables such as extraction temperature (50-70 °C), power of ultrasound (50-70 W), time (15-25 min) and solid-liquid ratio (1:10-1:20 g/ml) were selected. Experiments were conducted to evaluate the effects of four independent variables on the maximum extraction yield of polysaccharides. From the experimental data, second order polynomial mathematical model were developed with high coefficient of determination values (R(2)>0.96). From response surface plots, temperature and ultrasound power exhibited independent and interactive effects on the extraction yields. Extraction temperature of 70 °C, ultrasound power of 70 W, time of 23 min and solid-liquid ratio of 1:10 g/ml were determined as optimal conditions with a maximum polysaccharides yield of 16.21%, which was confirmed through the validation of the experiments.

  1. Ecofriendly ultrasound-assisted rapid synthesis of gold nanoparticles using Calothrix algae

    Science.gov (United States)

    Kumar, Brajesh; Smita, Kumari; Sánchez, Erika; Guerra, Sara; Cumbal, Luis

    2016-06-01

    In the present work we demonstrate the ultrasound assisted synthesis of gold nanoparticles (AuNPs) in an ecofriendly manner using Calothrix algae. The production of the AuNPs in the reaction mixture is significantly accelerated by inducing ultrasound irradiation. The optical property, size distribution, morphology and crystalline phase of the AuNPs were determined by visual, UV-vis spectroscopy, dynamic light scattering, transmission electron microscopy (TEM) and x-ray diffraction (XRD) technique. The appearance of a light pink color at λ max = 550 nm indicated the synthesis of AuNPs. TEM images showed the formation of anisotropic AuNPs with predominant truncated shape and particles are in the range of 30-120 nm. The XRD spectrum of the AuNPs exhibited a Bragg reflections peak at 38.23°, corresponding to elemental gold. Further, AuNPs showed significant catalytic efficiency (rate constant, k = 0.072 4752 min-1) in reducing 4-nitrophenol (2 mM) to 4-aminophenol. The advantage of using ultrasound relates to the ecofriendly and rapid synthesis of AuNPs and various biotechnological applications were suggested.

  2. Ultrasound assisted siRNA delivery using PEG-siPlex loaded microbubbles.

    Science.gov (United States)

    Vandenbroucke, Roosmarijn E; Lentacker, Ine; Demeester, Joseph; De Smedt, Stefaan C; Sanders, Niek N

    2008-03-20

    Short interfering RNA (siRNA) attracts much attention for the treatment of various diseases. However, its delivery, especially via systemic routes, remains a challenge. Indeed, naked siRNAs are rapidly degraded, while complexed siRNAs massively aggregate in the blood or are captured by macrophages. Although this can be circumvented by PEGylation, we found that PEGylation had a strong negative effect on the gene silencing efficiency of siRNA-liposome complexes (siPlexes). Recently, ultrasound combined with microbubbles has been used to deliver naked siRNA but the gene silencing efficiency is rather low and very high amounts of siRNA are required. To overcome the negative effects of PEGylation and to enhance the efficiency of ultrasound assisted siRNA delivery, we coupled PEGylated siPlexes (PEG-siPlexes) to microbubbles. Ultrasound radiation of these microbubbles resulted in massive release of unaltered PEG-siPlexes. Interestingly, PEG-siPlexes loaded on microbubbles were able to enter cells after exposure to ultrasound, in contrast to free PEG-siPlexes, which were not able to enter cells rapidly. Furthermore, these PEG-siPlex loaded microbubbles induced, in the presence of ultrasound, much higher gene silencing than free PEG-siPlexes. Additionally, the PEG-siPlex loaded microbubbles only silenced the expression of genes in the presence of ultrasound, which allows space and time controlled gene silencing.

  3. 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

  4. 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.

  5. Ultrasound assisted enzyme catalyzed hydrolysis of waste cooking oil under solvent free condition.

    Science.gov (United States)

    Waghmare, Govind V; Rathod, Virendra K

    2016-09-01

    The present work demonstrates the hydrolysis of waste cooking oil (WCO) under solvent free condition using commercial available immobilized lipase (Novozyme 435) under the influence of ultrasound irradiation. The process parameters were optimized using a sequence of experimental protocol to evaluate the effects of temperature, molar ratios of substrates, enzyme loading, duty cycle and ultrasound intensity. It has been observed that ultrasound-assisted lipase-catalyzed hydrolysis of WCO would be a promising alternative for conventional methods. A maximum conversion of 75.19% was obtained at mild operating parameters: molar ratio of oil to water (buffer pH 7) 3:1, catalyst loading of 1.25% (w/w), lower ultrasound power 100W (ultrasound intensity - 7356.68Wm(-2)), duty cycle 50% and temperature (50°C) in a relatively short reaction time (2h). The activation energy and thermodynamic study shows that the hydrolysis reaction is more feasible when ultrasound is combined with mechanical agitation as compared with the ultrasound alone and simple conventional stirring technique. Application of ultrasound considerably reduced the reaction time as compared to conventional reaction. The successive use of the catalyst for repetitive cycles under the optimum experimental conditions resulted in a loss of enzymatic activity and also minimized the product conversion. Copyright © 2016. Published by Elsevier B.V.

  6. 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.

  7. 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

    2013-03-12

    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.

  8. Response surface optimization of ultrasound assisted extraction of pectin from pomegranate peel.

    Science.gov (United States)

    Moorthy, I Ganesh; Maran, J Prakash; Surya, S Muneeswari; Naganyashree, S; Shivamathi, C S

    2015-01-01

    Ultrasound assisted extraction of pectin from waste pomegranate peel was investigated and optimized using Box-Behnken response surface design coupled with numerical optimization technique. The individual and interactive effect of process variables (solid-liquid ratio, pH, extraction time and temperature) on the pectin yield was studied. The experimental data obtained were analyzed by Pareto analysis of variance (ANOVA) and second-order polynomial models were developed using multiple regression analysis. The models developed from the experimental design were predictive and good fit with the experimental data with high coefficient of determination (R(2)) value. The optimal extraction condition was found to be 1:17.52 g/ml of solid-liquid ratio, 1.27 of pH, 28.31 min of extraction time and 61.90 °C of extraction temperature respectively. Under the optimal conditions, experimental yield was very close to the predicted values. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Optimization of ultrasound-assisted compound enzymatic extraction and characterization of polysaccharides from blackcurrant.

    Science.gov (United States)

    Xu, Yaqin; Zhang, Ling; Yang, Yu; Song, Xiumei; Yu, Zeyuan

    2015-03-06

    In the present study, an efficient procedure for ultrasound-assisted compound enzymatic extraction of polysaccharides from blackcurrant fruits was investigated using response surface methodology (RSM). The Box-Behnken design was applied to optimize the effects of enzyme concentration (X1), pH (X2) and ultrasonic time (X3). The statistical analysis indicated that the independent variables (X1) and the quadratic terms (X1(2) and X3(2)) had significant effects on the yield of blackcurrant polysaccharides (BCP). The optimal conditions were: enzyme concentration 1.575%, pH 5.3, and ultrasonic time 25.6 min. The experimental yield of BCP was 14.28±0.06%, which was closely matched with the predicted yield of 14.31%. After preliminary purification, BCP I was obtained and characterized by GC, HPLC, and IR. BCP I comprised rhamnose, arabinose, xylose, mannose, glucose, and galactose in a molar ratio of 1.818:1.362:0.377:0.501:1.581:1.722 and its molecular weight was 8146 kDa. BCP I showed notable α-amylase inhibitory activity. Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. Ultrasound assisted forward osmosis concentration of fruit juice and natural colorant.

    Science.gov (United States)

    Chanukya, B S; Rastogi, Navin K

    2017-01-01

    The present study deals with the effect of higher and lower molecular weight compounds present in the feed on concentration polarization during forward osmosis concentration and its mitigation by the application of ultrasound. The effects of ultrasound on transmembrane water flux at different forward osmosis membrane orientations and different model feed solutions consisting of sucrose and pectin have also been evaluated. The feed containing sucrose and pectin subjected towards active layer of the membrane was found to be the most suitable orientation. The application of ultrasound (30kHz) significantly reduced the concentration polarization when the feed contains sucrose concentration up to 5%. Whereas, in case of feed containing 0.5% pectin, the ultrasound was not found to be effective in dislodging the gel layer formation resulting in severe external concentration polarization on the membrane surface. In comparison to the ordinary forward osmosis process, the ultrasound-assisted forward osmosis process resulted in higher water fluxes in case of sweet lime juice as well as rose extract containing anthocyanin. The degradation of rose anthocyanin due to ultrasound was found to be 1.82%. Application of ultrasound was found to be an effective way in mitigating concentration polarization on the forward osmosis membrane resulting in increased flux.

  11. 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.

  12. 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.

  13. Antioxidant Capacity of Rapeseed Extracts Obtained by Conventional and Ultrasound-Assisted Extraction.

    Science.gov (United States)

    Szydłowska-Czerniak, Aleksandra; Tułodziecka, Agnieszka

    2014-01-01

    Ultrasound-assisted extraction (UAE) and conventional solid-liquid extraction were applied to extract total antioxidants from two rapeseed varieties. The antioxidant capacities (AC) of winter and spring rapeseed cultivars were determined by four different analytical methods: ferric reducing antioxidant power (FRAP), cupric reducing antioxidant capacity (CUPRAC), 2,2'-diphenyl-1-picrylhydrazyl (DPPH), 2,2'-azino-bis-3-ethylbenzothiazoline-6-sulfonic acid (ABTS). The average AC of the studied rapeseed cultivars ranged between 4.21-10.03 mmol Trolox (TE)/100 g, 7.82-10.61 mmol TE/100 g, 8.11-51.59 mmol TE/100 g, 22.48-43.13 mmol TE/100 g for FRAP, CUPRAC, DPPH and ABTS methods, respectively. There are positive correlations between total phenolics (TPC = 804-1625 mg sinapic acid (SA)/100 g) and AC of the studied rapeseed extracts (r = 0.2650-0.9931). Results of the principal component analysis (PCA) indicate that there are differences between the total amounts of antioxidants in rapeseed samples extracted by different extraction techniques. Rapeseed extracts obtained after 18 min of ultrasonication revealed the highest content of total antioxidants. The UAE is a very useful, efficient and rapid technique of oilseed samples preparation for determination of AC by different analytical methods.

  14. 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.

  15. Recent developments on ultrasound-assisted one-pot multicomponent synthesis of biologically relevant heterocycles.

    Science.gov (United States)

    Banerjee, Bubun

    2017-03-01

    Heterocycles are the backbone of organic compounds. Specially, N- &O-containing heterocycles represent privileged structural subunits well distributed in naturally occurring compounds with immense biological activities. Multicomponent reactions (MCRs) are becoming valuable tool for synthesizing structurally diverse molecular entities. On the other hand, the last decade has seen a tremendous outburst in modifying chemical processes to make them sustainable for the betterment of our environment. The application of ultrasound in organic synthesis is fulfilling some of the goals of 'green and sustainable chemistry' as it has some advantages over the traditional thermal methods in terms of reaction rates, yields, purity of the products, product selectivity, etc. Therefore the synthesis of biologically relevant heterocycles using one-pot multi-component technique coupled with the application of ultrasound is one of the thrusting areas in the 21st Century among the organic chemists. The present review deals with the "up to date" developments on ultrasound assisted one-pot multi-component synthesis of biologically relevant heterocycles reported so far.

  16. Optimization of ultrasound-assisted extraction of camptothecin from Camptotheca acuminata seeds

    Institute of Scientific and Technical Information of China (English)

    JING Li-jia; LI Si-yang; CHANG Zui; WANG Yang; YAN Xiu-feng

    2011-01-01

    Naturally occurring camptothecin (CPT) is an important source of chemotherapeutic agents. The extraction from Camptotheca acuminata is still the main approach to obtain CPT compared with total synthesis. In the present study, ultrasound-assisted extractions (UAE) of CPT from C. acuminata seeds with alkaline solutions were investigated and CPT yield were determined by High Performance Liquid Chromatography. The conditions of alkaline species and concentrations, extraction time, extraction temperature and ultrasonic power were optimized.Results show that both Na3PO4 and Na2CO3 solutions gain good extraction yields, whereas Na3PO4 solution has stronger basicity and need higher concentration than Na2CO3 solution does, thus aqueous Na2CO3 is more beneficial for the extraction. The optimal condition was ultrasonically extracted with 0.5% aqueous Na2CO3 at 50℃ and ultrasonic power of 400 W for 60 min. Comparing with UAE with ethanol, the extraction with 0.5% Na2CO3 solution achieves higher yield. Moreover, aqueous Na2CO3 as a solvent has various advantages including non-toxicity, inflammable, non-corrosive and low cost, which ensure this UAE method is a superior method with high utilizing prospect.

  17. Kinetic modeling of the ultrasound-assisted extraction of polyphenols from Picea abies bark.

    Science.gov (United States)

    Lazar, Liliana; Talmaciu, Adina Iulia; Volf, Irina; Popa, Valentin I

    2016-09-01

    In this paper, the kinetics of polyphenols extraction from spruce bark (Picea abies) under ultrasounds action was investigated. Studies were performed in order to express the effect of some specific parameters (as: ultrasounds, surface contact between solvent and solid, extraction time and temperature) on the total phenolic content (TPC). Experiments were performed in the presence and absence of ultrasounds, using different contact surfaces between solvent and solid, for times from 5 to 75min and temperatures of 318, 323 and 333K. All these factors have a positive influence on the process, enhancing the extraction rate by recovering higher amounts of polyphenols. The process takes place in two stages: a fast one in the first 20-30min (first stage), followed by a slow one approaching to an equilibrium concentration after 40min (second stage). In these conditions, the second-order kinetic model was successfully developed for describing the mechanism of ultrasound-assisted extraction of polyphenols from P. abies bark. Based on this model, values of second-order extraction rate constant (k), initial extraction rate (h), saturation concentration (Cs) and activation energy (Ea) could be predicted. Model validation was done by plotting experimental and predicted values of TPC's, revealing a very good correlation between the obtained data (R(2)>0.98).

  18. 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.

  19. [Study on the occurrence of ferrum in coal by ultrasound-assisted sequential chemical extraction].

    Science.gov (United States)

    Xiong, Jin-Yu; Li, Han-Xu; Dong, Zhong-Bing; Zhang, Song; Qian, Ning-Bo; Wu, Cheng-Li

    2013-11-01

    To reveal the occurrence of Ferrum in coal, seven coal samples were selected according to the different contents of ferric oxide in the coal ash, and the content of Ferric element was determined by atomic absorption spectrophotometer (AAS) using nitric acid-perchloric acid-hydrofluoric acid wet digestion. Modes of occurrence of ferrium in the seven coal samples were studied by AAS using ultrasound-assisted sequential chemical extraction experiment (SCEE). Ultrasound promoted the contact of the extraction reagent with the coal particles and enhanced the dissolution process by producing characteristic acoustic cavitations, which greatly shortened the experimental time. The total amount of ferrium obtained by sequential extraction was approximate to the result of wet digestion, which indicated the procedure of SCEE was reasonable. The results showed that the ferric element mainly occurred in forms of carbonate state, Fe-Mn oxides state, sulfide state, sialic state and organic bound Fe in these coal samples. Among the various forms of these occurrences, the content of carbonate was the least, below 3.1%, while the content of sulfide was the dominant occurrence, ranging from 40% to 81.5%.

  20. Ultrasound-assisted oxidative desulfurization of liquid fuels and its industrial application.

    Science.gov (United States)

    Wu, Zhilin; Ondruschka, Bernd

    2010-08-01

    Latest environmental regulations require a very deep desulfurization to meet the ultra-low sulfur diesel (ULSD, 15 ppm sulfur) specifications. Due to the disadvantages of hydrotreating technology on the slashing production conditions, costs and safety as well as environmental protection, the ultrasound-assisted oxidative desulfurization (UAOD) as an alternative technology has been developed. UAOD process selectively oxidizes sulfur in common thiophenes in diesel to sulfoxides and sulfones which can be removed via selective adsorption or extractant. SulphCo has successfully used a 5000 barrel/day mobile "Sonocracking" unit to duplicate on a commercial scale its proprietary process that applies ultrasonics at relatively low temperatures and pressures. The UAOD technology estimate capital costs less than half the cost of a new high-pressure hydrotreater. The physical and chemical mechanisms of UAOD process are illustrated, and the effective factors, such as ultrasonic frequency and power, oxidants, catalysts, phase-transfer agent, extractant and adsorbent, on reaction kinetics and product recovery are discussed in this review.

  1. Enhanced UV absorbance and photoluminescence properties of ultrasound assisted synthesized gold doped ZnO nanorods

    Science.gov (United States)

    Sahu, Dojalisa; Panda, N. R.; Acharya, B. S.; Panda, A. K.

    2014-06-01

    Au doped ZnO (ZnO:Au) nanostructures were synthesized by ultrasound assisted wet chemical method. The concentration of dopant was varied and both structural and optical properties of ZnO:Au were investigated. The crystal structure and morphology of the samples were examined by X-ray diffraction (XRD) and transmission electron microscopy (TEM). These results showed the formation of nanorods of ZnO:Au having wurtzite structure and c-axis orientation. Gradual increase in crystallite size and bond length was also observed with the increase in gold concentration in ZnO intending the expansion of lattice after gold doping. The optical absorption measurements showed high ultraviolet (UV) absorbance property of ZnO:Au with sharp and intense absorption band in this region as compared to pristine ZnO. Photoluminescence (PL) measurements showed excitonic emission band of ZnO around 390 nm for both undoped and Au doped ZnO nanoparticles. Further, a strong emission around 467 nm was observed in the PL spectra of ZnO/ZnO:Au which was attributed to the transitions related to excess of oxygen vacancies. Interestingly, a new band was observed at 582 nm for doped ZnO samples which grew in intensity with doping concentration. This band was ascribed to the gold nanoparticle adsorbed on the surface of ZnO.

  2. 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.

  3. 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.

  4. Optimization of olive leaf extract obtained by ultrasound-assisted extraction with response surface methodology.

    Science.gov (United States)

    Şahin, Selin; Samlı, Rüya

    2013-01-01

    In the present article, ultrasound-assisted extraction (UAE) of polyphenols from agricultural and industrial waste of olive oil and table oil productions, olive tree (Olea europaea) leaves were investigated. The aim of the study is to examine the extraction parameters such as solvent concentration (0-100% ethanol (EtOH), v/v), the ratio of solid to solvent (25-50mg/mL) and extraction time (20-60 min), and to obtain the best possible combinations of these parameters through response surface methodology (RSM). The extract yield was stated as mg extract per g of dried leaf (DL). Total phenolic content was expressed in gallic acid equivalent (GAE) per g of dried leaf. Free radical scavenging activity for the antioxidant capacity was tested by 1,1-diphenyl-2-picryl hydrazyl (DPPH) radical. The second order polynomial model gave a satisfactory description of the experimental data. 201.2158 mg extract/g DL, 25.0626 mg GAE/g DL, and 95.5610% in respect to inhibition of DPPH radical were predicted at the optimum operating conditions (500 mg solid to 10 mL solvent ratio, 60 min of extraction time and 50% EtOH composition), respectively.

  5. Ultrasound assisted enzymatic conversion of non edible oil to methyl esters.

    Science.gov (United States)

    Jadhav, Sanket H; Gogate, Parag R

    2014-07-01

    Conventional and ultrasound-assisted hydrolysis and subsequent esterification of Nagchampa oil under mild operating conditions have been investigated with an objective of intensification of methyl esters production using a sustainable approach. The effect of ratio of reactants, temperature, enzyme loading, pretreatment of enzyme (using ultrasonic irradiations) on the hydrolysis and esterification reaction has been studied. Optimum conditions for hydrolysis were observed to be 1:1 weight ratio of oil: water for Lip Z and 1:3 for Lip 2 enzymes, enzyme loading of 400 units for Lip Z and 800 mg for Lip 2 enzymes and reaction time of 6h. In the case of esterification reaction, optimum conditions obtained were oil to methanol molar ratio of 1:2, enzyme loading of 1000 mg and reaction time of 20 h. Use of pretreated enzyme (using ultrasonic irradiations) was found to increase the extent of esterification reaction from 75% to 92.5%. It was observed that use of ultrasound in the reaction significantly intensified the esterification reaction with time requirement reducing from 20 h for conventional stirring based approach to only about 7.5 h in the presence of ultrasound. The extent of esterification obtained with sonicated enzyme also increased to 96% from 75% with unsonicated enzyme. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Comparative kinetic analysis of silent and ultrasound-assisted catalytic wet peroxide oxidation of phenol.

    Science.gov (United States)

    Rokhina, Ekaterina V; Repo, Eveliina; Virkutyte, Jurate

    2010-03-01

    The kinetic study of silent and ultrasound-assisted catalytic wet peroxide oxidation of phenol in water was performed to qualitatively assess the effect of ultrasound on the process kinetics. Various kinetic parameters such as the apparent kinetic rate constants, the surface utilization coefficient and activation energy of phenol oxidation over RuI(3) catalyst were investigated. Comparative analysis revealed that the use of ultrasound irradiation reduced the energy barrier of the reaction but had no impact on the reaction pathway. The activation energy for the oxidation of phenol over RuI(3) catalyst in the presence of ultrasound was found to be 13kJmol(-1), which was four times smaller in comparison to the silent oxidation process (57kJmol(-1)). Finally, 'figures-of-merit' was utilized to assess different experimental strategies such as sonolysis alone, H(2)O(2)-enhanced sonolysis and sono-catalytic oxidation of phenol in order to estimate the electric energy consumption based on the kinetic rate constants of the oxidation process.

  7. 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.

  8. 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 KMnO4 assisted by ultra-sonication. The pre-treatment was conducted for different exposure times (10, 20, 30 and 40min) using different concentrations of KMnO4 (1, 2, 3, 4, 5%w/v) at room temperature with solid/liquid ratio of 1:10. Pretreating SCW with 4% KMnO4 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 KMnO4 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.

  9. Ultrasound-assisted hydrolysis of waste cooking oil catalyzed by homemade lipases.

    Science.gov (United States)

    Mulinari, J; Venturin, B; Sbardelotto, M; Dall Agnol, A; Scapini, T; Camargo, A F; Baldissarelli, D P; Modkovski, T A; Rossetto, V; Dalla Rosa, C; Reichert, F W; Golunski, S M; Vieitez, I; Vargas, G D L P; Dalla Rosa, C; Mossi, A J; Treichel, H

    2017-03-01

    This study aimed to evaluate the waste cooking oil (WCO) hydrolysis in ultrasonic system using lipase as catalyst. Lipase was produced by the fungus Aspergillus niger via solid state fermentation (SSF) using canola meal as substrate. Prior to the hydrolysis reaction, the lipase behavior when subjected to ultrasound was evaluated by varying the temperature of the ultrasonic bath, the exposure time and the equipment power. Having optimized the treatment on ultrasound, the WCO hydrolysis reaction was carried out by evaluating the oil:water ratio and the lipase concentration. For a greater homogenization of the reaction medium, a mechanical stirrer at 170rpm was used. All steps were analyzed by experimental design technique. The lipase treatment in ultrasound generated an increase of about 320% in its hydrolytic activity using 50% of ultrasonic power for 25min. at 45°C. The results of the experimental design conducted for ultrasound-assisted hydrolysis showed that the best condition was using an oil:water ratio of 1:3 (v:v) and enzyme concentration of 15% (v/v), generating 62.67μmol/mL of free fatty acids (FFA) in 12h of reaction. Thus, the use of Aspergillus niger lipase as a catalyst for hydrolysis reaction of WCO can be considered as a possible pretreatment technique of the oil in order to accelerate its degradation. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. 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.

  11. Ultrasound assisted synthesis of PMMA/clay nanocomposites: Study of oxygen permeation and flame retardant properties

    Indian Academy of Sciences (India)

    Subrata K Patra; Gyanaranjan Prusty; Sarat K Swain

    2012-02-01

    PMMA/clay nanocomposites were synthesized by ultrasound assisted emulsifier-free emulsion polymerization technique. Ultrasound waves of different power and frequencies were applied to enhance the dispersion of the clay layers with polymer matrix. The structural information of the synthesized materials was studied by X-ray diffraction (XRD) and it was revealed that the interlayer spacing increased with clay loading. The magnitude of dispersion of the clay in the polymer matrix was detected by transmission electron microscopy (TEM). The Young’s modulus, breaking stress, elongation at break, toughness, yield stress and yield strain of the nanocomposites as a function of different clay concentrations and ultrasonic power were measured. Particle diameter of the nanocomposites was measured by laser diffraction technique. Oxygen permeability of the samples was studied and it was found that the oxygen flow rate was reduced by the combined effect of clay loading and ultrasound. The flame retardant property of the nanocomposites due to clay dispersion was investigated by measurement of limiting oxygen index (LOI).

  12. Determination of aflatoxins in rice samples by ultrasound-assisted matrix solid-phase dispersion.

    Science.gov (United States)

    Manoochehri, Mahboobeh; Asgharinezhad, Ali Akbar; Safaei, Mahdi

    2015-01-01

    This work describes the application of ultrasound-assisted matrix solid-phase dispersion as an extraction and sample preparation approach for aflatoxins (B1, B2, G1 and G2) and subsequent determination of them by high-performance liquid chromatography-fluorescence detection. A Box-Behnken design in combination with response surface methodology was used to determine the affecting parameters on the extraction procedure. 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 was investigated in the optimization study. C18, primary-secondary amine (PSA) and acetonitrile were selected as dispersing phase, clean-up phase and elution solvent, respectively. The obtained optimized values were sample-to-dispersing phase ratio of 1 : 1, 60 mg of PSA, 11 min ultrasonication time, 30°C ultrasonication temperature and 4 mL acetonitrile. Under the optimal conditions, the limits of detection were ranged from 0.09 to 0.14 ng g(-1) and the precisions [relative standard deviation (RSD%)] were <8.6%. The recoveries of the matrix solid-phase dispersion process ranged from 78 to 83% with RSD <10% in all cases. Finally, this method was successfully applied to the extraction of trace amounts of aflatoxins in rice samples. © The Author [2014]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  13. 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.

  14. The determination of trace element concentrations in fly ash samples using ultrasound-assisted digestion followed with inductively coupled plasma optical emission spectrometry

    OpenAIRE

    Ilander, Aki; Väisänen, Ari

    2009-01-01

    A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of trace element (chromium, copper, lead, nickel, vanadium and zinc) concentrations in fly ash samples was developed. All the measurements were performed in robust plasma conditions. Ultrasound-assisted digestion procedures using digestion solutions of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 80% for all the analyte...

  15. A new coupling of spectrophotometric determination with ultrasound-assisted emulsification dispersive liquid-liquid microextraction of trace silver

    Science.gov (United States)

    Wen, Xiaodong; Kong, Lamei; Chen, Meihui; Deng, Qingwen; Zhao, Xia; Guo, Jie

    2012-11-01

    In this work, a new coupling of spectrophotometric determination with preconcentration method named as ultrasound-assisted emulsification dispersive liquid-liquid microextraction (UAE-DLLME) for trace silver was firstly established. Disperser solvent in traditional DLLME was substituted by ultrasound-assisted emulsification, which could afford more effective emulsification and make the extraction method greener. The extraction was accomplished efficiently in only 3 min during ultrasound-assisted emulsification. Compared to traditional DLLME, the established pretreatment was simpler, greener and more effective. The UAE-DLLME technique was effectively coupled with ordinary spectrophotometer to improve the analytical performance and expand the application of spectrophotometric determination. The factors influencing UAE-DLLME, such as concentration of chelating agent, kind and volume of extractant, pH, conditions of phase separation, ultrasound extraction time and instrumental conditions, were studied in detail. Under the optimal conditions, the limit of detection (LOD) for silver was 0.45 μg L-1, with sensitivity enhancement factor (EF) of 35. The established method was applied to the determination of trace silver in real and certified reference samples with satisfactory analytical results.

  16. Synthesis of titanium dioxide by ultrasound assisted sol-gel technique: effect of calcination and sonication time.

    Science.gov (United States)

    Pinjari, D V; Prasad, Krishnamurthy; Gogate, P R; Mhaske, S T; Pandit, A B

    2015-03-01

    Nanostructured titanium dioxide has been synthesized using both conventional and ultrasound assisted sol-gel technique with an objective of understanding the role of cavitational effects in the synthesis process. The experiments were conducted at a constant calcination temperature of 750 °C and the calcination time was varied from 30 min to 3 h to study the effect of calcination time on the properties of the synthesized TiO₂. The TiO₂ specimens were characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The influence of the sonication time on the phase transformation process from anatase to rutile and also on the crystallite size and percentage crystallinity of the synthesized TiO₂ has also been investigated. It was observed that 100% phase transformation occurred after 3 h of calcination for the ultrasound assisted sol-gel synthesized TiO₂. The study on the phase transformation via variation of sonication time yielded interesting results. It was observed that as the sonication time increased, an initial increase in the rutile content is obtained and beyond optimum sonication time, the rutile content decreased. In general, the ultrasound assisted process results in synthesis of TiO₂ material with higher rutile content as compared to the conventional sol-gel process.

  17. 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 < 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.

  18. 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.

  19. 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

    2016-12-26

    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

  20. Ionic liquids based dispersive liquid-liquid microextraction coupled to gas chromatography for determination of aromatic hydrocarbons%基于离子液体的分散液液微萃取-气相色谱联用在苯系物分析中的应用

    Institute of Scientific and Technical Information of China (English)

    万晓星; 周兴旺; 汪敦佳

    2012-01-01

    通过改进气相色谱气化室,实现了离子液体分散液液微萃取与气相色谱的联用。以水不互溶的离子液体1-丁基-3-甲基咪唑六氟磷酸盐作为萃取剂,丙酮作为分散剂,能够从水溶液中有效地萃取苯系物。利用改进装置优化了苯、甲苯、乙苯的分散液液萃取及气相色谱分析条件,得到富集倍数为31~105,检出限为0.2~0.5μg/L.离子液体作为萃取剂在气相色谱进样后不产生溶剂干扰峰,且可回收重复利用。%The advantages of dipersive liquid-liquid microextraction(DLLME) coupled to gas chromatography are simplicity of operation,rapidity,low cost with high recovery rate and enrichment factor.Ionic liquids based DLLME coupled to gas chromatography for the simultaneous determination of diversified aromatic hydrocarbons was developed in this paper.The sample injection part of gas chromatographic instrument was modified to avoid the ionic liquid leaking into the chromatographic column.The parameters affecting extraction efficiency such as extractant,dispersive solvent,volume of the solvent and extraction time were studied.Under the optimum conditions,the enrichment factors ranged from 31 to 105.The linear range for the determination was 1-100 μg/L and the limits of detection were from 0.2 to 0.5 μg/L(S /N = 3),with the correlation coefficients(r) varying from 0.991 to 0.995.Using ionic liquid as extractantcan can effectively reduce the interference of solvent peak and enhance the extraction efficiency as well.

  1. 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.

  2. Ultrasound assisted dispersal of a copper nanopowder for electroless copper activation.

    Science.gov (United States)

    Graves, John E; Sugden, Mark; Litchfield, Robert E; Hutt, David A; Mason, Timothy J; Cobley, Andrew J

    2016-03-01

    This paper describes the ultrasound assisted dispersal of a low wt./vol.% copper nanopowder mixture and determines the optimum conditions for de-agglomeration. A commercially available powder was added to propan-2-ol and dispersed using a magnetic stirrer, a high frequency 850 kHz ultrasonic cell, a standard 40 kHz bath and a 20 kHz ultrasonic probe. The particle size of the powder was characterized using dynamic light scattering (DLS). Z-Average diameters (mean cluster size based on the intensity of scattered light) and intensity, volume and number size distributions were monitored as a function of time and energy input. Low frequency ultrasound was found to be more effective than high frequency ultrasound at de-agglomerating the powder and dispersion with a 20 kHz ultrasonic probe was found to be very effective at breaking apart large agglomerates containing weakly bound clusters of nanoparticles. In general, the breakage of nanoclusters was found to be a factor of ultrasonic intensity, the higher the intensity the greater the de-agglomeration and typically micron sized clusters were reduced to sub 100 nm particles in less than 30 min using optimum conditions. However, there came a point at which the forces generated by ultrasonic cavitation were either insufficient to overcome the cohesive bonds between smaller aggregates or at very high intensities decoupling between the tip and solution occurred. Absorption spectroscopy indicated a copper core structure with a thin oxide shell and the catalytic performance of this dispersion was demonstrated by drop coating onto substrates and subsequent electroless copper metallization. This relatively inexpensive catalytic suspension has the potential to replace precious metal based colloids used in electronics manufacturing.

  3. Ultrasound-assisted three-phase partitioning of polyphenol oxidase from potato peel (Solanum tuberosum).

    Science.gov (United States)

    Niphadkar, Sonali S; Rathod, Virendra K

    2015-01-01

    Conventional three phase partitioning (TPP) and ultrasound assisted three phase partitioning (UATPP) were optimized for achieving the maximum extraction and purification of polyphenol oxidase (PPO) from waste potato peels. Different process parameters such as ammonium sulfate (NH4)2SO4 concentration, crude extract to t-butanol ratio, time, temperature and pH were studied for conventional TPP. Except agitation speed, the similar parameters were also optimized for UATPP. Further additional parameters were also studied for UATPP viz. irradiation time at different frequencies, duty cycle and, rated power in order to obtain the maximum purification factor and recovery of PPO. The optimized conditions for conventional TPP were (NH4)2SO4 0-40% (w/v), extract to t-butanol ratio 1:1 (v/v), time 40 min and pH 7 at 30°C. These conditions provided 6.3 purification factor and 70% recovery of PPO from bottom phase. On the other hand, UATPP gives maximum purification fold of 19.7 with 98.3% recovery under optimized parameters which includes (NH4)2SO4 0-40% (w/v), crude extract to t-butanol ratio 1: 1 (v/v) pH 7, irradiation time 5 min with 25 kHz, duty cycle 40% and rated power 150W at 30°C. UATPP delivers higher purification factor and % recovery of PPO along with reduced operation time from 40 min to 5 min when compared with TPP. SDS PAGE showed partial purification of PPO enzyme with UATPP with molecular weight in the range of 26-36 kDa. Results reveal that UATPP would be an attractive option for the isolation and purification of PPO without need of multiple steps.

  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. Suspension column for recovery and separation of substances using ultrasound-assisted retention of bead sorbents.

    Science.gov (United States)

    Spivakov, Boris Ya; Shkinev, Valeriy M; Danilova, Tatiana V; Knyazkov, Nikolai N; Kurochkin, Vladimir E; Karandashev, Vasiliy K

    2012-12-15

    A novel approach to sorption recovery and separation of different substances is proposed which is based on the use of suspended bead sorbents instead of conventional packed beds of such sorbents. This makes it possible to employ small-sized beads which are trapped in a low-pressure column due to ultrasound-assisted retention, without any frits to hold the sorption material. A flow system including a separation mini-column, named herein a suspension column, has been developed and tested by the studies of solid phase extraction (SPE) of trace metals from bi-distilled water and sea water using a 150-μL column with a silica-based sorbent containing iminodiacetic groups (DIAPAK IDA) and having a grain size of 6 μm. The adsorption properties of DIAPAK IDA suspension (9.5mg) were evaluated through adsorption/desorption experiments, where the effect of solution pH and eluent on the SPE of trace metals were examined by ICP-MS or ICP-AES measurements. When sample solution was adjusted to pH 8.0 and 1 mol L(-1) nitric acid was used as eluent, very good recoveries of more than 90% were obtained for a number of elements in a single-step extraction. To demonstrate the versatility of the approach proposed and to show another advantage of ultrasonic field (acceleration of sorbate/sorbent interaction), a similar system was used for heterogeneous immunoassays of some antigens in ultrasonic field using agarose sorbents modified by corresponding antibodies. It has been shown that immunoglobulins, chlamidia, and brucellos bacteria can be quantitatively adsorbed on 15-μm sorbent (15 particles in 50 μL) and directly determined in a 50-μL mini-chamber using fluorescence detection.

  6. 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

    2017-04-12

    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 HNO3+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.

  7. Ionic liquids in chemical engineering.

    Science.gov (United States)

    Werner, Sebastian; Haumann, Marco; Wasserscheid, Peter

    2010-01-01

    The development of engineering applications with ionic liquids stretches back to the mid-1990s when the first examples of continuous catalytic processes using ionic liquids and the first studies of ionic liquid-based extractions were published. Ever since, the use of ionic liquids has seen tremendous progress in many fields of chemistry and engineering, and the first commercial applications have been reported. The main driver for ionic liquid engineering applications is to make practical use of their unique property profiles, which are the result of a complex interplay of coulombic, hydrogen bonding and van der Waals interactions. Remarkably, many ionic liquid properties can be tuned in a wide range by structural modifications at their cation and anion. This review highlights specific examples of ionic liquid applications in catalysis and in separation technologies. Additionally, the application of ionic liquids as working fluids in process machines is introduced.

  8. Ultrasound-assisted dispersive liquid-liquid microextraction for the determination of synthetic musk fragrances in aqueous matrices by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Homem, Vera; Alves, Alice; Alves, Arminda; Santos, Lúcia

    2016-01-01

    A rapid and simple method for the simultaneous determination of twelve synthetic musks in water samples, using ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) was successfully developed. The influence of seven factors (volume of the extraction solvent and disperser solvent, sample volume, extraction time, ionic strength, type of extraction and disperser solvent) affecting the UA-DLLME extraction efficiency was investigated using a screening design. The significant factors were selected and optimised employing a central composite design: 80 μL of chloroform, 880 μL of acetonitrile, 6 mL of sample volume, 3.5% (wt) of NaCl and 2 min of extraction time. Under the optimised conditions, this methodology was successfully validated for the analysis of 12 synthetic musk compounds in different aqueous samples (tap, sea and river water, effluent and influent wastewater). The proposed method showed enrichment factors between 101 and 115 depending on the analyte, limits of detection in the range of 0.004-54 ng L(-1) and good repeatability (most relative standard deviation values below 10%). No significant matrix effects were found, since recoveries ranged between 71% and 118%. Finally, the method was satisfactorily applied to the analysis of five different aqueous samples. Results demonstrated the existence of a larger amount of synthetic musks in wastewaters than in other water samples (average concentrations of 2800 ng L(-1) in influent and 850 ng L(-1) in effluent). Galaxolide, tonalide and exaltolide were the compounds most detected.

  9. Preparation of two HSO3-functionalized ionic liquids based on piperazinum cation and characterization of their structure as well as determination of their physical properties%两种基于哌嗪阳离子的磺酸功能化离子液体的合成及其结构表征和物理性质测定

    Institute of Scientific and Technical Information of China (English)

    崔文辉; 贾如琰; 王都留; 王昱; 吴磊

    2013-01-01

      以哌嗪、1,4-丁磺酸内酯及硫酸或磷酸为原料,合成了两种基于哌嗪阳离子的磺酸功能化酸性离子液体硫酸氢盐([(HSO3-b)2 pi]2+·2[HSO4]-)和1,4-二(4-磺酸基丁基)哌嗪磷酸二氢盐([(HSO3-b)2 pi]2+·2[H2 PO4]-);利用傅立叶变换红外光谱、核磁共振氢谱和碳谱表征了两种产物的结构,并测定了其熔点、黏度、电导率、热稳定性等物理性质。%Two kinds of bi-HSO3-functionalized ionic liquids based on piperazinum cation ,in-cluding 1 ,4-bis (4-sulfobutyl)piperazinum bis (hydrogen sulfate) coded as ([(HSO3-b)2 pi] [HSO4 ]2 ) and 1 ,4-bis(4-sulfobutyl) piperazinum bis(dihydrogen phosphate) coded as (HSO3-b)2 pi][H2 PO4 ]2 ) ,were synthesized with piperazine and 1 ,4-butane sultone as well as H2 SO4 or H3 PO4 as raw materials .The structure of as-synthesized products was confirmed by Fourier transform infrared spectrometry and nuclear magnetic resonance spectrometry (1 H NM R and 13C NMR);and their physical properties such as melting point ,viscosity in water ,electrical conductivity in water and ethanol ,and thermal stability were determined .

  10. 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.

  11. 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

    . 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.......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...

  12. The determination of trace element concentrations in fly ash samples using ultrasound-assisted digestion followed with inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Ilander, Aki; Väisänen, Ari

    2009-08-01

    A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of trace element (chromium, copper, lead, nickel, vanadium and zinc) concentrations in fly ash samples was developed. All the measurements were performed in robust plasma conditions. Ultrasound-assisted digestion procedures using digestion solutions of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 80% for all the analyte elements. Ultrasound-assisted two-step digestion with digestion solutions of 6mL of HNO(3) (Step 1) and 3mL of HNO(3)+3mL of HF (Step 2) resulted in recovery rates of over 92% for all the analyte elements with one exception, chromium, which had a recovery of about 85%. The analysis of SRM 1633b showed that the two-step ultrasound-assisted digestion method developed resulted in chromium, copper, nickel and zinc concentrations higher than the microwave digestion method standardized by the United States Environmental Protection Agency (USEPA method 3052). This is the very first time when a digestion method using ultrasound resulted in higher efficiency than microwave (USEPA method 3052) for chromium and nickel in very hard to dissolve samples. The major advantages of the ultrasound-assisted digestion over microwave digestion is the high treatment rate (about 30 samples simultaneously with a sonication time of 18min) and the possibility to use new sample vessels without a significant increase in costs.

  13. Augmented reality surgical navigation with ultrasound-assisted registration for pedicle screw placement: a pilot study.

    Science.gov (United States)

    Ma, Longfei; Zhao, Zhe; Chen, Fang; Zhang, Boyu; Fu, Ligong; Liao, Hongen

    2017-08-05

    We present a novel augmented reality (AR) surgical navigation system based on ultrasound-assisted registration for pedicle screw placement. This system provides the clinically desired targeting accuracy and reduces radiation exposure. Ultrasound (US) is used to perform registration between preoperative computed tomography (CT) images and patient, and the registration is performed by least-squares fitting of these two three-dimensional (3D) point sets of anatomical landmarks taken from US and CT images. An integral videography overlay device is calibrated to accurately display naked-eye 3D images for surgical navigation. We use a 3.0-mm Kirschner wire (K-wire) instead of a pedicle screw in this study, and the K-wire is calibrated to obtain its orientation and tip location. Based on the above registration and calibration, naked-eye 3D images of the planning path and the spine are superimposed onto patient in situ using our AR navigation system. Simultaneously, a 3D image of the K-wire is overlaid accurately on the real one to guide the insertion procedure. The targeting accuracy is evaluated postoperatively by performing a CT scan. An agar phantom experiment was performed. Eight K-wires were inserted successfully after US-assisted registration, and the mean targeting error and angle error were 3.35 mm and [Formula: see text], respectively. Furthermore, an additional sheep cadaver experiment was performed. Four K-wires were inserted successfully. The mean targeting error was 3.79 mm and the mean angle error was [Formula: see text], and US-assisted registration yielded better targeting results than skin markers-based registration (targeting errors: 2.41 vs. 5.18 mm, angle errors: [Formula: see text] vs. [Formula: see text]. Experimental outcomes demonstrate that the proposed navigation system has acceptable targeting accuracy. In particular, the proposed navigation method reduces repeated radiation exposure to the patient and surgeons. Therefore, it has promising

  14. Very superficial ultrasound-assisted lipoplasty for the treatment of axillary osmidrosis.

    Science.gov (United States)

    Park, S

    2000-01-01

    Treatment of axillary osmidrosis has been mainly concerned with surgical excision of glandular tissues and involved major surgical procedures with high morbidities and many complications. Search for a less invasive procedure for axillary osmidrosis resulted in the use of liposuction. However, there have been controversies over the efficacy of this method. The problem was that liposuction could not effectively remove the apocrine gland located in the dermis and dermosubcutaneous junction. A high rate of residual malodor and dissatisfaction were reported. The author used ultrasound-assisted lipoplasty (UAL) in the very superficial plane to remove the apocrine gland located in the dermis and dermosubcutaneous junction. The purpose of this study was to prove the efficacy of the very superficial UAL (VSUAL) for the treatment of axillary osmidrosis. From December 1998 to December 1999, 21 consecutive patients underwent UAL in their axilla for axillary osmidrosis. The follow-up period ranged from 2 to 12 months (mean: 8 months). UAL was performed in the very superficial plane with an amplitude of 40%. The very superficial UAL (VSUAL) was done mainly in a withdrawing manner with the tip of the cannula against the skin. The UAL (VSUAL) was done aggressively until the skin changed slightly erythematous. The results were assessed subjectively and objectively, and classified as excellent, good, fair, and poor. Nineteen patients were graded as excellent and one patient as good. The total satisfaction rate was 95.2%. One patient complained of residual malodor in her left axilla. There were no cases of skin necrosis, hematoma, or seroma. Histology showed partial removal of the subcutaneous layer and deep dermis, and degenerative epithelial changes in the apocrine glands in the residual deep dermis. These microscopic findings meant near-total functional ablation of the apocrine gland in the axilla comparable to "flap-to-graft conversion" or surgical excision of axillary skin. The

  15. Ionic-Liquid Based Separation of Azeotropic Mixtures

    DEFF Research Database (Denmark)

    Kulajanpeng, Kusuma; Suriyapraphadilok, Uthaiporn; Gani, Rafiqul

    2014-01-01

    such as stability, toxicity, and environmental impacts of the ILs. A Hildebrand solubility parameter group contribution model for ILs is highlighted to screen the miscibility of the ILs with the target solute component which was considered as a key target property to further screen the candidates from the previous...

  16. Ionic-Liquid-Based Polymer Electrolytes for Battery Applications.

    Science.gov (United States)

    Osada, Irene; de Vries, Henrik; Scrosati, Bruno; Passerini, Stefano

    2016-01-11

    The advent of solid-state polymer electrolytes for application in lithium batteries took place more than four decades ago when the ability of polyethylene oxide (PEO) to dissolve suitable lithium salts was demonstrated. Since then, many modifications of this basic system have been proposed and tested, involving the addition of conventional, carbonate-based electrolytes, low molecular weight polymers, ceramic fillers, and others. This Review focuses on ternary polymer electrolytes, that is, ion-conducting systems consisting of a polymer incorporating two salts, one bearing the lithium cation and the other introducing additional anions capable of plasticizing the polymer chains. Assessing the state of the research field of solid-state, ternary polymer electrolytes, while giving background on the whole field of polymer electrolytes, this Review is expected to stimulate new thoughts and ideas on the challenges and opportunities of lithium-metal batteries.

  17. Ionic-Liquid Based Separation of Azeotropic Mixtures

    DEFF Research Database (Denmark)

    Kulajanpeng, Kusuma; Suriyapraphadilok, Uthaiporn; Gani, Rafiqul

    2014-01-01

    such as stability, toxicity, and environmental impacts of the ILs. A Hildebrand solubility parameter group contribution model for ILs is highlighted to screen the miscibility of the ILs with the target solute component which was considered as a key target property to further screen the candidates from the previous...... on minimum concentration of the ILs required to break the given azeotrope, the best ILs as entrainers for water + ethanol and water + isopropanol azeotropic mixtures were [C1MIM][DMP] and [C2MIM][N(CN)2], respectively....

  18. Determination of polybrominated diphenyl ethers in water and soil samples by cloud point extraction-ultrasound-assisted back-extraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Fontana, Ariel R; Silva, María F; Martínez, Luis D; Wuilloud, Rodolfo G; Altamirano, Jorgelina C

    2009-05-15

    A novel and efficient analytical methodology is proposed for extracting and preconcentrating polybrominated diphenyl ethers (PBDEs) from samples of environmental interest prior gas chromatography-mass spectrometry (GC-MS) analysis. It is based on the induction of micellar organized medium by using a non-ionic surfactant (Triton X-114) to extract the target PBDEs. To enable coupling the efficient extracting technique with GC analysis, ultrasound-assisted back-extraction (UABE) into an organic solvent was required. Several factors, including surfactant type and concentration, equilibration temperature and time, ionic strength, pH and buffers nature and concentration were studied and optimized over the extraction efficiency of the proposed technique. Under optimal experimental conditions, the target analytes were quantitatively extracted achieving an enrichment factor of 250 when 10mL aliquot of ultrapure water spiked with PBDE-standard mixture (10pgmL(-1) each PBDE) was extracted. Method detection limits (MDLs) calculated with aqueous PBDEs solutions as three times the signal-to-noise ratio (S/N), ranged from 1 to 2pgmL(-1) with RSDs values /=0.9987 and linear range of all PBDEs was 4-150pgmL(-1). The proposed methodology was validated by carrying out a recovery study by spiking the samples at two different concentration levels of PBDEs (10 and 50pgmL(-1) for waters samples). Recoveries values in the range of 96-106% for water samples were obtained showing satisfactory robustness of the method for analyzing PBDEs in water samples. The proposed methodology was applied for the analysis of PBDEs: 2,2',4,4'-tetraBDE (BDE-47), 2,2',4,4,5-pentaBDE (BDE-99), 2,2',4,4,6-pentaBDE (BDE-100) and 2,2,4,4',5,5'-hexaBDE (BDE-153) in water samples, including drinking, lake, river water and soil samples. Significant quantities of PBDEs were not found in the analyzed samples.

  19. 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.

  20. Towards the industrial production of antioxidants from food processing by-products with ultrasound-assisted extraction.

    Science.gov (United States)

    Virot, Matthieu; Tomao, Valérie; Le Bourvellec, Carine; Renard, Catherine M C G; Chemat, Farid

    2010-08-01

    Apple pomace, a by-product of the cider production, has been studied as a potential source of polyphenols, compounds of great interest for the industry. Ultrasound has been used to improve extraction efficiency in terms of time needed and total polyphenol content. A preliminary study has been first investigated to optimize ethanol proportion of aqueous extractant (50%, v/v) and solid/liquid ratio (<15%, w/v). A response surface methodology has then been used to maximize total polyphenol content of extracts and investigate influence of parameters involved in extraction procedures for both total polyphenols content and composition of extracts. Optimal settings reached from a central composite design were applied for ultrasound-assisted extraction and were compared to conventional procedure: yields were increased by more than 20%. Ultrasound-assisted polyphenols extraction from apple pomace appears to be a relevant, rapid, sustainable alternative to conventional procedure, and that scale up of the process is possible. Copyright 2009 Elsevier B.V. All rights reserved.

  1. 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....

  2. Ultrasound-assisted extraction of pectins from grape pomace using citric acid: a response surface methodology approach.

    Science.gov (United States)

    Minjares-Fuentes, R; Femenia, A; Garau, M C; Meza-Velázquez, J A; Simal, S; Rosselló, C

    2014-06-15

    An ultrasound-assisted procedure for the extraction of pectins from grape pomace with citric acid as the extracting agent was established. A Box-Behnken design (BBD) was employed to optimize the extraction temperature (X1: 35-75°C), extraction time (X2: 20-60 min) and pH (X3: 1.0-2.0) to obtain a high yield of pectins with high average molecular weight (MW) and degree of esterification (DE) from grape pomace. Analysis of variance showed that the contribution of a quadratic model was significant for the pectin extraction yield and for pectin MW whereas the DE of pectins was more influenced by a linear model. An optimization study using response surface methodology was performed and 3D response surfaces were plotted from the mathematical model. According to the RSM model, the highest pectin yield (∼32.3%) can be achieved when the UAE process is carried out at 75°C for 60 min using a citric acid solution of pH 2.0. These pectic polysaccharides, composed mainly by galacturonic acid units (ultrasound-assisted extraction could be a good option for the extraction of functional pectins with citric acid from grape pomace at industrial level. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. 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

    2016-11-28

    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.

  4. 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.

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

    Science.gov (United States)

    He, Kuang; Lv, YuanCai; Chen, YuanCai

    2014-10-01

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

  6. 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.

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

    Science.gov (United States)

    Ilander, Aki; Väisänen, Ari

    2007-10-29

    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).

  8. 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

  9. 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

  10. Application of ultrasound-assisted emulsification microextraction based on applying low-density organic solvent for the determination of organochlorine pesticides in water samples.

    Science.gov (United States)

    Zhang, Yufeng; Lee, Hian Kee

    2012-08-24

    In this study, a polyethylene Pasteur pipette-based ultrasound-assisted emulsification microextraction (USAEME) applying low-density organic solvent was successfully developed for the extraction of trace levels of organochlorine pesticides (OCPs) in water samples and followed by gas chromatography-mass spectrometry (GC-MS) analysis. In this approach, a polyethylene Pasteur squeeze-type pipette was employed as a convenient extraction device and ultrasound radiation was applied to accelerate the emulsification of low-density organic solvent in aqueous solutions to enhance the microextraction efficiency of OCPs in water samples. Thirty microliters of extraction solvent (isooctane), of lower density than water, were injected into the aqueous sample solution held in the pipette. The latter was then immersed in an ultrasound water bath to form an emulsion. After 30s extraction, phase separation was achieved by centrifugation. The upper layer (isooctane) was collected and analyzed by GC-MS. No disperser solvent was required in this procedure. Significantly, fast analysis and high extraction efficiency were achieved. Another feature of the procedure was the use of the pipette as the extraction device, which permitted less dense than water organic solvent to be used as extraction solvent. This method broadens the applicability of USAEME to a wider range of solvent. Additionally, carry-over problems were avoided with the use of the disposable pipette. Parameters affecting the efficiency of polyethylene Pasteur pipette-based USAEME, such as the extraction solvent, extraction solvent volume, extraction and centrifugation time, ionic strength and extraction temperature were investigated. Under the optimum conditions, the proposed method provided good enrichment factors (EFs) in the range of 128 and 328, with relative standard deviations (RSDs) ranging from 2.7% to 12.4%. The limits of detection were in the range of 0.8 and 10ng/L depending on the analytes. The linearities were

  11. Coacervative microextraction ultrasound-assisted back-extraction technique for determination of organophosphates pesticides in honey samples by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Fontana, Ariel R; Camargo, Alejandra B; Altamirano, Jorgelina C

    2010-10-08

    Coacervative microextraction ultrasound-assisted back-extraction technique (CME-UABE) is proposed for the first time for extracting and preconcentrating organophosphates pesticides (OPPs) from honey samples prior to gas chromatography-mass spectrometry (GC-MS) analysis. The extraction/preconcentration technique is supported on the micellar organized medium based on non-ionic surfactant. To enable coupling the proposed technique with GC, it was required to back extract the analytes into hexane. Several variables including, surfactant type and concentration, equilibration temperature and time, matrix modifiers, pH and buffers nature were studied and optimized over the relative response of the analytes. The best working conditions were as follows: an aliquot of 10 mL 50 gL(-1) honey blend solution was conditioned by adding 100 μL 0.1 molL(-1) hydrochloric acid (pH 2) and finally extracted with 100 μL Triton X-114 100 gL(-1) at 85°C for 5 min using CME technique. Under optimal experimental conditions, the enrichment factor (EF) was 167 and limits of detection (LODs), calculated as three times the signal-to-noise ratio (S/N=3), ranged between 0.03 and 0.47 ngg(-1). The method precision was evaluated over five replicates at 1 ngg(-1) with RSDs ≤ 9.5%. The calibration graphs were linear within the concentration range of 0.3-1000 ngg(-1) for chlorpirifos; and 1-1000 ngg(-1) for fenitrothion, parathion and methidathion, respectively. The coefficients of correlation were ≥ 0.9992. Validation of the methodology was performed by standard addition method at two concentration levels (2 and 20 ngg(-1)). The recoveries were ≥ 90%, indicating satisfactory robustness of the methodology, which could be successfully applied for determination of OPPs in honey samples of different Argentinean regions. Two of the analyzed samples showed levels of methidathion ranged between 1.2 and 2.3 ngg(-1).

  12. 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).

  13. Optimization for ultrasound-assisted extraction of polysaccharides with antioxidant activity in vitro from the aerial root of Ficus microcarpa.

    Science.gov (United States)

    Jiang, Changxing; Li, Xia; Jiao, Yunpeng; Jiang, Dingyun; Zhang, Ling; Fan, Benxia; Zhang, Qianghua

    2014-09-22

    In this study, optimization of ultrasound-assisted extraction and antioxidant activity of polysaccharides from the aerial root of Ficus microcarpa (FMPS) were investigated. The optimal conditions for extraction of FMPS were determined as followings: ultrasound power 200 W, ultrasound temperature 70°C, extraction temperature 74°C, liquid-solid ratio 35, extraction time 238 min, ultrasound time 49 min. The experimental yield of FMPS (3.44%) obtained under these conditions was well agreement with the value predicted by the model. In addition, Fourier transform-infrared spectroscopy and antioxidant activity assays revealed that FMPS were acidic polysaccharides and had strong Fe2+ chelating activity and moderate hydrogen peroxide scavenging effect. Further work on the purification, structure characterization and antioxidant activity in vivo of FMPS is in progress.

  14. 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.

  15. Ultrasound-assisted extraction of syringin from the bark of Ilex rotunda thumb using response surface methodology.

    Science.gov (United States)

    Zhao, Li-Chun; He, Ying; Deng, Xin; Xia, Xiang-Hua; Liang, Jian; Yang, Geng-Liang; Li, Wei; Wang, Hui

    2012-01-01

    In this work, a rapid extraction method based on ultrasound-assisted extraction (UAE) of syringin from the bark of Ilex rotunda Thumb using response surface methodology (RSM) is described. The syringin was analyzed and quantified by high performance liquid chromatography coupled with UV detection (HPLC-UV). The extraction solvent, extraction temperature and extraction time, the three main factors for UAE, were optimized with Box-Behnken design (BBD) to obtain the highest extraction efficiency. The optimal conditions were the use of a sonication frequency of 40 kHz, 65% methanol as the solvent, an extraction time of 30 min and an extraction temperature of 40 °C. Using these optimal conditions, the experimental values agreed closely with the predicted values. The analysis of variance (ANOVA) indicated a high goodness of model fit and the success of the RSM method for optimizing syringin extraction from the bark of I. rotunda.

  16. 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.

  17. Phase structuring in metal alloys: Ultrasound-assisted top-down approach to engineering of nanostructured catalytic materials.

    Science.gov (United States)

    Cherepanov, Pavel V; Andreeva, Daria V

    2017-03-01

    High intensity ultrasound (HIUS) is a novel and efficient tool for top-down nanostructuring of multi-phase metal systems. Ultrasound-assisted structuring of the phase in metal alloys relies on two main mechanisms including interfacial red/ox reactions and temperature driven solid state phase transformations which affect surface composition and morphology of metals. Physical and chemical properties of sonication medium strongly affects the structuring pathways as well as morphology and composition of catalysts. HIUS can serve as a simple, fast, and effective approach for the tuning of structure and surface properties of metal particles, opening the new perspectives in design of robust and efficient catalysts. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Recovery and purification of cholesterol from cholesterol-β-cyclodextrin inclusion complex using ultrasound-assisted extraction.

    Science.gov (United States)

    Li, Yong; Chen, Youliang; Li, Hua

    2017-01-01

    Response surface methodology was used to optimize ultrasound-assisted ethanol extraction (UAE) of cholesterol from cholesterol-β-cyclodextrin (C-β-CD) inclusion complex prepared from duck yolk oil. The best extraction conditions were solvent-solid ratio 10mL/g, ultrasonic power 251W, extraction temperature 56°C and sonication time 36min. Under these conditions, the highest cholesterol extraction yield and cholesterol content obtained 98.12±0.25% and 43.38±0.61mg/g inclusion complex, respectively. As compared with Reflux extraction and Soxhlet extraction, the UAE was more efficient and economical. To increase the purity of crude cholesterol extraction, silica gel column chromatography and crystallization were carried out. Finally, cholesterol was obtained at 95.1% purity, 71.7% recovery and 22.0% yield.

  19. "Solvent-free" ultrasound-assisted extraction of lipids from fresh microalgae cells: a green, clean and scalable process.

    Science.gov (United States)

    Adam, Fanny; Abert-Vian, Maryline; Peltier, Gilles; Chemat, Farid

    2012-06-01

    In order to comply with criteria of green chemistry concepts and sustainability, a new procedure has been performed for solvent-free ultrasound-assisted extraction (UAE) to extract lipids from fresh Nannochloropsis oculata biomass. Through response surface methodology (RSM) parameters affecting the oil recovery were optimized. Optimum conditions for oil extraction were estimated as follows: (i) 1000 W ultrasonic power, (ii) 30 min extraction time and (iii) biomass dry weight content at 5%. Yields were calculated by the total fatty acids methyl esters amounts analyzed by GC-FID-MS. The maximum oil recovery was around 0.21%. This value was compared with the one obtained with the conventional extraction method (Bligh and Dyer). Furthermore, effect of temperature on the yield was also investigated. The overall results show an innovative and effective extraction method adapted for microalgae oil recovery, without using solvent and with an enable scaling up. Copyright © 2012 Elsevier Ltd. All rights reserved.

  20. Response surface modeling and optimization of ultrasound-assisted extraction of three flavonoids from tartary buckwheat (Fagopyrum tataricum

    Directory of Open Access Journals (Sweden)

    Lian-Xin Peng

    2013-01-01

    Full Text Available Background: Buckwheat (Fagopyrum spp., Polygonaceae is a widely planted food crop. Flavonoids, including quercetin, rutin, and kaempferol, are the main bioactive components in tartary buckwheat (Fagopyrum tataricum (L. Gaertn. From the nutriological and pharmacological perspectives, flavonoids have great value in controlling blood glucose and blood pressure levels, and they also have antioxidant properties. Objective: To optimize the conditions for extraction of quercetin, rutin, and kaempferol from F. tataricum. Materials and Methods: A combination of ultrasound-assisted extraction (UAE and response surface methodology (RSM was used for flavonoid extraction and yield assessment. The RSM was based on a three-level, three-variable Box-Behnken design. Results: Flavonoids were optimally extracted from F. tataricum by using 72% methanol, at 60°C, for 21 minutes. Under these conditions, the obtained extraction yield of the total flavonoids was 3.94%. Conclusion : The results indicated that the UAE method was effective for extraction of flavonoids from tartary buckwheat.

  1. 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.

  2. Ultrasound assisted polymerization for synthesis of ZnO/Polypyrrole composites for zinc/nickel rechargeable battery

    Science.gov (United States)

    Huang, Jianhang; Yang, Zhanhong; Yang, Bin; Wang, Ruijuan; Wang, Tingting

    2014-12-01

    ZnO/Polypyrrole (PPy) composites are synthesized by ultrasound assisted chemical polymerization of PPy in the presence of ZnO particles. With different initial content of pyrrole, granular and layered ZnO/PPy composite are formed. The fourier transform infrared spectra (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) are adopted to characterize the as-prepared samples. ZnO/PPy composites are used as anode material for Zn/Ni batteries. Galvanostatic charge/discharge experiments, cyclic voltammograms (CV) and electrochemical impedance spectroscopy (EIS) are conducted to evaluate the cycle performance of electrodes. ZnO/PPy composites show superior capacity stability, more stable charge plateau and higher discharge plateau compared to conventional ZnO electrode. Furthermore, rate performance is also improved by ZnO/PPy composites.

  3. 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.

  4. 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 sludge < sediment.

  5. Kinetic modeling of ultrasound-assisted extraction of phenolic compounds from grape marc: influence of acoustic energy density and temperature.

    Science.gov (United States)

    Tao, Yang; Zhang, Zhihang; Sun, Da-Wen

    2014-07-01

    The effects of acoustic energy density (6.8-47.4 W/L) and temperature (20-50 °C) on the extraction yields of total phenolics and tartaric esters during ultrasound-assisted extraction from grape marc were investigated in this study. The ultrasound treatment was performed in a 25-kHz ultrasound bath system and the 50% aqueous ethanol was used as the solvent. The initial extraction rate and final extraction yield increased with the increase of acoustic energy density and temperature. The two site kinetic model was used to simulate the kinetics of extraction process and the diffusion model based on the Fick's second law was employed to determine the effective diffusion coefficient of phenolics in grape marc. Both models gave satisfactory quality of data fit. The diffusion process was divided into one fast stage and one slow stage and the diffusion coefficients in both stages were calculated. Within the current experimental range, the diffusion coefficients of total phenolics and tartaric esters for both diffusion stages increased with acoustic energy density. Meanwhile, the rise of temperature also resulted in the increase of diffusion coefficients of phenolics except the diffusion coefficient of total phenolics in the fast stage, the value of which being the highest at 40 °C. Moreover, an empirical equation was suggested to correlate the effective diffusion coefficient of phenolics in grape marc with acoustic energy density and temperature. In addition, the performance comparison of ultrasound-assisted extraction and convention methods demonstrates that ultrasound is an effective and promising technology to extract bioactive substances from grape marc. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Determination of metals in coal fly ashes using ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Pontes, Fernanda V M; Mendes, Bruna A de O; de Souza, Evelyn M F; Ferreira, Fernanda N; da Silva, Lílian I D; Carneiro, Manuel C; Monteiro, Maria I C; de Almeida, Marcelo D; Neto, Arnaldo A; Vaitsman, Delmo S

    2010-02-05

    A method for determination of Co, Cr, Cu, Fe, Mn, Ni, Ti, V and Zn in coal fly ash samples using ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) is proposed. The digestion procedure consisted in the sonication of the previously dried sample with hydrofluoric acid and aqua regia at 80 degrees C for 30 min, elimination of fluorides by heating until dryness for about 1h and dissolution of the residue with nitric acid solution. A classical digestion method, used as comparative method, consisted in the addition of HCl, HNO(3) and HF to 1 g of sample, and heating on a hot plate until dryness for about 6h. The proposed method presents several advantages: it requires lower amounts of sample and reagents, and it is faster. It is also advantageous when compared to the published methods, which also use ultrasound-assisted digestion procedure: lower detection limits for Co, Cu, Ni, V and Zn, and it does not require shaking during the digestion. The detection limits (microg g(-1)) for Co, Cr, Cu, Fe, Mn, Ni, Ti, V and Zn were 0.06, 0.37, 1.0, 25, 0.93, 0.45, 4.0, 1.7 and 4.3, respectively. The results were in good agreement with those obtained by the classical method and reference values. The exception was Cr, which presented low recoveries in classical and proposed methods (83 and 87%, respectively). Also, the concentration for Cu obtained by the proposed method was significantly different from the reference value, in spite of the good recovery (91+/-1%).

  7. 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.

  8. Application of an optimized dispersive nanomaterial ultrasound-assisted microextraction method for preconcentration of carbofuran and propoxur and their determination by high-performance liquid chromatography with UV detection.

    Science.gov (United States)

    Khodadoust, Saeid; Talebianpoor, Mohammad Sharif; Ghaedi, Mehrorang

    2014-11-01

    An extraction method based on dispersive nanomaterial ultrasound-assisted microextraction was used for the preconcentration of carbofuran and propoxur insecticides in water samples prior to high-performance liquid chromatography with UV detection. ZnS:Ni nanoparticles were synthesized based on the reaction of the mixture of zinc acetate and nickel acetate with thioacetamide in aqueous media and then loaded on activated carbon (ZnS:Ni-AC). Different methods were used for recognizing the properties of ZnS:Ni-AC and then this nanomaterial was used for extraction of carbamate insecticide as new adsorbent. The influence of variables on the extraction method (such as amount of adsorbent (mg: NiZnS-AC), pH and ionic strength of sample solution, vortex and ultrasonic time (min), ultrasound temperature and desorption volume (mL) was investigated by a screening 2(7-4) Plackett-Burman design. Then the significant variables were optimized by using a central composite design combined with a desirability function. At optimum conditions, this method had linear response >0.0060-10 μg/mL with detection limit 0.0015 μg/mL and relative standard deviations <5.0% (n = 3). © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Simultaneous Determination of Flavonoids in Rhododendron Mucronatum Leaves by Ionic Liquid-based Ultrasonic-assisted Extraction Combined with High Performance Liquid Chromatography%离子液体-超声辅助萃取/高效液相色谱法测定白花杜鹃叶中的黄酮

    Institute of Scientific and Technical Information of China (English)

    陈君; 周光明; 杨远高; 秦红英; 窦文虎

    2013-01-01

    建立了以离子液体1-丁基-3-甲基咪唑溴化盐([BMIM] Br)水溶液为萃取剂,超声辅助萃取结合反相高效液相色谱/紫外检测器同时分离测定白花杜鹃叶中的芦丁、槲皮素和山奈酚3种黄酮化合物的方法.采用Phenomenex C18色谱柱(250 mm ×4.6 nn,5μm)进行分离,以乙腈-0.25%乙酸水溶液梯度洗脱,流速1.0 mL·min-1,紫外检测波长355 nm,柱温34℃.在优化条件下,芦丁、槲皮素和山奈酚分别在0.064~128、0.076~152、0.064~128 mg·L-1范围内线性关系良好,相关系数(r)均为0.9999,检出限(S/N=3)分别为0.0066、0.0092、0.005 0 mg·L-1;样品的回收率为90%~97%.实验结果表明,该萃取方法操作简单快速,定量结果准确可靠,且绿色环保,为白花杜鹃叶中黄酮的提取、分离及检测提供了有效的方法.%A novel ionic liquid-based ultrasonic-assisted extraction (ILUAE) combined with reverse-phase high performance liquid chromatography tandem UV detection ( HPLC - UV) was first developed to isolate and determinate flavonoids in rhododendron mucronatum leaves. The 1-butyl-3-methylimid-azolium chloride ( [BMIM]Br) aqueous solution was selected as extraction solvent. The sample was separated on a Phenomenex C18 column using acetonitrile -0. 25% acetic acid as mobile phase by gradient elution at a flow rate of 1. 0 mL·min-1. The UV detection wavelength was set at 355 nm. The quantitative analysis of rutin, quercetin and kaempferol were carried out by the external standard method. Under the optimal extraction conditions, the calibration curves of rutin, quercetin, and kaempferol were linear in the ranges of 0. 064 - 128, 0. 076 - 152 and 0.064 - 128 mg·L-1, respectively, with correlation coefficients of 0. 999 9. Their limits of detection(LODs, S/N = 3) were 0. 006 6, 0. 009 2 and 0. 005 0 mg·L-1, respectively. The spiked recoveries of three compounds ranged from 90% to 97% . The results indicated that the proposed method was an

  10. 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.

  11. Synthesis, characterization and thermal properties of thiosalicylate ionic liquids

    Indian Academy of Sciences (India)

    Cecilia Devi Wilfred; Fadwa Babiker Mustafa

    2013-11-01

    In an attempt to produce new functionalized ionic liquids, a series of thiosalicylate ionic liquids based on imidazolium, ammonium, phosphonium, choline and pyrrolidinium cations were synthesized. The compounds were characterized by Infra Red (IR), Nuclear Magnetic Resonance (NMR) and mass spectra (ESI-MS). Their glass-transition temperatures, melting points and decomposition temperatures have been measured. Physicochemical properties of ionic liquids are influenced by alkyl chain length and nature of the cation of ionic liquids.

  12. 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.

  13. 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.

  14. Evaluation, prediction and optimization the ultrasound-assisted extraction method using response surface methodology: antioxidant and biological properties of Stachys parviflora L.

    OpenAIRE

    2016-01-01

    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 ...

  15. Ultrasound-Assisted Thoracic Paravertebral Block Reduces Intraoperative Opioid Requirement and Improves Analgesia after Breast Cancer Surgery: A Randomized, Controlled, Single-Center Trial.

    Directory of Open Access Journals (Sweden)

    Lijian Pei

    Full Text Available The contribution of ultrasound-assisted thoracic paravertebral block to postoperative analgesia remains unclear. We compared the effect of a combination of ultrasound assisted-thoracic paravertebral block and propofol general anesthesia with opioid and sevoflurane general anesthesia on volatile anesthetic, propofol and opioid consumption, and postoperative pain in patients having breast cancer surgery.Patients undergoing breast cancer surgery were randomly assigned to ultrasound-assisted paravertebral block with propofol general anesthesia (PPA group, n = 121 or fentanyl with sevoflurane general anesthesia (GA group, n = 126. Volatile anesthetic, propofol and opioid consumption, and postoperative pain intensity were compared between the groups using noninferiority and superiority tests.Patients in the PPA group required less sevoflurane than those in the GA group (median [interquartile range] of 0 [0, 0] vs. 0.4 [0.3, 0.6] minimum alveolar concentration [MAC]-hours, less intraoperative fentanyl requirements (100 [50, 100] vs. 250 [200, 300]μg,, less intense postoperative pain (median visual analog scale score 2 [1, 3.5] vs. 3 [2, 4.5], but more propofol (median 529 [424, 672] vs. 100 [100, 130] mg. Noninferiority was detected for all four outcomes; one-tailed superiority tests for each outcome were highly significant at P<0.001 in the expected directions.The combination of propofol anesthesia with ultrasound-assisted paravertebral block reduces intraoperative volatile anesthetic and opioid requirements, and results in less post operative pain in patients undergoing breast cancer surgery.ClinicalTrial.gov NCT00418457.

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

    OpenAIRE

    Ilander, Aki; Väisänen, Ari

    2007-01-01

    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...

  17. 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.

  18. Optimization of the ultrasound-assisted extraction of anthocyanins and total phenolic compounds in mulberry (Morus nigra) pulp.

    Science.gov (United States)

    Espada-Bellido, Estrella; Ferreiro-González, Marta; Carrera, Ceferino; Palma, Miguel; Barroso, Carmelo G; Barbero, Gerardo F

    2017-03-15

    New ultrasound-assisted extraction methods for the determination of anthocyanins and total phenolic compounds present in mulberries have been developed. Several extraction variables, including methanol composition (50-100%), temperature (10-70°C), ultrasound amplitude (30-70%), cycle (0.2-0.7s), solvent pH (3-7) and solvent-solid ratio (10:1.5-20:1.5) were optimized. A Box-Behnken design in conjunction with a response surface methodology was employed to optimize the conditions for the maximum response based on 54 different experiments. Two response variables were considered: total anthocyanins and total phenolic compounds. Extraction temperature and solvent composition were found to be the most influential parameters for anthocyanins (48°C and 76%) and phenolic compounds (64°C and 61%). The developed methods showed high reproducibility and repeatability (RSD<5%). Finally, the new methods were successfully applied to real samples in order to investigate the presence of anthocyanins and total phenolic compounds in several mulberry jams. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. 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.

  20. 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.

  1. Transient neurological deficit due to a misplacement of central venous catheter despite ultrasound guidance and ultrasound assistance.

    Science.gov (United States)

    Idialisoa, Rado; Jouffroy, Romain; Saint Martin, Laure Castres; Lamhaut, Lionel; Baud, Frédéric; Philippe, Pascal; Carli, Pierre; Vivien, Benoît

    2015-10-01

    Central venous catheters (CVC) are frequently used in intensive care units (ICU), with a low incidence of complications, most of them being of mechanical origin and occurring during the insertion of the catheter. To avoid such complications, "ultrasound guidance" and "ultrasound assistance" are recommended. Nevertheless, even with trained and experienced physicians, mechanical complications of IJV access such as carotid punctures are still reported. We report the case of a 75-year-old woman, admitted into the ICU for CVC insertion due to impossibility of peripheral venous access. About 12 hours after the procedure, the patient presented a neurological deficit. The cervical and thoracic CT scan showed a transfixing path of the catheter from the left IJV into the left common carotid artery, with distal extremity of the catheter localized in the ascending aorta. The catheter was removed, and thereafter the neurological deficit immediately and definitely disappeared. Onset of a neurological deficit after CVC insertion into the IJV, regardless the time of occurrence after the procedure, should suggest complication due to the CVC insertion, even if procedure was uneventful and chest radiography confirmed the apparent accurate position of CVC.

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

    Science.gov (United States)

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

    2014-09-01

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

  3. Ultrasound-assisted dispersive liquid-liquid microextraction for the determination of six pyrethroids in river water.

    Science.gov (United States)

    Yan, Hongyuan; Liu, Baomi; Du, Jingjing; Yang, Gengliang; Row, Kyung Ho

    2010-08-06

    A simple ultrasound-assisted dispersive liquid-liquid microextraction method combined with liquid chromatography was developed for the preconcentration and determination of six pyrethroids in river water samples. The procedure was based on a ternary solvent system to formatting tiny droplets of extractant in sample solution by dissolving appropriate amounts of water-immiscible extractant (tetrachloromethane) in watermiscible dispersive solvent (acetone). Various parameters that affected the extraction efficiency (such as type and volume of extraction and dispersive solvent, extraction time, ultrasonic time, and centrifuging time) were evaluated. Under the optimum condition, good linearity was obtained in a range of 0.00059-1.52 mg L(-1) for all analytes with the correlation coefficient (r(2))>0.999. Intra-assay and inter-assay precision evaluated as the relative standard deviation (RSD) were less than 3.4 and 8.9%. The recoveries of six pyrethroids at three spiked levels were in the range of 86.2-109.3% with RSD of less than 8.7%. The enrichment factors for the six pyrethroids were ranged from 767 to 1033 folds.

  4. Detection of optical and mechanical property inhomogeneities in tissue mimicking phantoms using an ultrasound assisted optical probe.

    Science.gov (United States)

    Devi, C Usha; Chandran, R Sreekumari Bharat; Vasu, R Mohan; Sood, Ajay K

    2008-01-01

    We discuss the issue of separating contributions from mechanical and optical properties of a moderately scattering tissue phantom to the modulation depth (M) of intensity autocorrelation measured in an ultrasound-assisted optical tomography system using axial and transverse illuminations. For axial illumination, M is affected by both the displacement and absorption coefficient, more prominently by displacement. But transverse illumination has very little contribution from displacement of scattering centers. Since displacement is related to the elastic property of the insonified region, we show that there is a possibility of separating the contributions from elastic and optical properties of the insonified region using axial and transverse illuminations. The main conclusions of our study using moderately scattering phantoms are: 1. axial illumination is the best for mapping storage modulus inhomogeneities, but M is also affected by optical absorption; 2. transverse illumination is the best for mapping absorption inhomogeneities; and 3. for the practically relevant case of an inclusion with larger storage modulus and absorption, both illuminations produced large contrast in M. When the scattering coefficient is high, the angle dependence of illumination is lost and the present method is shown to fail to separate these contributions based on direction of illumination.

  5. Phase transformation of nanostructured titanium dioxide from anatase-to-rutile via combined ultrasound assisted sol-gel technique.

    Science.gov (United States)

    Prasad, Krishnamurthy; Pinjari, D V; Pandit, A B; Mhaske, S T

    2010-02-01

    An effort was made to synthesize nanostructured TiO(2) via sol-gel technique to obtain a 100% rutile polymorph of nanostructured TiO(2). The sol-gel synthesis technique was suitably modified by incorporating ultrasound to study the effect of cavitation on the phase transformation, crystallite size, crystallinity and morphological (scanning electron microscopy) properties of the obtained nano-TiO(2). It was observed that using ultrasound, yield of the nano-TiO(2) was improved from 86.35% to 95.078%. The phase transformation of anatase-to-rutile of TiO(2) was studied for both (ultrasound assisted and conventional) the processes. Complete phase transformation of the TiO(2) was observed as expected with and without the use of ultrasound but the marked reduction in the required calcination temperature for obtaining 100% phase transformation with ultrasound was the major achievement in the present study, leading to 70% energy savings during calcination.

  6. 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 Fe3O4-loaded coffee waste hydrochar (Fe3O4-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 Fe3O4-CHC. The specific surface area of hydrochar increased from 17.2 to 34.7m(2)/g after loading of Fe3O4 nanoparticles onto it. The prepared Fe3O4-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 Na2SO4, respectively. The synthesized Fe3O4-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 Fe3O4-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.

  7. Optimization of ultrasound-assisted extraction of colchicine compound from Colchicum haussknechtii by using response surface methodology

    Directory of Open Access Journals (Sweden)

    Saeid Khodadoust

    2017-04-01

    Full Text Available In this research an ultrasound-assisted extraction (UAE method was used for extraction of colchicine in root of Colchicum haussknechtii prior to high-performance liquid chromatography with UV detection. C. haussknechtii is used widely in traditional medicine for the treatment of various diseases. The root of this plant is full of colchicine that is suitable for the treatment of gout and cirrhosis and applicable in plant breeding studies to produce polyploidy. The influence of variables on the extraction method was investigated by response surface methodology (RSM and composite design (CCD to achieve maximum extraction yield of colchicine from the root of C. haussknechtii. The most suitable condition for the extraction of colchicine was found to at 40 °C temperature, 32 min extraction time, and 70:30 v/v ethanol–water mixtures with 45:1 solvent-solid ratio. Obtained results showed that there is 1.2% colchicine in the root of C. haussknechtii, so this plant could be introduced as a rich source of colchicine.

  8. Synthesis of Caffeine/Maleic Acid Co-crystal by Ultrasound-assisted Slurry Co-crystallization.

    Science.gov (United States)

    Apshingekar, Prafulla P; Aher, Suyog; Kelly, Adrian L; Brown, Elaine C; Paradkar, Anant

    2017-01-01

    A green approach has been used for co-crystallization of noncongruent co-crystal pair of caffeine/maleic acid using water. Ultrasound is known to affect crystallization; hence, the effect of high power ultrasound on the ternary phase diagram has been investigated in detail using a slurry co-crystallization approach. A systematic investigation was performed to understand how the accelerated conditions during ultrasound-assisted co-crystallization will affect different regions of the ternary phase diagram. Application of ultrasound showed considerable effect on the ternary phase diagram, principally on caffeine/maleic acid 2:1 (disappeared) and 1:1 co-crystal (narrowed) regions. Also, the stability regions for pure caffeine and maleic acid in water were narrowed in the presence of ultrasound, expanding the solution region. The observed effect of ultrasound on the phase diagram was correlated with solubility of caffeine and maleic acid and stability of co-crystal forms in water. Copyright © 2016. Published by Elsevier Inc.

  9. Ultrasound-assisted heating extraction of pectin from grapefruit peel: optimization and comparison with the conventional method.

    Science.gov (United States)

    Wang, Wenjun; Ma, Xiaobin; Xu, Yuting; Cao, Yongqiang; Jiang, Zhumao; Ding, Tian; Ye, Xingqian; Liu, Donghong

    2015-07-01

    The extraction of pectin from grapefruit peel by ultrasound-assisted heating extraction (UAHE) was investigated using response surface methodology and compared with the conventional heating extraction (CHE). The optimized conditions were power intensity of 12.56 W/cm(2), extraction temperature of 66.71°C, and sonication time of 27.95 min. The experimental optimized yield was 27.34%, which was well matched with the predicted value (27.46%). Compared with CHE, UAHE provided higher yield increased by 16.34% at the temperature lowered by 13.3°C and the time shortened by 37.78%. Image studies showed that pectin extracted by UAHE showed better color and more loosen microstructure compared to that extracted by CHE, although Fourier Transform Infrared Analysis indicated insignificant difference in their chemical structures. Furthermore, UAHE pectin possessed lower viscosity, molecular weight and degree of esterification, but higher degree of branching and purity than CHE pectin, indicating that the former was preliminarily modified during the extraction process.

  10. Effects of Microwave and Ultrasound Assisted Extraction on the Recovery of Soy Proteins for Soy Allergen Detection.

    Science.gov (United States)

    Amponsah, Amma; Nayak, Balunkeswar

    2016-10-14

    The extraction of soy proteins for soy allergen detections is conventionally achieved with PBS buffer for at least 2 h at room temperature or 4 °C. This method has been reported to be inefficient due to time consumption and inadequate protein extraction resulting in false negative allergen detection and mislabeling of foods containing allergenic proteins. This study investigated the application of microwave (MAE) and ultrasound assisted extraction (UAE) techniques to extract and improve recovery of allergens from various soy matrices. Soy proteins were extracted from raw soy flour, soy protein isolate (SPI) and soy milk using MAE at 60, 70, and 100 °C for 5 and 10 min and UAE at 4 and 23 °C for extraction times of 1, 5, and 10 min with PBS, Laemmli and urea buffers. Extracts were analyzed for total proteins, protein profile, and antibody-based detection (ELISA) of soy proteins. Conventional extraction with each of the buffers was used as controls. Overall, proteins recovered from MAE and UAE samples were higher than recoveries from the controls in all soy matrices. Under all extraction conditions, Laemmli and urea buffer recovered more proteins than PBS. Electrophoresis analysis of protein showed bands around 75, 50, and 33 kDa indicating the presence of soy allergenic proteins β-conglycinin and glycinin, in all samples. Using sandwich ELISA, control and UAE extracts resulted in high soy protein detection but this reduced in MAE extracts.

  11. 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.

  12. Intensification of ultrasound-assisted process for the preparation of spindle-shape sodium zinc molybdate nanoparticles.

    Science.gov (United States)

    Bhanvase, B A; Patel, M A; Sonawane, S H; Pandit, A B

    2016-01-01

    In the present work, sodium zinc molybdate (SZM) nanoparticles were prepared using conventional and an innovative ultrasound assisted co-precipitation of sodium molybdate, zinc oxide and HNO3 at different temperatures. Prepared product was characterized by XRD, TEM, FT-IR, particle size distribution (PSD), TGA and DTA techniques. TEM analysis shows the spindle-shaped morphology of the formed SZM nanoparticles. The average particle size of SZM nanoparticles is found to be lower in case of sonochemical method (78.3 nm) compared to conventional method (340.2 nm) which is attributed to faster solute transfer rate due to ultrasonic irradiation leading to rapid nucleation and restricted growth of SZM nanoparticles. Further, the kinetics of synthesis of SZM nanoparticles are studied using the sonochemical method at different operating temperature and conventional method at 80°C. It is shown that the rate of reaction is significantly faster at 40°C compared to other temperatures and also conventional method. This can be attributed to intense cavity collapse at lower temperature (low vapour pressure) compared to higher temperature (high vapour pressure) of the reaction mixture.

  13. Determination of Oleanolic and Ursolic Acids in Hedyotis diffusa Using Hyphenated Ultrasound-Assisted Supercritical Carbon Dioxide Extraction and Chromatography

    Directory of Open Access Journals (Sweden)

    Ming-Chi Wei

    2015-01-01

    Full Text Available Oleanolic acid (OA and ursolic acid (UA were extracted from Hedyotis diffusa using a hyphenated procedure of ultrasound-assisted and supercritical carbon dioxide (HSC–CO2 extraction at different temperatures, pressures, cosolvent percentages, and SC–CO2 flow rates. The results indicated that these parameters significantly affected the extraction yield. The maximal yields of OA (0.917 mg/g of dry plant and UA (3.540 mg/g of dry plant were obtained at a dynamic extraction time of 110 min, a static extraction time of 15 min, 28.2 MPa, and 56°C with a 12.5% (v/v cosolvent (ethanol/water = 82/18, v/v and SC–CO2 flowing at 2.3 mL/min (STP. The extracted yields were then analyzed by high performance liquid chromatography (HPLC to quantify the OA and UA. The present findings revealed that H. diffusa is a potential source of OA and UA. In addition, using the hyphenated procedure for extraction is a promising and alternative process for recovering OA and UA from H. diffusa at high concentrations.

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

    Science.gov (United States)

    Barros, Joélia M; Bezerra, Marcos A; Valasques, Gisseli S; Do Nascimento Jr, Baraquízio B; Souza, Anderson S; De Aragão, Nádia M

    2013-09-01

    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.

  15. 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.

  16. Intensification of extraction of curcumin from Curcuma amada using ultrasound assisted approach: Effect of different operating parameters.

    Science.gov (United States)

    Shirsath, S R; Sable, S S; Gaikwad, S G; Sonawane, S H; Saini, D R; Gogate, P R

    2017-09-01

    Curcumin, a dietary phytochemical, has been extracted from rhizomes of Curcuma amada using ultrasound assisted extraction (UAE) and the results compared with the conventional extraction approach to establish the process intensification benefits. The effect of operating parameters such as type of solvent, extraction time, extraction temperature, solid to solvent ratio, particle size and ultrasonic power on the extraction yield have been investigated in details for the approach UAE. The maximum extraction yield as 72% was obtained in 1h under optimized conditions of 35°C temperature, solid to solvent ratio of 1:25, particle size of 0.09mm, ultrasonic power of 250W and ultrasound frequency of 22kHz with ethanol as the solvent. The obtained yield was significantly higher as compared to the batch extraction where only about 62% yield was achieved in 8h of treatment. Peleg's model was used to describe the kinetics of UAE and the model showed a good agreement with the experimental results. Overall, ultrasound has been established to be a green process for extraction of curcumin with benefits of reduction in time as compared to batch extraction and the operating temperature as compared to Soxhlet extraction. Copyright © 2017. Published by Elsevier B.V.

  17. Ultrasound-assisted rapid extraction and kinetic modelling of influential factors: Extraction of camptothecin from Nothapodytes nimmoniana plant.

    Science.gov (United States)

    Patil, Dhiraj M; Akamanchi, Krishnacharya G

    2017-07-01

    Ultrasound-assisted extraction (UAE) of commercially important natural product camptothecin (CPT) from Nothapodytes nimmoniana plant has been investigated. The influences of process factors such as electric acoustic intensity, solid to liquid ratio, duty cycle, temperature and particle size on the maximum extraction yield and kinetic mechanisms of the entire extraction process have been investigated. The kinetics results showed that increasing the intensity, duty cycle, solid to liquid ratio and decreasing the particle size lead to substantial increase in extraction yields compared to classical stirring extraction. Different kinetic models were applied to fit the experimental data. The second order rate model appears to be the best. The extraction rate constant, initial extraction rate and the equilibrium concentration for all experimental conditions have been calculated. SEM analysis of spent plant material clearly showed hollow openings on cell structure, which could be directly correlated to explosive disruption by the action of ultrasound waves. Overall 1.7-fold increase in extraction yields of CPT (0.32% w/w) and decrease in time from 6h to 18min was observed over the stirring method. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Effects of ultrasound-assisted α-amylase degradation treatment with multiple modes on the extraction of rice protein.

    Science.gov (United States)

    Yang, Xue; Li, Yunliang; Li, Suyun; Oladejo, Ayobami Olayemi; Wang, Yucheng; Huang, Shanfen; Zhou, Cunshan; Ye, Xiaofei; Ma, Haile; Duan, Yuqing

    2018-01-01

    The effects of ultrasound-assisted α-amylase degradation (UAD) treatment with multiple modes on the extraction of rice protein (RP) from rice dreg powder were studied. The results showed that UAD treatment increased protein extraction rate significantly (pextraction rate compared to that of simultaneous or single frequency ultrasound treatment. The highest protein extraction rate was obtained under 20/35kHz of sequential frequency UAD treatment with the protein extraction rate of 89.58% and protein purity of 92.99%. The test and analysis of fourier transform infrared spectroscopy, ultraviolet-visible spectroscopy, starch content, non-protein nitrogen content, SH and SS content, surface hydrophobicity, amino acids content and proteins characteristics were studied to reveal the mechanism of UAD on the protein extraction effect. After treated with UAD, the starch-protein agglomerates disintegrated completely, moreover, protein advanced structure was changed to some extent and the disulfide bond was partially broken, but the main chain structure (peptide chain), specificity of protein and amino acid composition were not obviously changed. Consequently, the structure modified RP extracted by UAD treatment presented higher solubility, emulsifying activity and foaming capacity, which was beneficial for the application of RP. In conclusion, UAD treatment is an effective method for maximizing extraction rate, purity and modifying properties of extracted protein. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Optimization of Ultrasound-Assisted Extraction of phenolic compounds and anthocyanins from blueberry (Vaccinium ashei) wine pomace.

    Science.gov (United States)

    He, Bo; Zhang, Ling-Li; Yue, Xue-Yang; Liang, Jin; Jiang, Jun; Gao, Xue-Ling; Yue, Peng-Xiang

    2016-08-01

    Ultrasound-Assisted Extraction (UAE) of total anthocyanins (TA) and phenolics (TP) from Blueberry Wine Pomace (BWP) was optimized using Response Surface Methodology (RSM). A Box-Behnken design was used to predict that the optimized conditions were an extraction temperature of 61.03°C, a liquid-solid ratio of 21.70mL/g and a sonication time of 23.67min. Using the modeled optimized conditions, the predicted and experimental yields of TA and TP were within a 2% difference. The yields of TA and TP obtained through the optimized UAE method were higher than those using a Conventional Solvent Extraction (CSE) method. Seven anthocyanins, namely delphinidin-3-O-glucoside, delphindin-3-O-arabinoside, petunidin-3-O-glucoside, cyanidin-3-O-arabinoside, cyanidin-3-O-glucoside, malvidin-3-O-glucoside and malvidin-3-O-arabinoside, were found in the BWP extract from both the UAE and CSE methods. Copyright © 2016 Elsevier Ltd. All rights reserved.

  20. Optimization of Ultrasound-assisted Extraction Procedure to Determine Astaxanthin in Xanthophyllomyces dendrorhous by Box-Behnken Designn

    Directory of Open Access Journals (Sweden)

    Wei Wu

    2013-11-01

    Full Text Available An ultrasonic-assisted extraction method has been developed for the effective extraction of astaxanthin from Xanthophyllomyces dendrorhous. Single-factor experiment design was employed to optimize the disruption temperature, disruption time, ethanol concentration, extraction time. The ethanol concentration was 60% ethanol in ethyl lactate and temperature for disrupting (40-60°C, time for disrupting extraction time (15-35 min, extraction time (20-40 min were used for further optimization of extraction conditions. The optimal conditions for the ultrasound-assisted extraction of astaxanthin were determined using Response Surface Methodology (RSM by Box-Behnken design. The optimal extraction conditions were that the yeast was disrupted at 49.08°C for 26.09 min under ultrasound irradiation of 200 W and then extracted for 32.43 min. Under optimal conditions, the astaxanthin content was 1472.85±43.64 &mug/g DW. This study introduces a simple, green and highly efficient method for extraction of astaxanthin fromX. dendrorhous

  1. Integrated downstream processing of lactoperoxidase from milk whey involving aqueous two-phase extraction and ultrasound-assisted ultrafiltration.

    Science.gov (United States)

    Nandini, K E; Rastogi, Navin K

    2011-01-01

    The present work involves the adoption of an integrated approach for the purification of lactoperoxidase from milk whey by coupling aqueous two-phase extraction (ATPE) with ultrasound-assisted ultrafiltration. The effect of system parameters of ATPE such as type of phase system, polyethylene glycol (PEG) molecular mass, system pH, tie line length and phase volume ratio was evaluated so as to obtain differential partitioning of contaminant proteins and lactoperoxidase in top and bottom phases, respectively. PEG 6000-potassium phosphate system was found to be suitable for the maximum activity recovery of lactoperoxidase 150.70% leading to 2.31-fold purity. Further, concentration and purification of enzyme was attempted using ultrafiltration. The activity recovery and purification factor achieved after ultrafiltration were 149.85% and 3.53-fold, respectively. To optimise productivity and cost-effectiveness of integrated process, influence of ultrasound for the enhancement of permeate flux during ultrafiltration was also investigated. Intermittent use of ultrasound along with stirring (2 min acoustic and 2 min stirring) resulted in increased permeate flux from 0.94 to 2.18 l/m(2) h in comparison to the ultrafiltration without ultrasound. The use of ultrasound during ultrafiltration resulted in increase in flux, but there was no significant change in activity recovery and purification factor. The integrated approach involving ATPE and ultrafiltration may prove to be a feasible method for the downstream processing of lactoperoxidase from milk whey.

  2. 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.

  3. The ultrasound-assisted extraction and identification of antifungal substances from B. amyloliquefaciens strain NJN-6 suppressing Fusarium oxysporum.

    Science.gov (United States)

    Yuan, Jun; Raza, Waseem; Huang, Qiwei; Shen, Qirong

    2012-12-01

    The primary mechanism underlying antagonism among microorganisms is the production of antagonistic substances called antibiotics that inhibit the growth of pathogens. In this study, the antagonistic substances produced by the Bacillus amyloliquefaciens strain NJN-6 that had antifungal activity against Fusarium oxysporum were extracted and identified. The active antifungal substance was extracted from dried leavening with ultrasound-assisted extraction (UAE), using n -butanol as the extractant. HPLC/ESI-MS was performed to investigate the components of the extracts. The results of the study showed that the antimicrobial substances consisted of three homologues of the iturin A family with molecular weights of 1043, 1057 and 1071 Da and of two homologues of the fengycin family with molecular weights of 1477 and 1491 Da. The effects of ultrasonic treatment time, extraction time and extractant volume, three major methodological parameters, were also studied to determine the optimal conditions for extraction. Compared with traditional extraction techniques, UAE is a simple, cheap and environmentally friendly method that represents a new option for the isolation and identification of lipopeptides and other active compounds. These antifungal substances extracted and identified from Bacillus amyloliquefaciens NJN-6 will help us to understand its biocontrol mechanism against Fusarium oxysporum.

  4. 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.

  5. Comparison of Ultrasound-assisted Extraction and Dynamic Maceration Over Content of Tagitinin C obtained from Tithonia diversifolia (Hemsl.) A. Gray Leaves Using Factorial Design.

    Science.gov (United States)

    Silva, Aline M R; Ferreira, Nayara L O; Oliveira, Anselmo E; Borges, Leonardo L; Conceição, Edemilson C

    2017-01-01

    Tithonia diversifolia belongs to the Asteraceae family. The leaves of T. diversifolia have been studied lately because of the presence of tagitinin C. Looking for an easy and inexpensive method to extract tagitinin C from T. diversifolia leaves, this work aims to conduct a screening to evaluate the influence of different experimental factors using the dynamic maceration and ultrasound-assisted extraction methods with 2(3) factorial design based on response surface methodology in enhancing this chemical marker extraction. The experimental factors were: extraction time (ET) of 30 and 60 minutes, solid: liquid ratio (SLR) of 5 and 10 grams/grams and ethanolic strength (ES) 48 and 96% (w/w). The experiments were done tripled. The content of tagitinin C in each produced extract was quantified by HPLC method. The highest concentrations of tagitinin C obtained under the experimental design were 0.53 mg/mL and 0.71 mg/mL, respectively for dynamic maceration (DM) and ultrasound-assisted extraction (UAE) from Tithonia diversifolia powdered leaves. For the UAE method, the main parameter for higher contents of tagitinin C was the solid: liquid ratio, followed by the ethanolic strength, and the extraction time was not significant for this method. As for the DM method, all the parameters (SLR, ES, and ET) were significant for a higher content of tagitinin C. Based on the obtained results, it was revealed that the ultrasound-assisted extraction was more effective than dynamic maceration for tagitinin C extraction from T. diversifolia powdered leaves. Tithonia diversifolia leaves possess tagitinin C, a sesquiterpene lactone, as an important secondary metabolite with several biological activities, such as antimalarial, gastroprotective, chemotherapeutic adjuvants, and toxic activities.Ultrasound-assisted extraction was more effective to obtain higher levels of tagitinin C when compared with dynamic maceration extraction.Factorial design can be employed as a screening tool to find

  6. 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.

  7. Ultrasound-assisted extraction of β-d-glucan from hull-less barley: Assessment of physicochemical and functional properties.

    Science.gov (United States)

    Hematian Sourki, Abdollah; Koocheki, Arash; Elahi, Mohammad

    2017-02-01

    The present study was carried out to investigate the effect of ultrasound-assisted extraction (UAE) method on physicochemical and molecular properties of hull-less barley β-d-glucan. With increasing sonication time, β-d-glucan flow behavior index (n) and its extraction yield significantly increased while its consistency coefficient and lightness decreased. Sonication time had no significant effect on β-d-glucan purity, emulsion and foam stabilizing effect and colour. Increasing pH from 5 to 9 significantly enhanced extraction yield, purity, consistency coefficient (k), emulsion stabilizing effect and yellowness of the final product. At higher pHs, flow behavior index (n) and redness and yellowness decreased. With increasing the amplitude, extracted β-d-glucan flow behavior index (n), redness significantly increased. In contrast, β-d-glucan purity, emulsion stability, consistency coefficient (k) and yellowness decreased as a result of increase in sound amplitude. However, sound amplitude had no significant effect on β-d-glucan lightness. Models presented in this study were highly significant and the correlation coefficient could be used for optimization of β-d-glucan extraction from hull-less barley. Considering the importance and desirability of the response variables, the best results were obtained when the sonication time, amplitude and pH were 4.8min, 50% and 9, respectively. β-d-Glucans extracted by UAE had lower average molecular weight compared to those extracted by water extraction method. There was no difference between the chemical structures of β-d-glucans extracted by UAE and conventional method. This means that short time ultrasonic extraction had no effect on chemical structure of β-d-glucan. These results indicate that UAE method was a very effective tool for extraction of β-d-glucan as a potential hydrocolloid agent for food industries.

  8. Spectrofluorimetric determination of melatonin in kernels of four different Pistacia varieties after ultrasound-assisted solid-liquid extraction

    Science.gov (United States)

    Oladi, Elham; Mohamadi, Maryam; Shamspur, Tayebeh; Mostafavi, Ali

    2014-11-01

    Melatonin is normally consumed to regulate the body's biological cycle. However it also has therapeutic properties, such as anti-tumor, anti-aging and protects the immune system. There are some reports on the presence of melatonin in edible kernels such as walnuts, but the extraction of melatonin from pistachio kernels is reported here for the first time. For this, the methanolic extract of pistachio kernels was exposed to gas chromatography/mass spectrometry analysis which confirmed the presence of melatonin. A fluorescence-based method was applied for the determination of melatonin in different extracts. When excited at λ = 275 nm, the fluorescence emission intensity of melatonin was measured at λ = 366 nm. Ultrasound-assisted solid-liquid extraction was used for the extraction of melatonin from pistachio kernels prior to fluorimetric determination. To achieve the highest extraction recovery, the main parameters affecting the extraction efficiency such as extracting solvent type and volume, temperature, sonication time and pH were evaluated. Under the optimized conditions, a linear dependence of fluorescence intensity on melatonin concentration was observed in the range of 0.0040-0.160 μg mL-1, with a detection limit of 0.0036 μg mL-1. This method was applied successfully for measuring and comparing the melatonin content in the kernels of four different varieties of Pistacia including Ahmad Aghaei, Akbari, Kalle Qouchi and Fandoghi. In addition, the results obtained were compared with those obtained using GC/MS. A good agreement was observed indicating the reliability of the proposed method.

  9. 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.

  10. Shadow-casted ultrathin surface coatings of titanium and titanium/silicon oxide sol particles via ultrasound-assisted deposition.

    Science.gov (United States)

    Karahan, H Enis; Birer, Özgür; Karakuş, Kerem; Yıldırım, Cansu

    2016-07-01

    Ultrasound-assisted deposition (USAD) of sol nanoparticles enables the formation of uniform and inherently stable thin films. However, the technique still suffers in coating hard substrates and the use of fast-reacting sol-gel precursors still remains challenging. Here, we report on the deposition of ultrathin titanium and titanium/silicon hybrid oxide coatings using hydroxylated silicon wafers as a model hard substrate. We use acetic acid as the catalyst which also suppresses the reactivity of titanium tetraisopropoxide while increasing the reactivity of tetraethyl orthosilicate through chemical modifications. Taking the advantage of this peculiar behavior, we successfully prepared titanium and titanium/silicon hybrid oxide coatings by USAD. Varying the amount of acetic acid in the reaction media, we managed to modulate thickness and surface roughness of the coatings in nanoscale. Field-emission scanning electron microscopy and atomic force microscopy studies showed the formation of conformal coatings having nanoroughness. Quantitative chemical state maps obtained by x-ray photoelectron spectroscopy (XPS) suggested the formation of ultrathin (coatings and thickness measurements by rotating analyzer ellipsometry supported this observation. For the first time, XPS chemical maps revealed the transport effect of ultrasonic waves since coatings were directly cast on rectangular substrates as circular shadows of the horn with clear thickness gradient from the center to the edges. In addition to the progress made in coating hard substrates, employing fast-reacting precursors and achieving hybrid coatings; this report provides the first visual evidence on previously suggested "acceleration and smashing" mechanism as the main driving force of USAD.

  11. Ultrasound-assisted extraction of arabinogalactan and dihydroquercetin simultaneously from Larix gmelinii as a pretreatment for pulping and papermaking.

    Directory of Open Access Journals (Sweden)

    Chunhui Ma

    Full Text Available An ultrasound-assisted extraction (UAE method using ethanol was applied for extracting arabinogalactan (AG and dihydroquercetin (DHQ simultaneously from larch wood, as a pretreatment for pulping and papermaking. The extraction parameters were optimized by a Box-Behnken experimental design with the yields of AG and DHQ as the response values. Under optimum conditions (three extractions, each using 40% ethanol, for 50 min, 200 W ultrasound power and 1∶18 solid-liquid ratio, the yields of AG and DHQ were 183.4 and 36.76 mg/g, respectively. After UAE pretreated, the wood chips were used for Kraft pulping (KP and high boiling solvent pulping (HBSP. The pulping yield after pretreatment was higher than that of untreated (the pulping yields of untreated HBSP and KP were 42.37% and 39.60%, and the pulping yields of HBSP and KP after UAE-pretreated were 44.23% and 41.50% respectively, as indicated by a lower kappa number (77.91 and 27.30 for untreated HBSP and KP; 77.01 and 26.83 for UAE-pretreated HBSP and KP. Furthermore, the characteristics of paper produced from pretreated wood chips were superior to those from the untreated chips: the basis weight was lower (85.67 and 82.48 g·cm(-2 for paper from untreated KP and HBSP; 79.94 and 80.25 g·cm(-2 for paper from UAE-pretreated KP and HBSP, and the tensile strengths, tearing strengths, bursting strengths, and folding strengths were higher than these of paper after UAE-pretreated, respectively.

  12. Chromolithic method development, validation and system suitability analysis of ultra-sound assisted extraction of glycyrrhizic acid and glycyrrhetinic acid from Glycyrrhiza glabra.

    Science.gov (United States)

    Gupta, Suphla; Sharma, Rajni; Pandotra, Pankaj; Jaglan, Sundeep; Gupta, Ajai Prakash

    2012-08-01

    An ultrasound-assisted extraction and chromolithic LC method was developed for simultaneous determination of glycyrrhizic acid (GA) and glycyrrhetinic acid (GL) from the root extract of Glycyrrhizza glabra using RPLC-PDA. The developed method was validated according to the International Conference on Harmonisation. The method exhibited good linearity (r2 > 0.9989) with high precision and achieved good accuracies between 97.5 to 101.3% of quantitative results. The method is more sensitive and faster (resolved within ten minutes) than the earlier developed methods using normal LC columns.

  13. 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

  14. Nanoparticles in ionic liquids: interactions and organization.

    Science.gov (United States)

    He, Zhiqi; Alexandridis, Paschalis

    2015-07-28

    Ionic liquids (ILs), defined as low-melting organic salts, are a novel class of compounds with unique properties and a combinatorially great chemical diversity. Ionic liquids are utilized as synthesis and dispersion media for nanoparticles as well as for surface functionalization. Ionic liquid and nanoparticle hybrid systems are governed by a combined effect of several intermolecular interactions between their constituents. For each interaction, including van der Waals, electrostatic, structural, solvophobic, steric, and hydrogen bonding, the characterization and quantitative calculation methods together with factors affecting these interactions are reviewed here. Various self-organized structures based on nanoparticles in ionic liquids are generated as a result of a balance of these intermolecular interactions. These structures, including colloidal glasses and gels, lyotropic liquid crystals, nanoparticle-stabilized ionic liquid-containing emulsions, ionic liquid surface-functionalized nanoparticles, and nanoscale ionic materials, possess properties of both ionic liquids and nanoparticles, which render them useful as novel materials especially in electrochemical and catalysis applications. This review of the interactions within nanoparticle dispersions in ionic liquids and of the structure of nanoparticle and ionic liquid hybrids provides guidance on the rational design of novel ionic liquid-based materials, enabling applications in broad areas.

  15. Ultrasound-Assisted Freezing

    Science.gov (United States)

    Delgado, A. E.; Sun, Da-Wen

    Freezing is a well-known preservation method widely used in the food industry. The advantages of freezing are to a certain degree counterbalanced by the risk of damage caused by the formation and size of ice crystals. Over recent years new approaches have been developed to improve and control the crystallization process, and among these approaches sonocrystallization has proved to be very useful, since it can enhance both the nucleation rate and the crystal growth rate. Although ultrasound has been successfully used for many years in the evaluation of various aspects of foods and in medical applications, the use of power ultrasound to directly improve processes and products is less popular in food manufacturing. Foodstuffs are very complex materials, and research is needed in order to define the specific sound parameters that aid the freezing process and that can later be used for the scale-up and production of commercial frozen food products.

  16. Ultrasound-assisted dispersive liquid-liquid microextraction combined with high-performance liquid chromatography-fluorescence detection for sensitive determination of biogenic amines in rice wine samples.

    Science.gov (United States)

    Huang, Ke-Jing; Wei, Cai-Yun; Liu, Wei-Li; Xie, Wan-Zhen; Zhang, Jun-Feng; Wang, Wei

    2009-09-18

    Ultrasound-assisted dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography-fluorescence detection was used for the extraction and determination of three biogenic amines including octopamine, tyramine and phenethylamine in rice wine samples. Fluorescence probe 2,6-dimethyl-4-quinolinecarboxylic acid N-hydroxysuccinimide ester was applied for derivatization of biogenic amines. Acetonitrile and 1-octanol were used as disperser solvent and extraction solvent, respectively. Extraction conditions including the type of extraction solvent, the volume of extraction solvent, ultrasonication time and centrifuging time were optimized. After extraction and centrifuging, analyte was injected rapidly into high-performance liquid chromatography and then detected with fluorescence. The calibration graph of the proposed method was linear in the range of 5-500 microg mL(-1) (octopamine and tyramine) and 0.025-2.5 microg mL(-1) (phenethylamine). The relative standard deviations were 2.4-3.2% (n=6) and the limits of detection were in the range of 0.02-5 ng mL(-1). The method was applied to analyze the rice wine samples and spiked recoveries in the range of 95.42-104.56% were obtained. The results showed that ultrasound-assisted dispersive liquid-liquid microextraction was a very simple, rapid, sensitive and efficient analytical method for the determination of trace amount of biogenic amines.

  17. Ultrasound-assisted emulsification microextraction for the determination of ephedrines in human urine by capillary electrophoresis with direct injection. Comparison with dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Alshana, Usama; Göğer, Nilgün G; Ertaş, Nusret

    2012-08-01

    Ultrasound-assisted emulsification microextraction and dispersive liquid-liquid microextraction were compared for extraction of ephedrine, norephedrine, and pseudoephedrine from human urine samples prior to their determination by capillary electrophoresis. Formation of a microemulsion of the organic extract with an aqueous solution (at pH 3.2) containing 10% methanol facilitated the direct injection of the final extract into the capillary. Influential parameters affecting extraction efficiency were systematically studied and optimized. In order to enhance the sensitivity further, field-amplified sample injection was applied. Under optimum extraction and stacking conditions, enrichment factors of up to 140 and 1750 as compared to conventional capillary zone electrophoresis were obtained resulting in limits of detection of 12-33 μg/L and 1.0-2.8 μg/L with dispersive liquid-liquid microextraction and ultrasound-assisted emulsification microextraction when combined with field-amplified sample injection. Calibration graphs showed good linearity for urine samples by both methods with coefficients of determination higher than 0.9973 and percent relative standard deviations of the analyses in the range of 3.4-8.2% for (n = 5). The results showed that the use of ultrasound to assist microextraction provided higher extraction efficiencies than disperser solvents, regarding the hydrophilic nature of the investigated analytes.

  18. 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.

  19. AgI/TiO2 nanocomposites: ultrasound-assisted preparation, visible-light induced photocatalytic degradation of methyl orange and antibacterial activity.

    Science.gov (United States)

    Xue, Bin; Sun, Tao; Wu, Ji-Kui; Mao, Fang; Yang, Wei

    2015-01-01

    AgI/TiO2 nanocomposites were prepared by an ultrasound-assisted precipitation process and subsequent low-temperature (350°C) calcination. The crystal phase, morphology and optical properties of the AgI/TiO2 nanocomposites were characterized by X-ray diffraction, transmission electron microscopy and UV-vis absorption spectroscopy. After calcination, the crystallite size of AgI nanoparticles in the AgI/TiO2 nanocomposites decreased, and visible light absorption intensity of the AgI/TiO2 nanocomposites was significantly enhanced. The AgI/TiO2 nanocomposites after calcination exhibited the superior photocatalytic activity for methyl orange degradation and killing of Escherichia coli under visible light irradiation. The improvement of photocatalytic activity could be attributed to two reasons, namely, reduced crystallite size and enhanced visible light absorption of AgI nanoparticles in calcined AgI/TiO2 nanocomposites. The trapping experiments demonstrated that superoxide radical (O2(-)) and holes (h(+)) were the main reactive species for the photodegradation of methyl orange under visible light irradiation. The ultrasound-assisted preparation approach is efficient and facile, which promotes large-scale production and application of AgI/TiO2 nanocomposites in photocatalytic degradation of organic pollutants, disinfection and other fields.

  20. 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.

  1. Optimisation of ultrasound-assisted extraction of oil from papaya seed by response surface methodology: oil recovery, radical scavenging antioxidant activity, and oxidation stability.

    Science.gov (United States)

    Samaram, Shadi; Mirhosseini, Hamed; Tan, Chin Ping; Ghazali, Hasanah Mohd; Bordbar, Sara; Serjouie, Alireza

    2015-04-01

    The present study aimed to investigate the effects of ultrasound-assisted extraction (UAE) condition on the yield, antioxidant activity and stability of the oil from papaya seed. The studied ultrasound variables were time, temperature, ultrasound power and solvent to sample ratio. The main goal was to optimise UAE condition providing the highest recovery of papaya seed oil with the most desirable antioxidant activity and stability. The interaction of ultrasound variables had the most and least significant effects on the antioxidant activity and stability, respectively. Ultrasound-assisted extraction provided a relatively high oil recovery (∼ 73%) from papaya seed. The strongest antioxidant activity was achieved by the extraction at the elevated temperature using low solvent to sample ratio. The optimum ultrasound extraction was set at the elevated temperature (62.5 °C) for 38.5 min at high ultrasound power (700 W) using medium solvent to sample ratio (∼ 7:1 v/w). The optimum point was practically validated. Copyright © 2014. Published by Elsevier Ltd.

  2. Phenols and antioxidant activity in vitro and in vivo of aqueous extracts obtained by ultrasound-assisted extraction from artichoke by-products.

    Science.gov (United States)

    Punzi, Rossana; Paradiso, Annalisa; Fasciano, Cristina; Trani, Antonio; Faccia, Michele; de Pinto, Maria Concetta; Gambacorta, Giuseppe

    2014-09-01

    Artichoke by-products are rich in phenolic compounds although they represent a waste for the food industry. This paper examines the application of ultrasound-assisted extraction (UAE) for obtaining organic solvent-free extracts rich in nutraceuticals from artichoke scraps. Application of ultrasounds for 60 minutes on test samples, using water as a solvent, improved recovery of phenolic substances compared with untreated samples. Among the phenols detected by high performance liquid chromatography, 5-O-caffeoylquinic and 1,5-di-O-caffeoylquinic acids were identified. In vivo treatments of tobacco BY-2 cells with ultrasonic extracts consistently enhanced their antioxidant power, making the cells more resistant to heat stress. UAE applied to artichoke by-products, using water as a solvent, appears to be a powerful eco-friendly technique that can provide extracts rich in nutraceuticals and turn waste products into resources. The extracts could be advantageously utilized in the food industry to produce functional foods.

  3. Synthesis of Bifunctional Fe3O4@SiO2-Ag Magnetic-Plasmonic Nanoparticles by an Ultrasound Assisted Chemical Method

    Science.gov (United States)

    Chu, Dung Tien; Sai, Doanh Cong; Luu, Quynh Manh; Tran, Hong Thi; Quach, Truong Duy; Kim, Dong Hyun; Nguyen, Nam Hoang

    2017-03-01

    Bifunctional magnetic-plasmonic nanoparticles (NPs)—Fe3O4@SiO2-Ag were successfully synthesized by an ultrasound assisted chemical method. Silver ions were absorbed and then reduced by sodium borohydride on the surface of 3-aminopropyltriethoxysilane (APTES) functionalized silica-coated magnetic NPs, then they were reduced under the influence of a 200 W ultrasonic wave for 60 min. When the amount of precursor silver ions increased, the relative intensity of diffraction peaks of silver crystals in all samples increased with the atomic ratio of silver/iron increasing from 0.208 to 0.455 and saturation magnetization (M s) decreasing from 44.68 emu/g to 34.74 emu/g. The NPs have superparamagnetic properties and strong surface plasmon absorption at 420 nm, which make these particles promising for biomedical applications.

  4. MWCNT-Based Ag2S-TiO2 Nanocomposites Photocatalyst: Ultrasound-Assisted Synthesis, Characterization, and Enhanced Catalytic Efficiency

    Directory of Open Access Journals (Sweden)

    Lei Zhu

    2012-01-01

    Full Text Available Multiwalled carbon nanotube based nanoscale Ag2S and TiO2 composites have successfully synthesized via a facile ultrasound-assisted method. The nanocomposites were characterized by Fourier transform infrared (FT-IR spectroscopy, UV-vis absorption spectra, BET surface area measurements, X-ray diffraction (XRD, and transmission electron microscopy (TEM. The Ag2S-TiO2/CNT nanocomposites exhibited much higher photocatalytic activity than pure TiO2 for the degradation of Rhodamine B (Rh.B under UV and visible light. The improved photocatalytic activities may be attributed to increased adsorbability of Rh.B molecules and increased charge transfer rate in the presence of a one-dimensional MWCNT network.

  5. Molecularly imprinted solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction for the determination of four Sudan dyes in sausage samples.

    Science.gov (United States)

    Yan, Hongyuan; Qiao, Jindong; Wang, Hui; Yang, Gengliang; Row, Kyung Ho

    2011-06-21

    A simple and highly selective molecularly imprinted solid-phase extraction (MISPE) combined with ultrasound-assisted dispersive liquid-liquid microextraction (DLLME) was developed for the determination of four Sudan dye (I, II, III, and IV) residues in sausage products. The novel molecularly imprinted microspheres (MIMs) synthesized by aqueous suspension polymerization using phenylamine-naphthol as the dummy template show high affinity to the four Sudan dyes and were applied as selective sorbents of MISPE-DLLME to overcome the drawbacks of template leakage in quantitative analysis. Good linearity was obtained in a range of 0.005-2.0 μg g(-1) and the average recoveries of the four Sudan dyes at three spiked levels ranged from 86.3 to 107.5%. The MISPE-DLLME-HPLC protocol significantly improved the purification and enrichment of the analytes and eliminated the template leakage of the conventional MISPE on quantitative analysis.

  6. A simple and fast ultrasound-assisted extraction procedure for Fe and Zn determination in milk-based infant formulas using flame atomic absorption spectrometry (FAAS).

    Science.gov (United States)

    Machado, Ignacio; Bergmann, Gabriela; Pistón, Mariela

    2016-03-01

    A simple and fast ultrasound-assisted procedure for the determination of iron and zinc in infant formulas is presented. The analytical determinations were carried out by flame atomic absorption spectrometry. Multivariate experiments were performed for optimization; in addition, a comparative study was carried out using two ultrasonic devices. A method using an ultrasonic bath was selected because several samples can be prepared simultaneously, and there is less contamination risk. Analytical precision (sr(%)) was 3.3% and 4.1% for iron and zinc, respectively. Trueness was assessed using a reference material and by comparison of the results obtained analyzing commercial samples using a reference method. The results were statistically equivalent to the certified values and in good agreement with those obtained using the reference method. The proposed method can be easily implemented in laboratories for routine analysis with the advantage of being rapid and in agreement with green chemistry.

  7. Development of a novel ultrasound-assisted alkali pretreatment strategy for the production of bioethanol and xylanases from chili post harvest residue.

    Science.gov (United States)

    Sindhu, Raveendran; Binod, Parameswaran; Mathew, Anil Kuruvilla; Abraham, Amith; Gnansounou, Edgard; Ummalyma, Sabeela Beevi; Thomas, Leya; Pandey, Ashok

    2017-10-01

    A novel ultrasound-assisted alkali pretreatment strategy was developed which could effectively remove lignin and hemicelluloses and improve the sugar yield from chili post harvest residue. Operational parameters that affect the pretreatment efficiency were studied and optimized. Inhibitor analysis of the hydrolyzate revealed that major fermentation inhibitors like furfural, 5-hydroxymethyl furfural as well as organic acids like citric acid, succinic acid and propionic acid were absent. Hence fermentation can be carried out without detoxification of the hydrolyzate. Changes in structural properties of the biomass were studied in relation to the pretreatment process using Scanning Electron Microscopy (SEM) and the changes in chemical composition were also monitored. The biomass pretreated with the optimized novel method could yield 0.428g/g of reducing sugars upon enzymatic hydrolysis. The hydrolyzate obtained by this novel pretreatment strategy was found to be suitable for bioethanol and xylanase production. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Influence of Accelerated Solvent Extraction and Ultrasound-Assisted Extraction on the Anthocyanin Profile of Different Vaccinium Species in the Context of Statistical Models for Authentication.

    Science.gov (United States)

    Heffels, Peter; Weber, Fabian; Schieber, Andreas

    2015-09-02

    Anthocyanins are frequently discussed as marker compounds for fruit product authenticity. Proper analysis including sample preparation for the determination of anthocyanin concentrations is crucial for the comparability of authenticity data. The present study determined the influence of accelerated solvent extraction (ASE) and ultrasound-assisted extraction (UAE), using two different solvent compositions on the anthocyanin profile of bilberries (Vaccinium myrtillus L.), lowbush blueberries (Vaccinium angustifolium Ait.), and American cranberries (Vaccinium macrocarpon Ait.). Besides differences in total anthocyanin concentrations in the extracts, significant deviations (p ≤ 0.05) in the individual anthocyanin concentration were observed, resulting in differing anthocyanin proportions. Linear discriminant analysis comparing the differences caused by the extraction method to the natural differences within a set of 26 bilberry and lowbush blueberry samples of different origins was conducted. It revealed that profile variations induced by the extraction methods are in a similar scale to profile variations as a result of geographic and climatic differences.

  9. Synthesis of Bifunctional Fe3O4@SiO2-Ag Magnetic-Plasmonic Nanoparticles by an Ultrasound Assisted Chemical Method

    Science.gov (United States)

    Chu, Dung Tien; Sai, Doanh Cong; Luu, Quynh Manh; Tran, Hong Thi; Quach, Truong Duy; Kim, Dong Hyun; Nguyen, Nam Hoang

    2017-06-01

    Bifunctional magnetic-plasmonic nanoparticles (NPs)—Fe3O4@SiO2-Ag were successfully synthesized by an ultrasound assisted chemical method. Silver ions were absorbed and then reduced by sodium borohydride on the surface of 3-aminopropyltriethoxysilane (APTES) functionalized silica-coated magnetic NPs, then they were reduced under the influence of a 200 W ultrasonic wave for 60 min. When the amount of precursor silver ions increased, the relative intensity of diffraction peaks of silver crystals in all samples increased with the atomic ratio of silver/iron increasing from 0.208 to 0.455 and saturation magnetization ( M s) decreasing from 44.68 emu/g to 34.74 emu/g. The NPs have superparamagnetic properties and strong surface plasmon absorption at 420 nm, which make these particles promising for biomedical applications.

  10. Impact of enzyme- and ultrasound-assisted extraction methods on biological properties of red, brown, and green seaweeds from the central west coast of Portugal.

    Science.gov (United States)

    Rodrigues, Dina; Sousa, Sérgio; Silva, Aline; Amorim, Manuela; Pereira, Leonel; Rocha-Santos, Teresa A P; Gomes, Ana M P; Duarte, Armando C; Freitas, Ana Cristina

    2015-04-01

    Seaweeds are an excellent source of bioactive compounds, and therefore the use of sustainable and food compatible extraction methods such as enzyme-assisted (EAE) and ultrasound-assisted extraction were applied on Sargassum muticum, Osmundea pinnatifida, and Codium tomentosum. Extracts were evaluated for proximate characterization and biological properties. Higher extraction yields were observed for C. tomentosum EAE (48-62%; p polysaccharide (44 ± 8 mgNa2SO4 acid/glyoph extract) contents characterized O. pinnatifida extracts. A higher effect on hydroxyl-radical scavenging activity (35-50%) was observed for all extracts, whereas S. muticum Alcalase and C. tomentosum Cellulase extracts exhibited higher prebiotic activity than fructooligosaccharides. O. pinnatifida and C. tomentosum EAE showed inhibitory potential against α-glucosidase (38-49%).

  11. 3D rod-like copper oxide with nanowire hierarchical structure: Ultrasound assisted synthesis from Cu2(OH)3NO3 precursor, optical properties and formation mechanism

    Science.gov (United States)

    Ba, Ningning; Zhu, Lianjie; Li, Hongbin; Zhang, Guangzhi; Li, Jianfa; Sun, Jingfeng

    2016-03-01

    3-dimensional (3D) rod-like CuO with nanowire hierarchical structure has been synthesized successfully by a facile ultrasound assisted method combined with thermal conversion, using rouaite Cu2(OH)3NO3 as the precursor. The product was characterized by XRD, SEM, TEM, HRTEM and FT-IR spectrum. Its optical properties were studied by means of UV-Vis diffuse reflectance absorption spectroscopy and photoluminescence (PL) spectrum. Series of control experiments have been performed to explore influencing factors to the product morphologies and a possible formation mechanism has been proposed. The results show that each CuO rod assembled by tens of nanowires is 200-300 nm in diameter and about 1000 nm in length. Each nanowire contains many interconnected nanoparticles with sizes of about 15 nm. Particularly, ultrasound processing was found beneficial to the formation of the 3D rod-like CuO with nanowire hierarchical structure.

  12. Optimization of ultrasound-assisted extraction of total monomeric anthocyanin (TMA) and total phenolic content (TPC) from eggplant (Solanum melongena L.) peel.

    Science.gov (United States)

    Dranca, Florina; Oroian, Mircea

    2016-07-01

    The present study describes the extraction of total monomeric anthocyanin (TMA) and total phenolic content (TPC) from eggplant peel using ultrasonic treatments and methanol and 2-propanol as extraction solvents. The extraction yields were optimized by varying the solvent concentration, ultrasonic frequency, temperature and time of ultrasonic treatment. Box-Behnken design was used to investigate the effect of process variables on the ultrasound-assisted extraction. The results showed that for TPC extraction the optimal condition were obtained with a methanol concentration of 76.6%, 33.88 kHz ultrasonic frequency, a temperature of 69.4 °C and 57.5 min extraction time. For TMA the optimal condition were the following: 54.4% methanol concentration, 37 kHz, 55.1 °C and process time of 44.85 min. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Baseline-Corrected Second-Order Derivative Electroanalysis Combined With Ultrasound-Assisted Liquid-Liquid Microextraction: Simultaneous Quantification of Fluoroquinolones at Low Levels.

    Science.gov (United States)

    de Oliveira, Luiz Henrique; Trindade, Magno Aparecido Gonçalves

    2016-06-21

    A baseline-corrected second-order derivative procedure and a miniaturized sample preparation based on low-density solvent and ultrasound-assisted liquid-liquid microextraction (LDS-UA-LLME) was combined to provide the simultaneous electroanalysis of three fluoroquinolones (FQ) as emerging contaminants (ECs). The enhanced mathematical processing provided the best separation with an accurate measurement of the overlapping peaks during the simultaneous electro-oxidation of target FQs that were directly dropped on the surface of carbon nanofiber-modified screen-printed electrodes. The adapted LDS-UA-LLME protocol was the key step involved in the sample preparation, which preconcentrate target analytes from diluted tap water samples with an enrichment factor of around 80×, allowing their quantification at trace levels. This combined feature demonstrated the unique application of an electroanalytical technique for the simultaneous electroanalysis of three FQs in spiked tap water samples, with recovery values remarkably close to 100%.

  14. Ultrasound-assisted extraction methodology as a tool to improve the antioxidant properties of herbal drug Xiao-chia-hu-tang.

    Science.gov (United States)

    Liu, Chu-Ting; Wu, Ching-Yi; Weng, Yih-Ming; Tseng, Chin-Yin

    2005-06-03

    Xiao-chai-hu-tang (XCHT) is an important Chinese herbal prescription for curing many types of liver diseases. The contents of bioactive constituents (saikosaponins a, c and d, baicalin, baicalein, and glycyrrhizic acid), and antioxidant properties of XCHT extracts prepared with ultrasound-assisted (US) extraction in combination with ethanol (up to 95%) as extraction modifier were studied. The results showed that the US extraction significantly increased the bioactive constituents concentrations and antioxidant properties of XCHT extracts when compared with the XCHT prepared with traditional boiling-water extraction. Among the XCHT extracts made with US extraction, the sample prepared with 95% ethanol showed the highest bioactive constituent concentrations and the best antioxidant functionalities. The results suggest that US extraction of XCHT is feasible to replace the traditional time-consuming and low efficiency preparation procedure in the future modernized and commercialized manufacture of this highly valuable Chinese herbal medicine.

  15. Development and characterization of a layer by layer ultrasound assisted spray deposition process for thin polymer films

    Science.gov (United States)

    Balakrishnan, Anandh

    An Ultrasound assisted Atomization (UA) system has been developed and investigated to synthesize ˜20microm polyurethane thin films with uniform, repeatable thickness and microstructure. The UA system comprised a 20 kHz atomizer probe mounted on 750 W/cm2 transducer, a heated glass chamber and a rotating substrate. The rationale for the work has been built through a careful Design of Experiments (DoE) that sought to answer questions regarding the process-microstructure relationships from both the spray and material points of view. The independent variables chosen were the polymer solution weight percentage (0.2%, 2%, and 4%), power amplitude (energy) percentage supplied to the nozzle (23%, 29%, 37%, and 46%),the temperature of deposition (45°C, 80°C) and flow rate (50microL/min, 150microL/min). The research questions focused on influence of the process parameters on the microstructure and properties of the film. One of the problems involved fixing the trajectory of the spray and also making use of the droplet surfaces created by the spray. To achieve this, a simple air-draft attachment was devised and the influence of the same was evaluated through process and film characterization experiments. A mechanism for the draft has been schematically provided. The use of such a draft to fabricate thin polymer films via ultrasound atomization has not been achieved before and represents a 'first step' in advancing this ultrasound technology. The primary findings of the work were that the film microstructure and properties were heavily influenced by the flow rate, energy of atomization, and test temperature. In addition, the droplet diameters seemed to be readily amenable to change for the 0.2 and 2% solutions and the use of the air-draft made the process feasible, repeatable and accurate. For the 4% solutions, viscosity seemed to stabilize the liquid solution film at the tip requiring larger energies of atomization. In all, relative to the 0.2% films the fracture strengths

  16. 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.

  17. Ultrasound-assisted phase-transfer catalysis: benzoylation of sodium 4-acetylphenoxide by dual-site phase-transfer catalyst in a tri-liquid system.

    Science.gov (United States)

    Yang, Hung-Ming; Chiu, Chun-Cheng

    2011-01-01

    A novel dual-site phase-transfer catalyst (PTC) was prepared and used to conduct the benzoylation of sodium 4-acetylphenoxide by ultrasound-assisted third-liquid phase-transfer catalysis. The catalyst 1,4-bis(tributylammoniomethyl)benzene dibromide (BTBAMBB) was synthesized from the reaction of p-xylylene dibromide and tributylamine in toluene at 70°C. The dual-site PTC was employed to form the third-liquid phase by extra addition of 0.04-0.05 mol of NaCl into 10 cm(3) of water. In the condition of 0.0425 mol of NaCl at 30°C, the catalytic intermediate in the third-liquid phase reached a maximum value. Almost 80% of the catalyst was transferred from the aqueous phase into the third-liquid phase. The distributions of the catalytic intermediate and dual-site PTC between phases and the kinetics of benzoylation of sodium 4-acetylphenoxide catalyzed by BTBAMBB with ultrasound irradiation were performed. The pseudo-first-order kinetic equation was applied to describe the overall reaction. Under ultrasound irradiation (28 kHz/300 W) in a batch reactor, the yield of product 4-acetylphenyl benzoate in the organic phase was 98.1% in 2 min at 30°C and 250 rpm with the apparent rate constant k(app) to be 0.0075 s(-1), which was 6 times faster than that without using ultrasound (yield=14.4%, k(app)=0.0013 s(-1)). The present study provides a green method to synthesize esters by ultrasound-assisted third-liquid phase-transfer catalysis.

  18. Fe(II)–Al(III) layered double hydroxides prepared by ultrasound-assisted co-precipitation method for the reduction of bromate

    Energy Technology Data Exchange (ETDEWEB)

    Zhong, Yu [College of Environmental Science and Engineering, Hunan University, Changsha 410082 (China); Key Laboratory of Environmental Biology and Pollution Control, Hunan University, Ministry of Education, Changsha 410082 (China); Yang, Qi, E-mail: yangqi@hnu.edu.cn [College of Environmental Science and Engineering, Hunan University, Changsha 410082 (China); Key Laboratory of Environmental Biology and Pollution Control, Hunan University, Ministry of Education, Changsha 410082 (China); Luo, Kun; Wu, Xiuqiong [College of Environmental Science and Engineering, Hunan University, Changsha 410082 (China); Key Laboratory of Environmental Biology and Pollution Control, Hunan University, Ministry of Education, Changsha 410082 (China); Li, Xiaoming, E-mail: xmli@hnu.edu.cn [College of Environmental Science and Engineering, Hunan University, Changsha 410082 (China); Key Laboratory of Environmental Biology and Pollution Control, Hunan University, Ministry of Education, Changsha 410082 (China); Liu, Yang [College of Environmental Science and Engineering, Hunan University, Changsha 410082 (China); Urban and Rural Garbage Disposal Technology Research Center, Hunan Province, Changsha 410082 (China); Tang, Wangwang; Zeng, Guangming; Peng, Bo [College of Environmental Science and Engineering, Hunan University, Changsha 410082 (China); Key Laboratory of Environmental Biology and Pollution Control, Hunan University, Ministry of Education, Changsha 410082 (China)

    2013-04-15

    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{sub 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{sup 2+} were the main mechanisms responsible for the bromate removal by Fe–Al LDHs.

  19. A rapid ultrasound-assisted thiourea extraction method for the determination of inorganic and methyl mercury in biological and environmental samples by CVAAS.

    Science.gov (United States)

    Krishna, M V Balarama; Ranjit, Manjusha; Karunasagar, D; Arunachalam, J

    2005-07-15

    A rapid ultrasound-assisted extraction procedure for the determination of total mercury, inorganic and methyl mercury (MM) in various environmental matrices (animal tissues, samples of plant origin and coal fly ash) has been developed. The mercury contents were estimated by cold vapour atomic absorption spectrometry (CVAAS). Inorganic mercury (IM) was determined using SnCl(2) as reducing agent whereas total mercury was determined after oxidation of methyl mercury through UV irradiation. Operational parameters such as extractant composition (HNO(3) and thiourea), sonication time and sonication amplitude found to be different for different matrices and were optimized using IAEA-350 (Fish homogenate), IM and MM loaded moss and NIST-1633b (Coal fly ash) to get quantitative extraction of total mercury. The method was further validated through the analysis of additional certified reference materials (RM): NRCC-DORM2 (Dogfish muscle), NRCC-DOLT1 (Dogfish liver) and IAEA-336 (Lichen). Quantitative recovery of total Hg was achieved using mixtures of 5% HNO(3) and 0.02% thiourea, 10% HNO(3) and 0.02% thiourea, 20% HNO(3) and 0.2% thiourea for fish tissues, plant matrices and coal fly ash samples, respectively. The results obtained were in close agreement with certified values with an overall precision in the range of 5-15%. The proposed ultrasound-assisted extraction procedure significantly reduces the time required for sample treatment for the extraction of Hg species. The extracted mercury species are very stable even after 24h of sonication. Closed microwave digestion was also used for comparison purposes. The proposed method was applied for the determination of Hg in field samples of lichens, mosses, coal fly ash and coal samples.

  20. 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.

  1. 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

  2. Forming nanoparticles of water-soluble ionic molecules and embedding them into polymer and glass substrates

    Directory of Open Access Journals (Sweden)

    Stella Kiel

    2012-03-01

    Full Text Available This work describes a general method for the preparation of salt nanoparticles (NPs made from an aqueous solution of ionic compounds (NaCl, CuSO4 and KI. These nanoparticles were created by the application of ultrasonic waves to the aqueous solutions of these salts. When the sonication was carried out in the presence of a glass microscope slide, a parylene-coated glass slide, or a silicon wafer the ionic NPs were embedded in these substrates by a one-step, ultrasound-assisted procedure. Optimization of the coating process resulted in homogeneous distributions of nanocrystals, 30 nm in size, on the surfaces of the substrates. The morphology and structure of each of the coatings were characterized by physical and chemical methods, such as X-ray diffraction (XRD, scanning electron microscopy (SEM, atomic force microscopy (AFM, Raman spectroscopy and X-ray photoelectron spectroscopy (XPS. After 24 h of leaching into water the nanoparticles of the inorganic salts were still present on the slides, and complete leaching of nanoparticles occurred only after 96 h. A mechanism of the ultrasound-assisted coating is proposed.

  3. 离子液体掺杂聚苯胺固相微萃取涂层的电沉积制备及其在芳香胺检测中的应用%Electrochemical Preparation of Polyaniline-Ionic Liquid Based Solid Phase Microextraction Coating and Its Application in Determination of Aromatic Amines

    Institute of Scientific and Technical Information of China (English)

    王妹丽; 王娟; 赵发琼; 曾百肇

    2011-01-01

    新型萃取材料及相关涂层制备技术是固相微萃取技术发展的重点.本研究在1-羟丙基-3-甲基咪唑-四氟硼酸盐([C3(OH)mim][BF4])和HNO3混合溶液中,通过电化学方法在铂(Pt)丝表面固定新型聚苯胺-离子液体(PANI-IL)涂层.电镜分析表明,离子液体存在时,PANI膜孔结构变均匀、比表面积增大.以芳香胺为模拟物,考察萃取头的顶空固相微萃取(HS SPME)性能.在优化条件下,5种芳香胺的检出限为0.04~0.12μg/L(SIN=3);线性范围为0.15~1000 μg/L.同一萃取头萃取5次的相对标准偏差(RSD)小于4.6%;不同萃取头的RSD则在2.4%~9.5%(n=3)之间.与自制聚苯胺(PANI/Pt)及商品化的聚丙烯酸酯(PA)萃取头相比,PANI-IL/Pt萃取头具有更高的萃取率.此外,PANI-IL涂层对苯类化合物亦有较高的萃取能力.萃取头使用120余次后,萃取性能无明显变化,表明萃取头的稳定性好、使用寿命长.%A novel solid phase microextraction coating of polyaniline-ionic liquid (PANI-IL) was prepared by electrodeposition on a Pt wire in aqueous solutions containing ionic liquid [C3 (OH) mim][BF4] and nitric acid. The resulted coating was more uniform and porous than PANI coating. Taking five aromatic amines as models, the performance of the PANI-IL/Pt fiber was explored. Under the optimized conditions, when they were determined by GC after headspace SPME with the PANI-IL/Pt, the detection limits were 0. 04 - 0. 12 μg/L (S/N = 3) and the linear ranges were 0. 15 -1000 μg/L. These aromatic amines were determined for five times using a PANI-IL/Pt fiber coupled with GC and the RSD of chromatographic peak areas were smaller than 4.6% ; the fiber to fiber RSD was 2. 4-9. 5% for different aromatic amines. In comparison with PANI/Pt and commercial PA, the PANI-IL/Pt fiber showed higher extraction efficiency and repeatability. It also exhibited high extraction capability to benzene compounds. The PANI-IL/Pt fiber was used for more than 120

  4. 离子液体均相液液微萃取-高效液相色谱法测定婴儿奶粉中5种三嗪类除草剂%Determination of five triazine herbicides in infant milk powder by high performance liquid chromatography coupled with ionic liquid-based homogeneous liquid-liquid microextraction

    Institute of Scientific and Technical Information of China (English)

    张丽媛; 姚笛; 李娜; 张寒琦; 于爱民

    2015-01-01

    建立了婴儿配方奶粉中三嗪类除草剂的均相液液微萃取-高效液相色谱分析方法。以离子液体为液液微萃取溶剂,Eclipse XDB-C18为色谱柱,乙腈和水为流动相梯度洗脱分离。详细研究了液液微萃取条件对实验结果的影响。在最优实验条件下,三嗪类除草剂的标准曲线呈良好的线性( r≥0.9992),草净津、敌草净、特丁通、特丁津和异戊乙净的检出限分别是12.1、13.8、11.8、14.6和13.7μg/kg;婴儿配方奶粉中的加标回收率为92.2%~103.2%,相对标准偏差低于6%。该方法灵敏度高、操作简单,适用于奶粉样品中三嗪类除草剂残留的检测。%A high performance liquid chromatography coupled with homogeneous liquid-liquid microextraction was developed for the determination of five triazine herbicides in infant milk powders. The ionic liquid was used as microextraction solvent. The separation of the herbicides was performed on an Eclipse XDB-C18 column using acetonitrile and water as mobile phases in gradient mode. The effects of homogeneous liquid-liquid extraction conditions on the experi-mental results were investigated in detail. Under the optimized experimental conditions,the cal-ibration curves for determining the analytes were linear and the correlation coefficients were ≥0. 999 2. The limits of detection for cyanazine,desmetryn,terbumeton,terbuthylazine and dim-ethametryn were 12. 1,13. 8,11. 8,14. 6 and 13. 7 μg/kg,respectively. The recoveries of the analytes spiked in four infant milk powders ranged from 92. 2% to 103. 2% and the relative standard deviations were lower than 6%. This method is sensitive,simple,and suitable for the determination of triazine herbicides in milk powder samples.

  5. 纵向超声波辅助微注塑方法%Longitudinal Ultrasound-Assisted Micro-Injection Moulding Method

    Institute of Scientific and Technical Information of China (English)

    仇中军; 郑辉; 房丰洲; 王寰宇

    2012-01-01

    Polymer melt flowing in micro/nano structures in micro-injection moulding is relatively insuffi-cient in mould filling, compared with that in a conventional injection moulding, since the flow resistance of polymer melt flowing in micro-channel is larger, and product quality is affected by uncertainty and non-uniformity of heat loss. In this paper, a longitudinal ultrasound-assisted micro-injection moulding method was proposed, the mechanism of ultrasonic vibration affecting polymer melt was presented, and the effects of ultrasonic amplitude transformer on stress condition, amplitude and resonance frequency were ana-lyzed. An ultrasound-assisted micro-injection moulding system was developed based on the simulation re-sult of micro-injection moulding process. The system decreased the viscosity of polymer melt and im-proved fluidity and mould filling capability due to the energy exchange between longitudinal ultrasound and polymer melt. In order to verify the effect of ultrasound-assisted micro-injection moulding, an ultra-sound-assisted micro-injection moulding experiment on Fresnel lens was conducted. Experimental results show that the mould filling capability of polymer melt in micro-injection moulding process is improved by 6. 91% with the same injection parameters.%微注塑过程中,聚合物熔体在微小腔体中流动时充模阻力比常规注塑大,这影响了熔体填充效果,同时热量损失的不均衡性和不确定性容易导致注塑精度不高.提出了纵向超声波辅助微注塑方法,并对超声波振动对聚合物熔体的作用机理进行了探讨,分析了超声换能器结构对应力、振幅和响应频率的影响.基于对微注塑过程的模拟结果,开发了纵向超声波辅助微注塑装置.通过在微注塑过程中纵向超声波对熔体的能量作用降低熔体黏度,改善了熔体流动和充填性能.为了验证超声波辅助微注塑的效果,进行了菲涅尔透镜实际注塑实验.实验结果表明,相

  6. Ionic Liquid Solvent Based on Cyclic Guanidinium Cation for Nucleophilic Displacement Reactions

    Institute of Scientific and Technical Information of China (English)

    LIN Ying-jie; QIU Zhi-ming; DUAN Hai-feng; LI Sheng-hai; ZHANG Suo-bo

    2004-01-01

    The nucleophilic displacement reaction of n-bromooctane and potassium iodide in ionic liquid based on cyclic guanidinium cation(2) was investigated. The kinetic reasult shows that the rate of the reaction is enhanced in ionic liquid (2). The same reaction in [bmim][PF6](1)(where bmim=1-butyl-3-methylimidazolium) was also studied. It was found that as a reaction medium ionic liquid (2) is better than (1) for nucelophilic displacement reactions.

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

    OpenAIRE

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

    2012-01-01

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

  8. New Ionic Liquids from Natural Products for Environmentally Benign Aircraft Deicing and Anti-Icing

    Science.gov (United States)

    2010-12-10

    effective concentration to immobilize 50% microorganism GRAS ‘generally regarded as safe’, Food & Drug Administration ILs ionic liquids J·mol-1·K...mixture of propylene glycol/water just before takeoff. Although propylene glycol is ‘generally regarded as safe’ (GRAS) by the US Food & Drug ...Commun. 2004, 630-631. St. Kalb, R.; Kotschan, M. J. Ionic liquids based on dibutylphosphate; chiral and “natural” ionic liquids. proionic

  9. Effect of the ultrasound-assisted preliminary maceration on the efficiency of the essential oil distillation from selected herbal raw materials.

    Science.gov (United States)

    Kowalski, Radosław; Kowalska, Grażyna; Jamroz, Jerzy; Nawrocka, Agnieszka; Metyk, Damian

    2015-05-01

    The objective of the study was the estimation of the ultrasound-assisted preliminary maceration effect on the efficiency of essential oil distillation and on its qualitative and quantitative composition. The experiment included analyses on three herbal materials, i.e. peppermint leaves (Mentha piperita L.), marjoram herb (Origanum majorana L.), and chamomile flowers (Chamomilla recutita (L.) Rauschert). The study showed that the application of preliminary water maceration of raw material, augmented with ultrasounds, had a statistically significant increasing effect on the amount of oil distilled, in the case of mint leaf from 1.32% to 1.46% v/w, and in the case of marjoram herb from 1.13% to 1.27% v/w. In the case of chamomile flowers no significant effect of ultrasound on the amount of oil obtained was observed. Generally, comparing the composition of essential oils obtained in the experiments with the requirements of the relevant standards no unfavourable effect of the distillation augmenting techniques applied was noted. Therefore, it should be expected that the studied distillates of volatile fractions will have the desired biological activity. Copyright © 2014 Elsevier B.V. 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. Optimization of pulsed ultrasound-assisted technique for extraction of phenolics from pomegranate peel of Malas variety: Punicalagin and hydroxybenzoic acids.

    Science.gov (United States)

    Kazemi, Milad; Karim, Roselina; Mirhosseini, Hamed; Abdul Hamid, Azizah

    2016-09-01

    Pomegranate peel is a rich source of phenolic compounds (such as punicalagin and hydroxybenzoic acids). However, the content of such bioactive compounds in the peel extract can be affected by extraction type and condition. It was hypothesized that the optimization of a pulsed ultrasound-assisted extraction (PUAE) technique could result in the pomegranate peel extract with higher yield and antioxidant activity. The main goal was to optimize PUAE condition resulting in the highest yield and antioxidant activity as well as the highest contents of punicalagin and hydroxybenzoic acids. The operation at the intensity level of 105W/cm(2) and duty cycle of 50% for a short time (10min) had a high efficiency for extraction of phenolics from pomegranate peel. The application of such short extraction can save the energy and cost of the production. Punicalagin and ellagic acid were the most predominant phenolic compounds quantified in the pomegranate peel extract (PPE) from Malas variety. PPE contained a minor content of gallic acid.

  12. 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.

  13. Ultrasound-assisted magnetic solid-phase extraction for the determination of some transition metals in Orujo spirit samples by capillary electrophoresis.

    Science.gov (United States)

    Peña Crecente, Rosa M; Lovera, Carlha Gutiérrez; García, Julia Barciela; Latorre, Carlos Herrero; Martín, Sagrario García

    2016-01-01

    Ultrasound-assisted magnetic solid-phase extraction coupled to capillary electrophoresis was optimized for the preconcentration and determination of Zn(II), Cu(II), Mn(II) and Cd(II) as their complexes with 1,10-phenanthroline (Phen). Both pre- and on-capillary complexations were employed to obtain stable metal-Phen complexes. The parameters that have an influence on the electrophoretic separation and the MSPE process were studied and optimized using different experimental designs. Metals were extracted from 10 mL of sample at pH 5 using 3mg of magnetic particles functionalized with carboxylic groups. The metals were eluted as metal-Phen complexes and analyzed by capillary electrophoresis. The method showed low limits of detection for metals 0.49-2.19 μg L(-1), and high preconcentration factors, 39-44, The efficiencies of the extraction method were in the range 77.1-87.5% and the precision (RSD < 10%) and accuracy were between 98.2% and 101.6%. The method was applied to the determination of the aforementioned metals in Galician Orujo spirit samples.

  14. Integration of phase separation with ultrasound-assisted salt-induced liquid-liquid microextraction for analyzing the fluoroquinones in human body fluids by liquid chromatography.

    Science.gov (United States)

    Wang, Huili; Gao, Ming; Wang, Mei; Zhang, Rongbo; Wang, Wenwei; Dahlgren, Randy A; Wang, Xuedong

    2015-03-15

    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 (FQs) in human body fluids. The integrated device consisted of three simple HDPE components used to separate the extraction solvent from the aqueous phase prior to retrieving the extractant. A series of extraction parameters were optimized using the response surface method based on central composite design. Optimal conditions consisted of 945μL acetone extraction solvent, pH 2.1, 4.1min stir time, 5.9g Na2SO4, and 4.0min centrifugation. Under optimized conditions, the limits of detection (at S/N=3) were 0.12-0.66μgL(-1), the linear range was 0.5-500μgL(-1) and recoveries were 92.6-110.9% for the five FQs extracted from plasma and urine. The proposed method has several advantages, such as easy construction from inexpensive materials, high extraction efficiency, short extraction time, and compatibility with HPLC analysis. Thus, this method shows excellent prospects for sample pretreatment and analysis of FQs in human body fluids.

  15. Effect of Supplementation with Wheat Bran Aqueous Extracts Obtained by Ultrasound-Assisted Technologies on the Sensory Properties and the Antioxidant Activity of Dry Pasta.

    Science.gov (United States)

    Pasqualone, Antonella; Delvecchio, Laura Nunzia; Gambacorta, Giuseppe; Laddomada, Barbara; Urso, Valeria; Mazzaglia, Agata; Ruisi, Paolo; Di Miceli, Giuseppe

    2015-10-01

    Phenolic compounds have antioxidant properties and activate endogenous detoxification defense systems able to scavenge the reactive species of oxygen. The external layers of wheat caryopsis, largely constituting by-products of the milling industry such as bran and various middlings, contain relevant amounts of phenolic compounds. The aim of the research has been to evaluate the effect of supplementation with wheat bran aqueous extracts, obtained by ultrasound-assisted technologies, on the sensory properties and antioxidant activity of dry pasta. The HPLC-DAD characterization of the extract evidenced the presence of ferulic and p-coumaric acids. The supplemented pasta showed significantly higher antioxidant activity and phenolic content than the control, coupled to good overall sensory judgment. In addition, two different pasta drying diagrams were adopted, and the comparison of the corresponding end-products allowed it to be pointed out that the processing technology has to be carefully set up to prevent possible detrimental effects on the antioxidant activity. The proposed utilization of bran might add value to a milling by-product that, otherwise, is mostly employed in animal feeding.

  16. 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.

  17. A novel ultrasound-assisted back extraction reverse micelles method coupled with gas chromatography-flame ionization detection for determination of aldehydes in heated edibles oils.

    Science.gov (United States)

    Ramezani, Zahra; Mirzajani, Roya; Kardani, Fatemeh

    2015-12-01

    A novel ultrasound-assisted back extraction reverse micelles coupled with gas chromatography-flame ionization detection has been developed for the extraction and determination of some short chain aldehydes in different heated edible oil samples. After the homogenization of the oil samples with Triton X-100, 200 μL of methanol was added to facilitate the phase separation. The aqueous micelle phase has been separated by centrifugation, then it was treated with a mixture of H2O: CHCl3 and ultrasonic vibration, were used to effectively back-extraction of the analytes into the chloroform phase. The sedimented organic phase was obtained after centrifugation, withdrawn into the microsyringe and directly injected into the GC-FID system. The calibration graphs were linear in the range 0.05-20 mg L(-1). The limits of detection were in the range of 0.02-0.15 mg L(-1). This procedure was successfully applied for determination of propanal, butanal, hexanal and heptanal in real heated oil samples.

  18. Determination of volatile components of saffron by optimised ultrasound-assisted extraction in tandem with dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Sereshti, Hassan; Heidari, Reza; Samadi, Soheila

    2014-01-15

    In the present research, a combined extraction method of ultrasound-assisted extraction (UAE) in conjunction with dispersive liquid-liquid microextraction (DLLME) was applied to isolation and enrichment of saffron volatiles. The extracted components of the saffron were separated and determined by gas chromatography-mass spectrometry (GC-MS) technique. The mixture of methanol/acetonitrile was chosen for the extraction of the compounds and chloroform was used at the preconcentration stage. The important parameters, such as composition of extraction solvent, volume of preconcentration solvent, ultrasonic applying time, and salt concentration were optimised by using a half-fraction factorial central composite design (CCD). Under the optimal conditions, the linear dynamic ranges (LDRs) were 10-10,000mgL(-)(1). The determination coefficients (R(2)) were from 0.9990 to 0.9997. The limits of detection (LODs) and limits of quantification (LOQs) for the extracted compounds were 6-123mgL(-)(1) and 20-406mgL(-)(1), respectively. The relative standard deviations (RSDs) were 2.48-9.82% (n=3). The enhancement factors (EFs) were 3.6-41.3.

  19. Ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME)-a fast new approach to measure phthalate metabolites in nails.

    Science.gov (United States)

    Alves, Andreia; Vanermen, Guido; Covaci, Adrian; Voorspoels, Stefan

    2016-09-01

    A new, fast, and environmentally friendly method based on ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME) was developed and optimized for assessing the levels of seven phthalate metabolites (including the mono(ethyl hexyl) phthalate (MEHP), mono(2-ethyl-5-hydroxyhexyl) phthalate (5-OH-MEHP), mono(2-ethyl-5-oxohexyl) phthalate (5-oxo-MEHP), mono-n-butyl phthalate (MnBP), mono-isobutyl phthalate (MiBP), monoethyl phthalate (MEP), and mono-benzyl phthalate (MBzP)) in human nails by UPLC-MS/MS. The optimization of the US-DLLME method was performed using a Taguchi combinatorial design (L9 array). Several parameters such as extraction solvent, solvent volume, extraction time, acid, acid concentration, and vortex time were studied. The optimal extraction conditions achieved were 180 μL of trichloroethylene (extraction solvent), 2 mL trifluoroacetic acid in methanol (2 M), 2 h extraction and 3 min vortex time. The optimized method had a good precision (6-17 %). The accuracy ranged from 79 to 108 % and the limit of method quantification (LOQm) was below 14 ng/g for all compounds. The developed US-DLLME method was applied to determine the target metabolites in 10 Belgian individuals. Levels of the analytes measured in nails ranged between Extraction and phase separation of the US-DLLME procedure.

  20. Miniaturized matrix solid-phase dispersion combined with ultrasound-assisted dispersive liquid-liquid microextraction for the determination of three pyrethroids in soil.

    Science.gov (United States)

    Wang, Hui; Yan, Hongyuan; Qiao, Jindong

    2012-01-01

    A simple and miniaturized pretreatment procedure combining matrix solid-phase dispersion (MSPD) with ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) technique was proposed in first time for simultaneous determination of three pyrethroids (fenpropathrin, cyhalothrin and fenvalerate) in soils. The solid samples were directly extracted using MSPD procedure, and the eluent of MSPD was used as the dispersive solvent of the followed DLLME procedure for further purification and enrichment of the analytes before GC-ECD analysis. Good linear relationships were obtained for all the analytes in a range of 5.0-500.0 ng/g with LOQs (S/N=10) ranged from 1.51 to 3.77 ng/g. Average recoveries at three spiked levels were in a range of 83.6-98.5% with RSD≤7.3%. The present method combined the advantages of MSPD and DLLME, and was successfully applied for the determination of three pyrethroids in soil samples.

  1. Ultrasound-assisted dispersive liquid-liquid microextraction for the determination of seven recreational drugs in human whole blood using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lin, Zebin; Li, Jiaolun; Zhang, Xinyu; Qiu, Meihong; Huang, Zhibin; Rao, Yulan

    2017-03-01

    Recreational drugs have large impact on public health and security, and to monitor them is of urgent demand. In the present study, ultrasound-assisted dispersive liquid-liquid microextraction combined with the detection of gas chromatography-mass spectrometry was applied to the determination of seven common recreational drugs, including amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, meperidine, methadone and ketamine in 200μL of human whole blood. A series of factors which would affect the extraction efficiency were systematically investigated, including the nature and the volume of extraction and dispersing solvents, ultrasonication time, salting-out effect and pH value. The method consumed small amount of sample. The limits of detection and limits of quantification for each analyte were 10 and 40ng/mL, respectively, and the linearity was in the range of 0.04-25μg/mL (R(2) higher than 0.99). Good specificity, precision (1.5-8.2% for the intra-day study and 2.6-12.8% for the inter-day study), satisfactory accuracy (85.0-117.1%) and extraction recovery (77.0-92.4%) were obtained, which makes it a high performance method for the determination of recreational drugs in human whole blood samples.

  2. Determination of cyclic and linear siloxanes in wastewater samples by ultrasound-assisted dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cortada, Carol; dos Reis, Luciana Costa; Vidal, Lorena; Llorca, Julio; Canals, Antonio

    2014-03-01

    A fast, simple and environmentally friendly ultrasound-assisted dispersive liquid-liquid microextraction (USA-DLLME) procedure has been developed to preconcentrate eight cyclic and linear siloxanes from wastewater samples prior to quantification by gas chromatography-mass spectrometry (GC-MS). A two-stage multivariate optimization approach has been developed employing a Plackett-Burman design for screening and selecting the significant factors involved in the USA-DLLME procedure, which was later optimized by means of a circumscribed central composite design. The optimum conditions were: extractant solvent volume, 13 µL; solvent type, chlorobenzene; sample volume, 13 mL; centrifugation speed, 2300 rpm; centrifugation time, 5 min; and sonication time, 2 min. Under the optimized experimental conditions the method gave levels of repeatability with coefficients of variation between 10 and 24% (n=7). Limits of detection were between 0.002 and 1.4 µg L(-1). Calculated calibration curves gave high levels of linearity with correlation coefficient values between 0.991 and 0.9997. Finally, the proposed method was applied for the analysis of wastewater samples. Relative recovery values ranged between 71 and 116% showing that the matrix had a negligible effect upon extraction. To our knowledge, this is the first time that combines LLME and GC-MS for the analysis of methylsiloxanes in wastewater samples.

  3. Ultrasound-assisted dispersive liquid-liquid microextraction of tetracycline drugs from egg supplements before flow injection analysis coupled to a liquid waveguide capillary cell.

    Science.gov (United States)

    Rodríguez, Michael Pérez; Pezza, Helena Redigolo; Pezza, Leonardo

    2016-09-01

    A simple, rapid, and efficient ultrasound-assisted dispersive liquid-liquid microextraction (US-DLLME) method was developed for extraction of tetracycline residues from egg supplement samples, with subsequent determination by flow injection analysis (FIA) coupled to a liquid waveguide capillary cell (LWCC) and a controlled temperature heating bath. Tetracyclines react with diazotized p-sulfanilic acid, in a slightly alkaline medium, to form azo compounds that can be measured at 435 nm. The reaction sensitivity improved substantially (5.12-fold) using an in-line heating temperature of 45 °C. Multivariate methodology was used to optimize the factors affecting the extraction efficiency, considering the volumes of extraction and disperser solvents, sonication time, extraction time, and centrifugation time. Good linearity in the range 30-600 μg L(-1) was obtained for all the tetracyclines, with regression coefficients (r) higher than 0.9974. The limits of detection ranged from 6.4 to 11.1 μg L(-1), and the recoveries were in the range 85.7-96.4 %, with relative standard deviation lower than 9.8 %. Analyte recovery was improved by approximately 6 % when the microextraction was assisted by ultrasound. The results obtained with the proposed US-DLLME-FIA method were confirmed by a reference HPLC method and showed that the egg supplement samples analyzed were suitable for human consumption.

  4. Ultrasound-assisted extraction followed by disposable pipette purification for the determination of polychlorinated biphenyls in small-size biological tissue samples.

    Science.gov (United States)

    Pena-Abaurrea, M; García de la Torre, V S; Ramos, L

    2013-11-22

    The use of solid-phase extraction pipette tip (also called disposable pipette extraction, DPX) has been evaluated for the purification of environmentally relevant polychlorinated biphenyls (PCBs) in fatty extracts obtained by ultrasound-assisted extraction with a sonication probe from small-size biological tissues. Complete sample treatment involved only 50 mg of sample and was completed in ca. 15 min with minimal sample manipulation and reagents consumption (i.e., 1.5 mL of n-hexane and 0.8 g of acidic silica). The performance of the proposed methodology for the intended determination was firstly evaluated by determination of the endogenous PCB levels in a naturally contaminated internal reference material. The determined concentrations showed a good agreement with those obtained using a more conventional sample preparation procedure previously validated in our laboratory (recoveries, as compared to levels determined using the latter method, were in the 85-123% range for a large majority of the studied congeners, and the relative standard deviations were in general lower than 14%). Results obtained for the analysis of reference food samples and certified reference materials NIST 1945 and 1947 demonstrated that, when combined with gas chromatography coupled to ion trap mass spectrometry working in the tandem mode, GC-ITD(MS/MS), the proposed methodology allowed accurate determination of most of the investigated PCBs and that 50 mg of sample sufficed for the screening of less abundant toxic congeners. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. 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 B3) 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%.

  6. 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.

  7. Ultrasound-Assisted Surfactant-Enhanced Emulsification Micro-Extraction Followed by HPLC for Determination of Preservatives in Water, Beverages and Personal Care Products.

    Science.gov (United States)

    Jan-E, Sudarat; Santaladchaiyakit, Yanawath; Burakham, Rodjana

    2017-01-01

    An ultrasound-assisted surfactant-enhanced emulsification micro-extraction (UASEME) procedure has been developed for pre-concentration of benzoic acid (BA) and paraben preservatives, including methylparaben, ethylparaben, propylparaben and butylparaben, prior to high-performance liquid chromatography-ultraviolet (HPLC-UV) analysis. Separations were performed on a Lichrospher RP-18 endcapped 5 µm, using an isocratic mobile phase of 40% acetonitile, at a flow rate of 1 mL min(-1) The selected UASEME conditions comprised the use of 10 mL sample extract, 125 µL 1-octanol as extraction solvent and 0.05 mmol L(-1) Tween 20 as emulsifier, 0.5% sodium chloride, ultrasonication time of 6 min and centrifugation time of 10 min. Method performance demonstrated wide linear range between 0.5 and 7,000 µg L(-1) (R(2) > 0.9903) and limits of detection between 0.03 and 10 µg L(-1), which providing the enrichment factors of 15-184. The method precision (relative standard deviation) was HPLC-UV has been successfully applied to determine four paraben preservatives in various sample matrices such as water, beverages and personal care products. The recoveries in the range of 70-138.1% were obtained. However, BA could not be determined in real sample extracts. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  8. Determination of aminophenols and phenol in hair colorants by ultrasound-assisted solid-phase dispersion extraction coupled with ion chromatography.

    Science.gov (United States)

    Zhong, Zhixiong; Li, Gongke; Wu, Rong; Zhu, Binghui; Luo, Zhibin

    2014-08-01

    A simple and reliable ultrasound-assisted solid-phase dispersion extraction coupled with ion chromatography was developed for the determination of aminophenols and phenol. The highly viscous hair colorant was dispersed in solvents using anhydrous sodium sulfite having dual functions of dispersant and antioxidant. The use of anhydrous sodium sulfite did not change the sample volume because it could completely dissolve in solution after matrix dispersion. The extraction and cleanup were combined in one single step for simplifying operation. The extraction process could be rapidly accomplished within 9 min with high sample throughput under the synergistic effects of vibration, ultrasound, and heating. Satisfactory linearity was observed with correlation coefficients higher than 0.9992, and the limits of detection varied from 0.02 to 0.09 mg/L. The applicability of the proposed method was demonstrated by measuring the concentrations of aminophenols and phenol in 32 different commercial hair color products. The recoveries ranged from 86.4-101.2% with the relative standard deviations in the range of 0.52-4.3%. The method offers an attractive alternative for the analysis of trace phenols in complex matrices.

  9. Measurement of selected polychlorinated biphenyls (PCBs) in water via ultrasound assisted emulsification-microextraction (USAEME) using low-density organic solvents.

    Science.gov (United States)

    Yurdakok-Dikmen, Begum; Kuzukiran, Ozgur; Filazi, Ayhan; Kara, Erdem

    2016-04-01

    Despite bans and restrictions for their adverse health effects including endocrine disruption, due to their stability in the environment, polychlorinated biphenyls (PCBs) are still of concern for their residues in several matrices. This study employed low-density ultrasound-assisted emulsification-microextraction (USAEME) to measure selected PCBs (28, 52, 101, 118, 138, 153, and 180) in water samples for gas chromatography-mass spectrometry analysis. Among tested solvents (isooctane, chloroform, hexane, and cyclohexane), 200 μL isooctane resulted in the highest yield for a 10 mL sample. The optimized method was validated and yielded recoveries of 87.29-92.83% with the limit of detection and limit of quantification (LOQ) values 3-12 ng/L and 10-40 ng/L, respectively. Twelve tap water samples collected in September 2014 were screened using this simple, rapid, and validated method. PCB concentrations in two samples were above the LOQ values; one sample contained 1,380 ng/L of PCB 118, 530 ng/L of PCB 138, and 152 ng/L of PCB 153, and the other contained 444 ng/L of PCB 138. Despite the city water supply being clean and the municipality employing all available measures to ensure clean water supply, the general public must be made aware of the regular maintenance of local water pipelines and storage tanks for the prevention of PCB contamination.

  10. Optimization of Ultrasound-assisted extraction of polyphenols, tannins and epigallocatechin gallate from barks of Stryphnodendron adstringens (Mart. Coville bark extracts

    Directory of Open Access Journals (Sweden)

    Jordana N. Sousa

    2014-01-01

    Full Text Available Background: 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. Materials and Methods: 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. Results: 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. Conclusion: 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.

  11. Ultrasound-Assisted Extraction of Syringin from the Bark of Ilex rotunda Thumb Using Response Surface Methodology

    Directory of Open Access Journals (Sweden)

    Hui Wang

    2012-06-01

    Full Text Available In this work, a rapid extraction method based on ultrasound-assisted extraction (UAE of syringin from the bark of Ilex rotunda Thumb using response surface methodology (RSM is described. The syringin was analyzed and quantified by high performance liquid chromatography coupled with UV detection (HPLC-UV. The extraction solvent, extraction temperature and extraction time, the three main factors for UAE, were optimized with Box-Behnken design (BBD to obtain the highest extraction efficiency. The optimal conditions were the use of a sonication frequency of 40 kHz, 65% methanol as the solvent, an extraction time of 30 min and an extraction temperature of 40 °C. Using these optimal conditions, the experimental values agreed closely with the predicted values. The analysis of variance (ANOVA indicated a high goodness of model fit and the success of the RSM method for optimizing syringin extraction from the bark of I. rotunda.

  12. 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.

  13. Ultrasound assisted synthesis of doped TiO2 nano-particles: characterization and comparison of effectiveness for photocatalytic oxidation of dyestuff effluent.

    Science.gov (United States)

    Shirsath, S R; Pinjari, D V; Gogate, P R; Sonawane, S H; Pandit, A B

    2013-01-01

    The present work deals with the synthesis of titanium dioxide nanoparticles doped with Fe and Ce using sonochemical approach and its comparison with the conventional doping method. The prepared samples have been characterized using X-ray diffraction (XRD), FTIR, transmission electron microscopy (TEM) and UV-visible spectra (UV-vis). The effectiveness of the synthesized catalyst for the photocatalytic degradation of crystal violet dye has also been investigated considering crystal violet degradation as the model reaction. It has been observed that the catalysts prepared by sonochemical method exhibit higher photocatalytic activity as compared to the catalysts prepared by the conventional methods. Also the Ce-doped TiO(2) exhibits maximum photocatalytic activity followed by Fe-doped TiO(2) and the least activity was observed for only TiO(2). The presence of Fe and Ce in the TiO(2) structure results in a significant absorption shift towards the visible region. Detailed investigations on the degradation indicated that an optimal dosage with 0.8 mol% doping of Ce and 1.2 mol% doping of Fe in TiO(2) results in higher extents of degradation. Kinetic studies also established that the photocatalytic degradation followed the pseudo first-order reaction kinetics. Overall it has been established that ultrasound assisted synthesis of doped photocatalyst significantly enhances the photocatalytic activity.

  14. Comparison of rapidly synergistic cloud point extraction and ultrasound-assisted cloud point extraction for trace selenium coupled with spectrophotometric determination.

    Science.gov (United States)

    Wen, Xiaodong; Zhang, Yanyan; Li, Chunyan; Fang, Xiang; Zhang, Xiaocan

    2014-04-05

    In this work, rapidly synergistic cloud point extraction (RS-CPE) and ultrasound-assisted cloud point extraction (UA-CPE) were firstly compared and coupled with spectrophotometer for selenium preconcentration and detection. The established RS-CPE pretreatment was simple, rapid and high effective. The extraction time was only 1min without heating process. Under the effect of ultrasound, UA-CPE accomplished extraction efficiently although the extraction procedure was relatively time-consuming. In this study, RS-CPE and UA-CPE were firstly applied for selenium preconcentration and coupled with conventional spectrophotometer. Their applications were expanded and the analytical performance of spectrophotometric determination for selenium was considerably improved. The influence factors relevant to RS-CPE and UA-CPE were studied in detail. Under the optimal conditions, the limits of detection (LODs) for selenium were respectively 0.2μgL(-1) of RS-CPE and 0.3μgL(-1) of UA-CPE with sensitivity enhancement factors (EFs) of 124 and 103. The developed methods were applied to the determination of trace selenium in real water samples with satisfactory analytical results.

  15. 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.

  16. Ultrasound-assisted emulsification-microextraction combined with graphite furnace atomic absorption spectrometry for the determination of trace lead in water

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Hongmei; Zhang, Yu; Qiu, Bocheng; Li, Wenhua [College of Science, Nanjing Agricultural University, Nan Jing (China)

    2012-04-15

    The ultrasound-assisted emulsification-microextraction (USAEME) method was combined with graphite furnace atomic absorption spectrometry (GFAAS) for the determination of trace Pb using dithizone (H{sup 2}DZ) as chelating reagent. Some effective parameters influenced the detection and microextraction, such as ashing temperature and atomization temperature, pH, extraction solvent, sample volume, extraction time, and extraction temperature were selected and optimized. After extraction, the calibration curves for Pb was in the concentration range of 0.1-10 ng mL{sup -1}, and the linear equation was y = 0.097 x + 0.023 (R = 0.99). Under the optimized conditions, the detection limit of the method was 20 pg mL{sup -1} with an enrichment factor of 70 and the relative standards deviation (RSD) for seven determinations of 1 ng mL{sup -1} Pb was 11%. The proposed method was successfully applied to determine trace Pb in Yueya Lake water, pond water, and spiked samples. Furthermore, a certified reference material of Environment Water (GBW08607) was analyzed and the determined value was in good agreement with the certified value, which showed the accuracy, recovery, and applicability of the reported method. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)