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

Science.gov (United States)

Khezeli, Tahere; Daneshfar, Ali

2017-09-01

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

A new combined method of stable isotope-labeling derivatization-ultrasound-assisted dispersive liquid-liquid microextraction for the determination of neurotransmitters in rat brain microdialysates by ultra high performance liquid chromatography tandem mass spectrometry.

Science.gov (United States)

Zheng, Longfang; Zhao, Xian-En; Zhu, Shuyun; Tao, Yanduo; Ji, Wenhua; Geng, Yanling; Wang, Xiao; Chen, Guang; You, Jinmao

2017-06-01

In this work, for the first time, a new hyphenated technique of stable isotope-labeling derivatization-ultrasound-assisted dispersive liquid-liquid microextraction has been developed for the simultaneous determination of monoamine neurotransmitters (MANTs) and their biosynthesis precursors and metabolites. The developed method was based on ultra high performance liquid chromatography tandem mass spectrometry detection using multiple-reaction monitoring mode. A pair of mass spectrometry sensitizing reagents, d 0 -10-methyl-acridone-2-sulfonyl chloride and d 3 -10-methyl-acridone-2-sulfonyl chloride, as stable isotope probes was utilized to facilely label neurotransmitters, respectively. The heavy labeled MANTs standards were prepared and used as internal standards for quantification to minimize the matrix effects in mass spectrometry analysis. Low toxic bromobenzene (extractant) and acetonitrile (dispersant) were utilized in microextraction procedure. Under the optimized conditions, good linearity was observed with the limits of detection (S/N>3) and limits of quantification (S/N>10) in the range of 0.002-0.010 and 0.015-0.040nmol/L, respectively. Meanwhile, it also brought acceptable precision (4.2-8.8%, peak area RSDs %) and accuracy (recovery, 96.9-104.1%) results. This method was successfully applied to the simultaneous determination of monoamine neurotransmitters and their biosynthesis precursors and metabolites in rat brain microdialysates of Parkinson's disease and normal rats. This provided a new method for the neurotransmitters related studies in the future. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Energy Technology Data Exchange (ETDEWEB)

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

2011-11-30

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

Dispersive solid-phase extraction followed by vortex-assisted dispersive liquid-liquid microextraction based on the solidification of a floating organic droplet for the determination of benzoylurea insecticides in soil and sewage sludge.

Science.gov (United States)

Peng, Guilong; He, Qiang; Mmereki, Daniel; Lu, Ying; Zhong, Zhihui; Liu, Hanyang; Pan, Weiliang; Zhou, Guangming; Chen, Junhua

2016-04-01

A novel dispersive solid-phase extraction combined with vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet was developed for the determination of eight benzoylurea insecticides in soil and sewage sludge samples before high-performance liquid chromatography with ultraviolet detection. The analytes were first extracted from the soil and sludge samples into acetone under optimized pretreatment conditions. Clean-up of the extract was conducted by dispersive solid-phase extraction using activated carbon as the sorbent. The vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet procedure was performed by using 1-undecanol with lower density than water as the extraction solvent, and the acetone contained in the solution also acted as dispersive solvent. Under the optimum conditions, the linearity of the method was in the range 2-500 ng/g with correlation coefficients (r) of 0.9993-0.9999. The limits of detection were in the range of 0.08-0.56 ng/g. The relative standard deviations varied from 2.16 to 6.26% (n = 5). The enrichment factors ranged from 104 to 118. The extraction recoveries ranged from 81.05 to 97.82% for all of the analytes. The good performance has demonstrated that the proposed methodology has a strong potential for application in the multiresidue analysis of complex matrices. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultrasound-assisted leaching-dispersive solid-phase extraction followed by liquid-liquid microextraction for the determination of polybrominated diphenyl ethers in sediment samples by gas chromatography-tandem mass spectrometry.

Science.gov (United States)

Fontana, Ariel R; Lana, Nerina B; Martinez, Luis D; Altamirano, Jorgelina C

2010-06-30

Ultrasound-assisted leaching-dispersive solid-phase extraction followed by dispersive liquid-liquid microextraction (USAL-DSPE-DLLME) technique has been developed as a new analytical approach for extracting, cleaning up and preconcentrating polybrominated diphenyl ethers (PBDEs) from sediment samples prior gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis. In the first place, PBDEs were leached from sediment samples by using acetone. This extract was cleaned-up by DSPE using activated silica gel as sorbent material. After clean-up, PBDEs were preconcentrated by using DLLME technique. Thus, 1 mL acetone extract (disperser solvent) and 60 microL carbon tetrachloride (extraction solvent) were added to 5 mL ultrapure water and a DLLME technique was applied. Several variables that govern the proposed technique were studied and optimized. Under optimum conditions, the method detection limits (MDLs) of PBDEs calculated as three times the signal-to-noise ratio (S/N) were within the range 0.02-0.06 ng g(-1). The relative standard deviations (RSDs) for five replicates were or =0.9991. Validation of the methodology was carried out by standard addition method at two concentration levels (0.25 and 1 ng g(-1)) and by comparing with a reference Soxhlet technique. Recovery values were > or =80%, which showed a satisfactory robustness of the analytical methodology for determination of low PBDEs concentration in sediment samples. Copyright 2010 Elsevier B.V. All rights reserved.

Analysis of amino acid and monoamine neurotransmitters and their metabolites in rat urine of Alzheimer's disease using in situ ultrasound-assisted derivatization dispersive liquid-liquid microextraction with UHPLC-MS/MS.

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Zhao, Xian-En; He, Yongrui; Li, Meng; Chen, Guang; Wei, Na; Wang, Xiao; Sun, Jing; Zhu, Shuyun; You, Jinmao

2017-02-20

Neurotransmitters (NTs) may play an important role in neurodegenerative disorders such as Alzheimer's disease (AD). In order to investigate the potential links, a new simple, fast, accurate and sensitive analytical method, based on in situ ultrasound-assisted derivatization dispersive liquid-liquid microextraction (in situ UA-DDLLME) coupled with ultra high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS), has been developed and validated. The quantitation of amino acid neurotransmitters (AANTs) and monoamine neurotransmitters (MANTs) in urine of AD rats were performed in this work. The in situ UA-DDLLME procedure involved the rapid injection of the mixture of low toxic 4-bromoanisole (extractant) and acetonitrile (dispersant), which containing the new designed and synthesized 4'-carbonyl chloride rosamine (CCR) as derivatization reagent, into the aqueous phase of real sample and buffer. Under the selected conditions, the derivatization and microextraction of analytes were simultaneously completed within 1min. Good linearity for each analyte (R>0.992) was observed with low limit of detections (LODs, S/N>3). Moreover, the proposed method was compared with direct detection or other reported methods, and the results showed that low matrix effects and good recoveries results were obtained in this work. Taken together, in situ UA-DDLLME coupled with UHPLC-MS/MS analysis was demonstrated to be a good method for sensitive, accurate and simultaneous monitoring of AANTs and MANTs. This method would be expected to be highly useful in AD diseases' clinical diagnostics and may have potential value in monitoring the efficacy of treatment. Copyright © 2016 Elsevier B.V. All rights reserved.

Ultrasound-assisted oxidative desulfurization process of liquid fuel by phosphotungstic acid encapsulated in a interpenetrating amine-functionalized Zn(II)-based MOF as catalyst.

Science.gov (United States)

Afzalinia, Ahmad; Mirzaie, Abbas; Nikseresht, Ahmad; Musabeygi, Tahereh

2017-01-01

In this work, ultrasound-assisted oxidative desulfurization (UAOD) of liquid fuels performed with a novel heterogeneous highly dispersed Keggin-type phosphotungstic acid (H 3 PW 12 O 40 , PTA) catalyst that encapsulated into an amino-functionalized MOF (TMU-17-NH 2 ). The prepared composite exhibits high catalytic activity and reusability in oxidative desulfurization of model fuel. Ultrasound-assisted oxidative desulfurization (UAOD) is a new way to performed oxidation reaction of sulfur-contain compounds rapidly, economically, environment-friendly and safely, under mild conditions. Ultrasound waves can be apply as an efficient tool to decrease the reaction time and improves oxidative desulfurization system performance. PTA@TMU-17-NH 2 could be completely performed desulfurization of the model oil by 20mg of catalyst, O/S molar ratio of 1:1 in presence of MeCN as extraction solvent. The obtained results indicated that the conversions of DBT to DBTO 2 achieve 98% after 15min in ambient temperature. In this work, we prepared TMU-17-NH 2 and PTA/TMU-17-NH 2 composite by ultrasound irradiation for first time and employed in UAOD process. Prepared catalyst exhibit an excellent reusability without PTA leaching and loss of activity. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

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

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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.

Ceria nanocubic-ultrasonication assisted dispersive liquid-liquid microextraction coupled with matrix assisted laser desorption/ionization mass spectrometry for pathogenic bacteria analysis.

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Abdelhamid, Hani Nasser; Bhaisare, Mukesh L; Wu, Hui-Fen

2014-03-01

A new ceria (CeO2) nanocubic modified surfactant is used as the basis of a novel nano-based microextraction technique for highly sensitive detection of pathogenic bacteria (Pseudomonas aeruginosa and Staphylococcus aureus). The technique uses ultrasound enhanced surfactant-assisted dispersive liquid-liquid microextraction (UESA-DLLME) with and without ceria (CeO2) followed by matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS). In order to achieve high separation efficiency, we investigated the influential parameters, including extraction time of ultrasonication, type and volume of the extraction solvent and surfactant. Among various surfactants, the cationic surfactants can selectively offer better extraction efficiency on bacteria analysis than that of the anionic surfactants due to the negative charges of bacteria cell membranes. Extractions of the bacteria lysate from aqueous samples via UESA-DLLME-MALDI-MS were successfully achieved by using cetyltrimethyl ammonium bromide (CTAB, 10.0 µL, 1.0×10(-3) M) as surfactants in chlorobenzene (10.0 µL) and chloroform (10.0 µL) as the optimal extracting solvent for P. aeruginosa and S. aureus, respectively. Ceria nanocubic was synthesized, and functionalized with CTAB (CeO2@CTAB) and then characterized using transmission electron microscopy (TEM) and optical spectroscopy (UV and FTIR). CeO2@CTAB demonstrates high extraction efficiency, improve peaks ionization, and enhance resolution. The prime reasons for these improvements are due to the large surface area of nanoparticles, and its absorption that coincides with the wavelength of MALDI laser (337 nm, N2 laser). CeO2@CTAB-based microextraction offers lowest detectable concentrations tenfold lower than that of without nanoceria. The present approach has been successfully applied to detect pathogenic bacteria at low concentrations of 10(4)-10(5) cfu/mL (without ceria) and at 10(3)-10(4) cfu/mL (with ceria) from bacteria suspensions. Finally, the

New method based on combining ultrasonic assisted miniaturized matrix solid-phase dispersion and homogeneous liquid-liquid extraction for the determination of some organochlorinated pesticides in fish

International Nuclear Information System (INIS)

Rezaei, Farahnaz; Hosseini, Mohammad-Reza Milani

2011-01-01

Highlights: → Ultrasonic assisted miniaturized matrix solid-phase dispersion combined with HLLE was developed as a new method for the extraction of OCPs in fish. → The goal of this combination was to enhance the selectivity of HLLE procedure and to extend its application in biological samples. → This method proposed the advantages of good detection limits, lower consumption of reagents, and does not need any special instrumentation. - Abstract: In this study, ultrasonic assisted miniaturized matrix solid-phase dispersion (US-MMSPD) combined with homogeneous liquid-liquid extraction (HLLE) has been developed as a new method for the extraction of organochlorinated pesticides (OCPs) in fish prior to gas chromatography with electron capture detector (GC-ECD). In the proposed method, OCPs (heptachlor, aldrin, DDE, DDD, lindane and endrin) were first extracted from fish sample into acetonitrile by US-MMSPD procedure, and the extract was then used as consolute solvent in HLLE process. Optimal condition for US-MMSPD step was as follows: volume of acetonitrile, 1.5 mL; temperature of ultrasound, 40 deg. C; time of ultrasound, 10 min. For HLLE step, optimal results were obtained at the following conditions: volume of chloroform, 35 μL; volume of aqueous phase, 1.5 mL; volume of double distilled water, 0.5 mL; time of centrifuge, 10 min. Under the optimum conditions, the enrichment factors for the studied compounds were obtained in the range of 185-240, and the overall recoveries were ranged from 39.1% to 81.5%. The limits of detection were 0.4-1.2 ng g -1 and the relative standard deviations for 20 ng g -1 of the OCPs, varied from 3.2% to 8% (n = 4). Finally, the proposed method has been successfully applied to the analysis of the OCPs in real fish sample, and satisfactory results were obtained.

New method based on combining ultrasonic assisted miniaturized matrix solid-phase dispersion and homogeneous liquid-liquid extraction for the determination of some organochlorinated pesticides in fish

Energy Technology Data Exchange (ETDEWEB)

Rezaei, Farahnaz [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Narmak, Tehran 16846 (Iran, Islamic Republic of); Hosseini, Mohammad-Reza Milani, E-mail: drmilani@iust.ac.ir [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Narmak, Tehran 16846 (Iran, Islamic Republic of); Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Narmak, Tehran 16846 (Iran, Islamic Republic of)

2011-09-30

Highlights: {yields} Ultrasonic assisted miniaturized matrix solid-phase dispersion combined with HLLE was developed as a new method for the extraction of OCPs in fish. {yields} The goal of this combination was to enhance the selectivity of HLLE procedure and to extend its application in biological samples. {yields} This method proposed the advantages of good detection limits, lower consumption of reagents, and does not need any special instrumentation. - Abstract: In this study, ultrasonic assisted miniaturized matrix solid-phase dispersion (US-MMSPD) combined with homogeneous liquid-liquid extraction (HLLE) has been developed as a new method for the extraction of organochlorinated pesticides (OCPs) in fish prior to gas chromatography with electron capture detector (GC-ECD). In the proposed method, OCPs (heptachlor, aldrin, DDE, DDD, lindane and endrin) were first extracted from fish sample into acetonitrile by US-MMSPD procedure, and the extract was then used as consolute solvent in HLLE process. Optimal condition for US-MMSPD step was as follows: volume of acetonitrile, 1.5 mL; temperature of ultrasound, 40 deg. C; time of ultrasound, 10 min. For HLLE step, optimal results were obtained at the following conditions: volume of chloroform, 35 {mu}L; volume of aqueous phase, 1.5 mL; volume of double distilled water, 0.5 mL; time of centrifuge, 10 min. Under the optimum conditions, the enrichment factors for the studied compounds were obtained in the range of 185-240, and the overall recoveries were ranged from 39.1% to 81.5%. The limits of detection were 0.4-1.2 ng g{sup -1} and the relative standard deviations for 20 ng g{sup -1} of the OCPs, varied from 3.2% to 8% (n = 4). Finally, the proposed method has been successfully applied to the analysis of the OCPs in real fish sample, and satisfactory results were obtained.

Ultrasound assisted dispersive liquid-liquid microextraction coupled with high performance liquid chromatography designated for bioavailability studies of felodipine combinations in rat plasma.

Science.gov (United States)

Ahmed, Sameh; Atia, Noha N; Bakr Ali, Marwa Fathy

2017-03-01

Felodipine (FLD), a calcium channel antagonist, is commonly prescribed for the treatment of hypertension either with Metoprolol (MET) or Ramipril (RAM) in two different drug combinations. FLD has high plasma protein binding ability affecting its extraction recoveries from plasma samples. Hence, a specific ultrasound assisted dispersive liquid-liquid microextraction (UA-DLLME) method coupled with HPLC using photodiode array detector was developed and validated for the simultaneous determination of FLD, MET and RAM in rat plasma after oral administration of these combinations. The factors affecting UA-DLLME were carefully optimized. In this study, UA-DLLME method could provide simple and efficient plasma extraction procedures with superior recovery results. Under optimum condition, all target drugs were separated within 13min. The validation procedures was carried out in agreement with US-FDA guidelines and shown to be suitable for anticipated purposes. Linear calibration ranges were obtained in the range 0.05-2.0μgmL -1 for FLD and MET and 0.1-2.0μgmL -1 for RAM with detection limits of 0.013-0.031μgmL -1 for all the studied drug combinations. The%RSD for inter-day and intra-day precisions was in range of 0.63-3.85% and the accuracy results were in the range of 92.13-100.5%. The validated UA-DLLME-HPLC method was successfully applied for the bioavailability studies of FLD, MET and RAM. The pharmacokinetic parameters were calculated for all the investigated drugs in rats after single-dose administrations of two different drug combinations. Although FLD was bioequivalent in the two formulations, a small increase in plasma levels of MET and RAM was found in the presence of FLD. Copyright © 2017 Elsevier B.V. All rights reserved.

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

International Nuclear Information System (INIS)

Xu Xu; Su Rui; Zhao Xin; Liu Zhuang; Zhang Yupu; Li Dan; Li Xueyuan; Zhang Hanqi; Wang Ziming

2011-01-01

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

In situ derivatization-ultrasound-assisted dispersive liquid-liquid microextraction for the determination of neurotransmitters in Parkinson's rat brain microdialysates by ultra high performance liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

He, Yongrui; Zhao, Xian-En; Zhu, Shuyun; Wei, Na; Sun, Jing; Zhou, Yubi; Liu, Shu; Liu, Zhiqiang; Chen, Guang; Suo, Yourui; You, Jinmao

2016-08-05

Simultaneous monitoring of several neurotransmitters (NTs) linked to Parkinson's disease (PD) has important scientific significance for PD related pathology, pharmacology and drug screening. A new simple, fast and sensitive analytical method, based on in situ derivatization-ultrasound-assisted dispersive liquid-liquid microextraction (in situ DUADLLME) in a single step, has been proposed for the quantitative determination of catecholamines and their biosynthesis precursors and metabolites in rat brain microdialysates. The method involved the rapid injection of the mixture of low toxic bromobenzene (extractant) and acetonitrile (dispersant), which containing commercial Lissamine rhodamine B sulfonyl chloride (LRSC) as derivatization reagent, into the aqueous phase of sample and buffer, and the following in situ DUADLLME procedure. After centrifugation, 50μL of the sedimented phase (bromobenzene) was directly injected for ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) detection in multiple reaction monitoring (MRM) mode. This interesting combination brought the advantages of speediness, simpleness, low matrix effects and high sensitivity in an effective way. Parameters of in situ DUADLLME and UHPLC-MS/MS conditions were all optimized in detail. The optimum conditions of in situ DUADLLME were found to be 30μL of microdialysates, 150μL of acetonitrile containing LRSC, 50μL of bromobenzene and 800μL of NaHCO3-Na2CO3 buffer (pH 10.5) for 3.0min at 37°C. Under the optimized conditions, good linearity was observed with LODs (S/N>3) and LOQs (S/N>10) of LRSC derivatized-NTs in the range of 0.002-0.004 and 0.007-0.015 nmol/L, respectively. It also brought good precision (3.2-12.8%, peak area CVs%), accuracy (94.2-108.6%), recovery (94.5-105.5%) and stability (3.8-8.1%, peak area CVs%) results. Moreover, LRSC derivatization significantly improved chromatographic resolution and MS detection sensitivity of NTs when compared with the

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

International Nuclear Information System (INIS)

Mashayekhi, H.A.; Pourshamsian, K.

2012-01-01

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

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.

Ultrasound-air-assisted demulsified liquid-liquid microextraction by solidification of a floating organic droplet for determination of three antifungal drugs in water and biological samples.

Science.gov (United States)

Ezoddin, Maryam; Shojaie, Mehran; Abdi, Khosrou; Karimi, Mohammad Ali

2017-03-01

A novel ultrasound-air-assisted demulsified liquid-liquid microextraction by solidification of a floating organic droplet (UAAD-LLM-SFO) followed by HPLC-UV detection was developed for the analysis of three antifungal drugs in water and biological samples. In this method, 1-dodecanol was used as the extraction solvent. The emulsion was rapidly formed by pulling in and pushing out the mixture of sample solution and extraction solvent for 5 times repeatedly using a 10-mL glass syringe while sonication was performed. Therefore, an organic dispersive solvent required in common microextraction methods was not used in the proposed method. After dispersing, an aliquot of acetonitrile was introduced as a demulsifier solvent into the sample solution to separate two phases. Therefore, some additional steps, such as the centrifugation, ultrasonication, or agitation of the sample solution, are not needed. Parameters influencing the extraction recovery were investigated. The proposed method showed a good linearity for the three antifungal drugs studied with the correlation coefficients (R 2  > 0.9995). The limits of detection (LODs) and the limits of the quantification (LOQs) were between 0.01-0.03 μg L -1 and 0.03-0.08 μg L -1 , respectively. The preconcentration factors (PFs) were in the range of 107-116, respectively. The precisions, as the relative standard deviations (RSDs) (n = 5), for inter-day and intra-day analysis were in the range of 2.1-4.5% and 6.5-8.5%, respectively. This method was successfully applied to determine the three antifungal drugs in tap water and biological samples. The recoveries of antifungal drugs in these samples were 92.4-98.5%. Graphical abstract Ultrasound-air-assisted demulsified liquid-liquid microextraction by solidification of a floating organic droplet for the analysis of three antifungal drugs prior HPLC-UV.

Determination of carbohydrates in tobacco by pressurized liquid extraction combined with a novel ultrasound-assisted dispersive liquid-liquid microextraction method.

Science.gov (United States)

Cai, Kai; Hu, Deyu; Lei, Bo; Zhao, Huina; Pan, Wenjie; Song, Baoan

2015-07-02

A novel derivatization-ultrasonic assisted-dispersive liquid-liquid microextraction (UA-DLLME) method for the simultaneous determination of 11 main carbohydrates in tobacco has been developed. The combined method involves pressurized liquid extraction (PLE), derivatization, and UA-DLLME, followed by the analysis of the main carbohydrates with a gas chromatography-flame ionization detector (GC-FID). First, the PLE conditions were optimized using a univariate approach. Then, the derivatization methods were properly compared and optimized. The aldononitrile acetate method combined with the O-methoxyoxime-trimethylsilyl method was used for derivatization. Finally, the critical variables affecting the UA-DLLME extraction efficiency were searched using fractional factorial design (FFD) and further optimized using Doehlert design (DD) of the response surface methodology. The optimum conditions were found to be 44 μL for CHCl3, 2.3 mL for H2O, 11% w/v for NaCl, 5 min for the extraction time and 5 min for the centrifugation time. Under the optimized experimental conditions, the detection limit of the method (LODs) and linear correlation coefficient were found to be in the range of 0.06-0.90 μg mL(-1) and 0.9987-0.9999. The proposed method was successfully employed to analyze three flue-cured tobacco cultivars, among which the main carbohydrate concentrations were found to be very different. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous determination of organophosphorus pesticides and phthalates in baby food samples by ultrasound-vortex-assisted liquid-liquid microextraction and GC-IT/MS.

Science.gov (United States)

Notardonato, Ivan; Salimei, Elisabetta; Russo, Mario Vincenzo; Avino, Pasquale

2018-05-01

Baby foods are either a soft, liquid paste or an easily chewed food since babies lack developed muscles and teeth to chew effectively. Babies typically move to consuming baby food once nursing or formula is not sufficient for the child's appetite. Some commercial baby foods have been criticized for their contents. This article focuses on the simultaneous determination of organophosphorus pesticides and phthalates by means of a method based on ultrasound-vortex-assisted liquid-liquid microextraction coupled with gas chromatography-ion trap mass spectrometry (GC-IT/MS). The protocol developed allowed the determination of six phthalates [dimethyl phthalate, diethyl phthalate, dibutyl phthalate, isobutyl cyclohexyl phthalate, benzyl butyl phthalate, bis(2-ethylhexyl) phthalate] and 19 organophosphorus pesticides. Freeze-dried product samples (0.1-0.2 g) were dissolved in 10 mL of warm distilled water along with 5 μL of an internal standard (anthracene at 10 mg mL -1 in acetone): the choice of extraction solvent was studied, with the most suitable being n-heptane, which is used for phthalate determination in similar matrices. The solution, held for 5 min in a vortex mixer and for 6 min in a 100-W ultrasonic bath to favor solvent dispersion and consequently analyte extraction, was centrifuged at 4000 rpm for 30 min. Then 1 μL was injected into the GC-IT/MS system (SE-54 capillary column; length 30 m, inner diameter 250 μm, film thickness 0.25 μm). All analytical parameters investigated are discussed in depth. The method was applied to real commercial freeze-dried samples: significant contaminant concentrations were not found. Graphical abstract Simultaneous and sensitive determination of organophosphorus pesticides and phthalates in baby foods by the ultrasound-vortex-assisted liquid-liquid microextraction ֪gas chromatography-ion trap mass spectrometry procedure. 1 methacrifos, 2 pirofos, 3 phorate, 4 seraphos, 5 diazinon, 6 etrimphos, 7 dichlofenthion, 8

Magnetic matrix solid phase dispersion assisted dispersive liquid liquid microextraction of ultra trace polychlorinated biphenyls in water prior to GC-ECD determination

International Nuclear Information System (INIS)

Diao, Chunpeng; Li, Cong; Yang, Xiao; Sun, Ailing; Liu, Renmin

2016-01-01

Magnetic matrix solid phase dispersion (MMSPD) assisted dispersive liquid liquid microextraction (DLLME) was applied to extract ultra traces of polychlorinated biphenyls (PCBs) from water samples prior to gas chromatography with electron capture detection. PCBs in water were adsorbed by micro particles of magnetic bamboo charcoal and then transferred into the elution solvent. PCBs in the elution solvent of the MMSPD were further concentrated into trace volume extraction solvent of the DLLME procedure. Under optimized conditions, good linearity in the range of 0.2–100 ng L"−"1 was obtained with regression coefficients (r) higher than 0.9987. Based on a signal-noise ratio of 3, the limits of detection (LODs) range from 0.05–0.1 ng L"−"1. These LODs are much lower than those of MMSPD or DLLME alone. Relative standard deviations are between 4.9–8.2 %. The method was successfully applied to the determination of PCBs in lake and river water. Relative recoveries were 85.5–117.4 % for the spiked environmental water samples. (author)

Sensitive determination of three aconitum alkaloids and their metabolites in human plasma by matrix solid-phase dispersion with vortex-assisted dispersive liquid-liquid microextraction and HPLC with diode array detection.

Science.gov (United States)

Wang, Xiaozhong; Li, Xuwen; Li, Lanjie; Li, Min; Liu, Ying; Wu, Qian; Li, Peng; Jin, Yongri

2016-05-01

A simple and sensitive method for determination of three aconitum alkaloids and their metabolites in human plasma was developed using matrix solid-phase dispersion combined with vortex-assisted dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection. The plasma sample was directly purified by matrix solid-phase dispersion and the eluate obtained was concentrated and further clarified by vortex-assisted dispersive liquid-liquid microextraction. Some important parameters affecting the extraction efficiency, such as type and amount of dispersing sorbent, type and volume of elution solvent, type and volume of extraction solvent, salt concentration as well as sample solution pH, were investigated in detail. Under optimal conditions, the proposed method has good repeatability and reproducibility with intraday and interday relative standard deviations lower than 5.44 and 5.75%, respectively. The recoveries of the aconitum alkaloids ranged from 73.81 to 101.82%, and the detection limits were achieved within the range of 1.6-2.1 ng/mL. The proposed method offered the advantages of good applicability, sensitivity, simplicity, and feasibility, which makes it suitable for the determination of trace amounts of aconitum alkaloids in human plasma samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid-phase extraction assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet to determine sildenafil and its analogues in dietary supplements.

Science.gov (United States)

Li, Jing; Roh, Si Hun; Shaodong, Jia; Hong, Ji Yeon; Lee, Dong-Kyu; Shin, Byong-Kyu; Park, Jeong Hill; Lee, Jeongmi; Kwon, Sung Won

2017-08-01

A novel analytical method for the simultaneous determination of the concentration of sildenafil and its five analogues in dietary supplements using solid-phase extraction assisted reversed-phase dispersive liquid-liquid microextraction based on solidification of floating organic droplet combined with ion-pairing liquid chromatography with an ultraviolet detector was developed. Parameters that affect extraction efficiency were systematically investigated, including the type of solid-phase extraction cartridge, pH of the extraction environment, and the type and volume of extraction and dispersive solvent. The method linearity was in the range of 5.0-100 ng/mL for sildenafil, homosildenafil, udenafil, benzylsildenafil, and thiosildenafil and 10-100 ng/mL for acetildenafil. The coefficients of determination were ≥0.996 for all regression curves. The sensitivity values expressed as limit of detection were between 2.5 and 7.5 ng/mL. Furthermore, intraday and interday precisions expressed as relative standard deviations were less than 5.7 and 9.9%, respectively. The proposed method was successfully applied to the analysis of sildenafil and its five analogues in complex dietary supplements. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microwave-assisted of dispersive liquid-liquid microextraction and spectrophotometric determination of uranium after optimization based on Box-Behnken design and chemometrics methods

Science.gov (United States)

Niazi, Ali; Khorshidi, Neda; Ghaemmaghami, Pegah

2015-01-01

In this study an analytical procedure based on microwave-assisted dispersive liquid-liquid microextraction (MA-DLLME) and spectrophotometric coupled with chemometrics methods is proposed to determine uranium. In the proposed method, 4-(2-pyridylazo) resorcinol (PAR) is used as a chelating agent, and chloroform and ethanol are selected as extraction and dispersive solvent. The optimization strategy is carried out by using two level full factorial designs. Results of the two level full factorial design (24) based on an analysis of variance demonstrated that the pH, concentration of PAR, amount of dispersive and extraction solvents are statistically significant. Optimal condition for three variables: pH, concentration of PAR, amount of dispersive and extraction solvents are obtained by using Box-Behnken design. Under the optimum conditions, the calibration graphs are linear in the range of 20.0-350.0 ng mL-1 with detection limit of 6.7 ng mL-1 (3δB/slope) and the enrichment factor of this method for uranium reached at 135. The relative standard deviation (R.S.D.) is 1.64% (n = 7, c = 50 ng mL-1). The partial least squares (PLS) modeling was used for multivariate calibration of the spectrophotometric data. The orthogonal signal correction (OSC) was used for preprocessing of data matrices and the prediction results of model, with and without using OSC, were statistically compared. MA-DLLME-OSC-PLS method was presented for the first time in this study. The root mean squares error of prediction (RMSEP) for uranium determination using PLS and OSC-PLS models were 4.63 and 0.98, respectively. This procedure allows the determination of uranium synthesis and real samples such as waste water with good reliability of the determination.

Microwave-assisted of dispersive liquid-liquid microextraction and spectrophotometric determination of uranium after optimization based on Box-Behnken design and chemometrics methods.

Science.gov (United States)

Niazi, Ali; Khorshidi, Neda; Ghaemmaghami, Pegah

2015-01-25

In this study an analytical procedure based on microwave-assisted dispersive liquid-liquid microextraction (MA-DLLME) and spectrophotometric coupled with chemometrics methods is proposed to determine uranium. In the proposed method, 4-(2-pyridylazo) resorcinol (PAR) is used as a chelating agent, and chloroform and ethanol are selected as extraction and dispersive solvent. The optimization strategy is carried out by using two level full factorial designs. Results of the two level full factorial design (2(4)) based on an analysis of variance demonstrated that the pH, concentration of PAR, amount of dispersive and extraction solvents are statistically significant. Optimal condition for three variables: pH, concentration of PAR, amount of dispersive and extraction solvents are obtained by using Box-Behnken design. Under the optimum conditions, the calibration graphs are linear in the range of 20.0-350.0 ng mL(-1) with detection limit of 6.7 ng mL(-1) (3δB/slope) and the enrichment factor of this method for uranium reached at 135. The relative standard deviation (R.S.D.) is 1.64% (n=7, c=50 ng mL(-1)). The partial least squares (PLS) modeling was used for multivariate calibration of the spectrophotometric data. The orthogonal signal correction (OSC) was used for preprocessing of data matrices and the prediction results of model, with and without using OSC, were statistically compared. MA-DLLME-OSC-PLS method was presented for the first time in this study. The root mean squares error of prediction (RMSEP) for uranium determination using PLS and OSC-PLS models were 4.63 and 0.98, respectively. This procedure allows the determination of uranium synthesis and real samples such as waste water with good reliability of the determination. Copyright © 2014. Published by Elsevier B.V.

Stability of Anthocyanins from Red Grape Skins under Pressurized Liquid Extraction and Ultrasound-Assisted Extraction Conditions

Directory of Open Access Journals (Sweden)

Ali Liazid

2014-12-01

Full Text Available The stability of anthocyanins from grape skins after applying different extraction techniques has been determined. The following compounds, previously extracted from real samples, were assessed: delphinidin 3-glucoside, cyanidin 3-glucoside, petunidin 3-glucoside, peonidin 3-glucoside, malvidin 3-glucoside, peonidin 3-acetylglucoside, malvidin 3-acetylglucoside, malvidin 3-caffeoylglucoside, petunidin 3-p-coumaroylglucoside and malvidin 3-p-coumaroylglucoside (trans. The techniques used were ultrasound-assisted extraction and pressurized liquid extraction. In ultrasound-assisted extraction, temperatures up to 75 °C can be applied without degradation of the aforementioned compounds. In pressurized liquid extraction the anthocyanins were found to be stable up to 100 °C. The relative stabilities of both the glycosidic and acylated forms were evaluated. Acylated derivatives were more stable than non-acylated forms. The differences between the two groups of compounds became more marked on working at higher temperatures and on using extraction techniques with higher levels of oxygen in the extraction media.

Determination of triazine herbicides in juice samples by microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography.

Science.gov (United States)

Su, Rui; Li, Dan; Wu, Lijie; Han, Jing; Lian, Wenhui; Wang, Keren; Yang, Hongmei

2017-07-01

A novel microextraction method, termed microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction, has been developed for the rapid enrichment and analysis of triazine herbicides in fruit juice samples by high-performance liquid chromatography. Instead of using hazardous organic solvents, two kinds of ionic liquids, a hydrophobic ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) and a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate), were used as the extraction solvent and dispersion agent, respectively, in this method. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of 1-hexyl-3-methylimidazolium hexafluorophosphate dispersed entirely into sample solution with the help of 1-butyl-3-methylimidazolium tetrafluoroborate. In addition, an ion-pairing agent (NH 4 PF 6 ) was introduced to improve recoveries of the ionic liquid phase. Several experimental parameters that might affect the extraction efficiency were investigated. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 5.00-250.00 μg/L, with the correlation coefficients of 0.9982-0.9997. The practical application of this effective and green method is demonstrated by the successful analysis of triazine herbicides in four juice samples, with satisfactory recoveries (76.7-105.7%) and relative standard deviations (lower than 6.6%). In general, this method is fast, effective, and robust to determine triazine herbicides in juice samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A fully automated effervescence assisted dispersive liquid–liquid microextraction based on a stepwise injection system. Determination of antipyrine in saliva samples

Energy Technology Data Exchange (ETDEWEB)

Medinskaia, Kseniia; Vakh, Christina; Aseeva, Darina [Department of Analytical Chemistry, Institute of Chemistry, Saint Petersburg State University, RU-198504 Saint Petersburg (Russian Federation); Andruch, Vasil, E-mail: vasil.andruch@upjs.sk [Department of Analytical Chemistry, University of P.J. Šafárik, SK-04154 Košice (Slovakia); Moskvin, Leonid [Department of Analytical Chemistry, Institute of Chemistry, Saint Petersburg State University, RU-198504 Saint Petersburg (Russian Federation); Bulatov, Andrey, E-mail: bulatov_andrey@mail.ru [Department of Analytical Chemistry, Institute of Chemistry, Saint Petersburg State University, RU-198504 Saint Petersburg (Russian Federation)

2016-01-01

A first attempt to automate the effervescence assisted dispersive liquid–liquid microextraction (EA-DLLME) has been reported. The method is based on the aspiration of a sample and all required aqueous reagents into the stepwise injection analysis (SWIA) manifold, followed by simultaneous counterflow injection of the extraction solvent (dichloromethane), the mixture of the effervescence agent (0.5 mol L{sup −1} Na{sub 2}CO{sub 3}) and the proton donor solution (1 mol L{sup −1} CH{sub 3}COOH). Formation of carbon dioxide microbubbles generated in situ leads to the dispersion of the extraction solvent in the whole aqueous sample and extraction of the analyte into organic phase. Unlike the conventional DLLME, in the case of EA-DLLME, the addition of dispersive solvent, as well as, time consuming centrifugation step for disruption of the cloudy state is avoided. The phase separation was achieved by gentle bubbling of nitrogen stream (2 mL min{sup −1} during 2 min). The performance of the suggested approach is demonstrated by determination of antipyrine in saliva samples. The procedure is based on the derivatization of antipyrine by nitrite-ion followed by EA-DLLME of 4-nitrosoantipyrine and subsequent UV–Vis detection using SWIA manifold. The absorbance of the yellow-colored extract at the wavelength of 345 nm obeys Beer's law in the range of 1.5–100 µmol L{sup −1} of antipyrine in saliva. The LOD, calculated from a blank test based on 3σ, was 0.5 µmol L{sup −1}. - Highlights: • First attempt to automate the effervescence assisted dispersive liquid–liquid microextraction. • Automation based on Stepwise injection analysis manifold in flow batch system. • Counterflow injection of extraction solvent and the effervescence agent. • Phase separation performed by gentle bubbling of nitrogen. • Application for the determination of antipyrine in saliva samples.

A fully automated effervescence assisted dispersive liquid–liquid microextraction based on a stepwise injection system. Determination of antipyrine in saliva samples

International Nuclear Information System (INIS)

Medinskaia, Kseniia; Vakh, Christina; Aseeva, Darina; Andruch, Vasil; Moskvin, Leonid; Bulatov, Andrey

2016-01-01

A first attempt to automate the effervescence assisted dispersive liquid–liquid microextraction (EA-DLLME) has been reported. The method is based on the aspiration of a sample and all required aqueous reagents into the stepwise injection analysis (SWIA) manifold, followed by simultaneous counterflow injection of the extraction solvent (dichloromethane), the mixture of the effervescence agent (0.5 mol L"−"1 Na_2CO_3) and the proton donor solution (1 mol L"−"1 CH_3COOH). Formation of carbon dioxide microbubbles generated in situ leads to the dispersion of the extraction solvent in the whole aqueous sample and extraction of the analyte into organic phase. Unlike the conventional DLLME, in the case of EA-DLLME, the addition of dispersive solvent, as well as, time consuming centrifugation step for disruption of the cloudy state is avoided. The phase separation was achieved by gentle bubbling of nitrogen stream (2 mL min"−"1 during 2 min). The performance of the suggested approach is demonstrated by determination of antipyrine in saliva samples. The procedure is based on the derivatization of antipyrine by nitrite-ion followed by EA-DLLME of 4-nitrosoantipyrine and subsequent UV–Vis detection using SWIA manifold. The absorbance of the yellow-colored extract at the wavelength of 345 nm obeys Beer's law in the range of 1.5–100 µmol L"−"1 of antipyrine in saliva. The LOD, calculated from a blank test based on 3σ, was 0.5 µmol L"−"1. - Highlights: • First attempt to automate the effervescence assisted dispersive liquid–liquid microextraction. • Automation based on Stepwise injection analysis manifold in flow batch system. • Counterflow injection of extraction solvent and the effervescence agent. • Phase separation performed by gentle bubbling of nitrogen. • Application for the determination of antipyrine in saliva samples.

Determination of phenolic acids and flavonoids in raw propolis by silica-supported ionic liquid-based matrix solid phase dispersion extraction high performance liquid chromatography-diode array detection.

Science.gov (United States)

Wang, Zhibing; Sun, Rui; Wang, Yuanpeng; Li, Na; Lei, Lei; Yang, Xiao; Yu, Aimin; Qiu, Fangping; Zhang, Hanqi

2014-10-15

The silica-supported ionic liquid (S-SIL) was prepared by impregnation and used as the dispersion adsorbent of matrix solid phase dispersion (MSPD) for the simultaneous extraction of eight phenolic acids and flavonoids, including caffeic acid, ferulic acid, morin, luteolin, quercetin, apigenin, chrysin, and kaempferide in raw propolis. High performance liquid chromatography with a Zorbax SB-C18 column (150mm×4.6mm, 3.5μm) was used for separation of the analytes. The mobile phase consisted of 0.2% phosphoric acid aqueous solution and acetonitrile and the flow rate of the mobile phase was 0.5mL/min. The experimental conditions for silica-supported ionic liquid-based matrix solid phase dispersion (S-SIL-based MSPD) were optimized. S-SIL containing 10% [C6MIM]Cl was used as dispersant, 20mL of n-hexane as washing solvent and 15mL of methanol as elution solvent. The ratio of S-SIL to sample was selected to be 4:1. The standard curves showed good linear relationship (r>0.9995). The limits of detection and quantification were in the range of 5.8-22.2ngmL(-1) and 19.2-74.0ngmL(-1), respectively. The relative standard deviations (RSDs) of intra-day and inter-day determination were lower than 8.80% and 11.19%, respectively. The recoveries were between 65.51% and 92.32% with RSDs lower than 8.95%. Compared with ultrasound-assisted extraction (UAE) and soxhlet extraction, the present method consumed less sample, organic solvent, and extraction time, although the extraction yields obtained by S-SIL-based MSPD are slightly lower than those obtained by UAE. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

Altunay, Nail; Yıldırım, Emre; Gürkan, Ramazan

2018-04-15

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

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

Science.gov (United States)

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

2014-12-01

A series of novel tetramethylguanidinium ionic liquids and hexaalkylguanidinium ionic liquids have been synthesized based on 1,1,3,3-tetramethylguanidine. The structures of the ionic liquids were confirmed by (1)H NMR spectroscopy and mass spectrometry. A green guanidinium ionic liquid based microwave-assisted extraction method has been developed with these guanidinium ionic liquids for the effective extraction of Praeruptorin A from Radix peucedani. After extraction, reversed-phase high-performance liquid chromatography with UV detection was employed for the analysis of Praeruptorin A. Several significant operating parameters were systematically optimized by single-factor and L9 (3(4)) orthogonal array experiments. The amount of Praeruptorin A extracted by [1,1,3,3-tetramethylguanidine]CH2CH(OH)COOH is the highest, reaching 11.05 ± 0.13 mg/g. Guanidinium ionic liquid based microwave-assisted extraction presents unique advantages in Praeruptorin A extraction compared with guanidinium ionic liquid based maceration extraction, guanidinium ionic liquid based heat reflux extraction and guanidinium ionic liquid based ultrasound-assisted extraction. The precision, stability, and repeatability of the process were investigated. The mechanisms of guanidinium ionic liquid based microwave-assisted extraction were researched by scanning electron microscopy and IR spectroscopy. All the results show that guanidinium ionic liquid based microwave-assisted extraction has a huge potential in the extraction of bioactive compounds from complex samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultrasound-Assisted Transient Liquid Phase Bonding of Magnesium Alloy Using Brass Interlayer in Air

Institute of Scientific and Technical Information of China (English)

Zhiwei Lai; Ruishan Xie; Chuan Pan; Xiaoguang Chen; Lei Liu; Wenxian Wang; Guisheng Zou

2017-01-01

The microstructure evolution and oxide film behavior in ultrasound-assisted transient liquid phase (U-TLP) bonding of Mg alloy were investigated by applying different ultrasonic time at 460℃ withbrass interlayer in air.The results indicated that with increasing ultrasonic time,brass interlayer disappeared gradually and the Mg-Cu-Zn eutectic compounds were formed.The eutectic compounds in the joint decreased as the ultrasonic time increased further.The oxide removal process was divided into four steps.Continuous oxide film at the interface was partially fractured by ultrasonic vibration,and then suspended into liquid by undermining eutectic reaction.After that,the suspended oxide film was broken into small oxide fragments by ultrasonic cavitation effect,which was finally squeezed out of the joint by ultrasonic squeeze action.In addition,the mechanical properties of the joints were investigated.The maximum shear strength of the joint reached 105 MPa,which was 100％ of base metal.

A Facile Vortex-Assisted Dispersive Liquid-Liquid Microextraction Method for the Determination of Uranyl Ion at Low Levels by Spectrophotometry.

Science.gov (United States)

Corazza, Marcela Zanetti; Pires, Igor Matheus Ruiz; Diniz, Kristiany Moreira; Segatelli, Mariana Gava; Tarley, César Ricardo Teixeira

2015-08-01

A facile and reliable UV-Vis spectrophotometric method associated with vortex-assisted dispersive liquid-liquid microextraction has been developed and applied to the determination of U(VI) at low levels in water samples. It was based on preconcentration of 24.0 mL sample at pH 8.0 in the presence of 7.4 µmol L(-1) 1-(2-pyridylazo)-2-naphthol, 1.0 mL of methanol as disperser solvent and 1.0 mL of chloroform as extraction solvent. A high preconcentration factor was achieved (396 times), thus providing a wide analytical curve from 6.9 up to 75.9 µg L(-1) (r=0.9982) and limits of detection and quantification of 0.40 and 1.30 µg L(-1), respectively. When necessary, EDTA or KCN can be used to remove interferences of foreign ions. The method was applied to the analysis of real water samples, such as tap, mineral and lake waters with good recovery values.

Alternative solvent-based methyl benzoate vortex-assisted dispersive liquid-liquid microextraction for the high-performance liquid chromatographic determination of benzimidazole fungicides in environmental water samples.

Science.gov (United States)

Santaladchaiyakit, Yanawath; Srijaranai, Supalax

2014-11-01

Vortex-assisted dispersive liquid-liquid microextraction using methyl benzoate as an alternative extraction solvent for extracting and preconcentrating three benzimidazole fungicides (i.e., carbendazim, thiabendazole, and fluberidazole) in environmental water samples before high-performance liquid chromatographic analysis has been developed. The selected microextraction conditions were 250 μL of methyl benzoate containing 300 μL of ethanol, 1.0% w/v sodium acetate, and vortex agitation speed of 2100 rpm for 30 s. Under optimum conditions, preconcentration factors were 14.5-39.0 for the target fungicides. Limits of detection were obtained in the range of 0.01-0.05 μg/L. The proposed method was then applied to surface water samples and the recovery evaluations at three spiked concentration levels of 5, 30, and 50 μg/L were obtained in the range of 77.4-110.9% with the relative standard deviation water samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effervescence-assisted dispersive liquid-liquid microextraction using a solid effervescent agent as a novel dispersion technique for the analysis of fungicides in apple juice.

Science.gov (United States)

Jiang, Wenqing; Chen, Xiaochu; Liu, Fengmao; You, Xiangwei; Xue, Jiaying

2014-11-01

A novel effervescence-assisted dispersive liquid-liquid microextraction method has been developed for the determination of four fungicides in apple juice samples. In this method, a solid effervescent agent is added into samples to assist the dispersion of extraction solvent. The effervescent agent is environmentally friendly and only produces an increase in the ionic strength and a negligible variation in the pH value of the aqueous sample, which does not interfere with the extraction of the analytes. The parameters affecting the extraction efficiency were investigated including the composition of effervescent agent, effervescent agent amount, formulation of effervescent agent, adding mode of effervescent agent, type and volume of extraction solvent, and pH. Under optimized conditions, the method showed a good linearity within the range of 0.05-2 mg/L for pyrimethanil, fludioxonil, and cyprodinil, and 0.1-4 mg/L for kresoxim-methyl, with the correlation coefficients >0.998. The limits of detection for the method ranged between 0.005 and 0.01 mg/L. The recoveries of the target fungicides in apple juice samples were in the range of 72.4-110.8% with the relative standard deviations ranging from 1.2 to 6.8%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Dual ultrasonic-assisted dispersive liquid-liquid microextraction coupled with microwave-assisted derivatization for simultaneous determination of 20(S)-protopanaxadiol and 20(S)-protopanaxatriol by ultra high performance liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Zhao, Xian-En; Lv, Tao; Zhu, Shuyun; Qu, Fei; Chen, Guang; He, Yongrui; Wei, Na; Li, Guoliang; Xia, Lian; Sun, Zhiwei; Zhang, Shijuan; You, Jinmao; Liu, Shu; Liu, Zhiqiang; Sun, Jing; Liu, Shuying

2016-03-11

This paper, for the first time, reported a speedy hyphenated technique of low toxic dual ultrasonic-assisted dispersive liquid-liquid microextraction (dual-UADLLME) coupled with microwave-assisted derivatization (MAD) for the simultaneous determination of 20(S)-protopanaxadiol (PPD) and 20(S)-protopanaxatriol (PPT). The developed method was based on ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) detection using multiple-reaction monitoring (MRM) mode. A mass spectrometry sensitizing reagent, 4'-carboxy-substituted rosamine (CSR) with high reaction activity and ionization efficiency was synthesized and firstly used as derivatization reagent. Parameters of dual-UADLLME, MAD and UHPLC-MS/MS conditions were all optimized in detail. Low toxic brominated solvents were used as extractant instead of traditional chlorinated solvents. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect and extremely low limits of detection (LODs, 0.010 and 0.015ng/mL for PPD and PPT, respectively) were achieved. The main advantages were rapid, sensitive and environmentally friendly, and exhibited high selectivity, accuracy and good matrix effect results. The proposed method was successfully applied to pharmacokinetics of PPD and PPT in rat plasma. Copyright © 2016 Elsevier B.V. All rights reserved.

Ultrasound-Assisted Extraction of Total Phenolic Compounds from Inula helenium

Directory of Open Access Journals (Sweden)

Jin Wang

2013-01-01

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

Influence of High Shear Dispersion on the Production of Cellulose Nanofibers by Ultrasound-Assisted TEMPO-Oxidation of Kraft Pulp

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Claude Daneault

2012-09-01

Full Text Available Cellulose nanofibers can be produced using a combination of TEMPO, sodium bromide (NaBr and sodium hypochlorite, and mechanical dispersion. Recently, this process has been the subject of intensive investigation. However, studies on the aspects of mechanical treatment of this process remain marginal. The main objective of this study is to evaluate the high shear dispersion parameters (e.g., consistency, stator-rotor gap, recirculation rate and pH and determine their influences on nanocellulose production using ultrasound-assisted TEMPO-oxidation of Kraft pulp. All nanofiber gels produced in this study exhibited rheological behaviors known as shear thinning. From all the dispersion parameters, the following conditions were identified as optimal: 0.042 mm stator-rotor gap, 200 mL/min recycle rate, dispersion pH of 7 and a feed consistency of 2%. High quality cellulose gel could be produced under these conditions. This finding is surely of great interest for the pulp and paper industry.

Ultrasound-assisted extraction of fructans from agave (Agave tequilana Weber var. azul at different ultrasound powers and solid-liquid ratios

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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.

Evaluation and application of microwave-assisted extraction and dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for the determination of polar heterocyclic aromatic amines in hamburger patties.

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Aeenehvand, Saeed; Toudehrousta, Zahra; Kamankesh, Marzieh; Mashayekh, Morteza; Tavakoli, Hamid Reza; Mohammadi, Abdorreza

2016-01-01

This study developed an analytical method based on microwave-assisted extraction and dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for the determination of three polar heterocyclic aromatic amines from hamburger patties. Effective parameters controlling the performance of the microextraction process, such as the type and volume of extraction and disperser solvents, microwave time, nature of alkaline aqueous solution, pH and salt amount, were optimized. The calibration graphs were linear in the range of 1-200 ng g(-1), with a coefficient of determination (R(2)) better than 0.9993. The relative standard deviations (RSD) for seven analyses were between 3.2% and 6.5%. The recoveries of those compounds in hamburger patties were from 90% to 105%. Detection limits were between 0.06 and 0.21 ng g(-1). A comparison of the proposed method with the existing literature demonstrates that it is a simple, rapid, highly selective and sensitive, and it gives good enrichment factors and detection limits for determining HAAs in real hamburger patties samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

Air-assisted dispersive liquid-liquid microextraction based on a new hydrophobic deep eutectic solvent for the preconcentration of benzophenone-type UV filters from aqueous samples.

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Ge, Dandan; Zhang, Yi; Dai, Yixiu; Yang, Shumin

2018-04-01

Deep eutectic solvents are considered as new and green solvents that can be widely used in analytical chemistry such as microextraction. In the present work, a new dl-menthol-based hydrophobic deep eutectic solvent was synthesized and used as extraction solvents in an air-assisted dispersive liquid-liquid microextraction method for preconcentration and extraction of benzophenone-type UV filters from aqueous samples followed by high-performance liquid chromatography with diode array detection. In an experiment, the deep eutectic solvent formed by dl-menthol and decanoic acid was added to an aqueous solution containing the UV filters, and then the mixture was sucked up and injected five times by using a glass syringe, and a cloudy state was achieved. After extraction, the solution was centrifuged and the upper phase was subjected to high-performance liquid chromatography for analysis. Various parameters such as the type and volume of the deep eutectic solvent, number of pulling, and pushing cycles, solution pH and salt concentration were investigated and optimized. Under the optimum conditions, the developed method exhibited low limits of detection and limits of quantitation, good linearity, and precision. Finally, the proposed method was successfully applied to determine the benzophenone-type filters in environmental water samples with relative recoveries of 88.8-105.9%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quantitation of tetrabromobisphenol-A from dust sampled on consumer electronics by dispersed liquid-liquid microextraction

International Nuclear Information System (INIS)

Di Napoli-Davis, Gina; Owens, Janel E.

2013-01-01

Tetrabromobisphenol-A (TBBPA) is a brominated flame retardant used worldwide. Despite its widespread use, there are few data concerning environmental concentrations of TBBPA. Thus, the objective of this work was to optimize an ultrasound-assisted dispersed liquid-liquid microextraction (DLLME) method to analyze swabbed surfaces of consumer electronics to determine TBBPA concentrations. Upon sample preparation with DLLME, TBBPA was derivatized with acetic anhydride and then analyzed by gas chromatography–mass spectrometry (GC/MS). Using a 13 C 12 -TBBPA internal standard to improve precision and quantitation, a recovery study was performed. At concentrations of 250–1000 ng/mL, recoveries were 104–106%. Sample preparation with solid phase extraction had comparable recoveries, although overall, improved analyte recovery and precision were achieved with DLLME. In a small survey study, TBBPA concentrations in dust collected from 100 cm 2 areas on electronic surfaces (monitor, microwave, refrigerator, and TV) were determined to range from less than the LOQ to 523 ng/mL. -- Highlights: •Tetrabromobisphenol-A (TBBPA) concentrations in dust samples were determined. •Dust samples were collected from surfaces of consumer electronics. •Dispersed liquid-liquid microextraction was used to prepare samples for GC/MS. •A 13 C 12 -labeled internal standard was used to improve precision and quantitation. •TBBPA was found in dust samples at levels below LOQ to 523 ng/mL. -- This work describes the analysis of the brominated flame retardant, tetrabromobisphenol-A (TBBPA), from dust sampled on surfaces of consumer electronics

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

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Ruan, Chunqiang; Zhao, Xiang; Liu, Chenglan

2015-09-01

In this study, a simple and low-organic-solvent-consuming method combining an acetonitrile-partitioning extraction procedure followed by "quick, easy, cheap, effective, rugged and safe" cleanup with ionic-liquid-based dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic-liquid-based dispersive liquid-liquid microextraction was performed using the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid-liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An Ion-pair Dispersive Liquid-Liquid Microextraction for Simultaneous Determination of Synthetic Dyes in Ice Cream Samples by HPLC

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Mohammad Faraji

2017-05-01

Full Text Available An efficient, sensitive and fast method was developed based on an ultrasound-assisted extraction followed by an ion-pair dispersive liquid-liquid microextraction (USAE-IP-DLLME for the simultaneous determination of five commonly used synthetic sulfonate dyes (tartarazine, quinoline yellow, sunset yellow, azorubine, and brilliant blue in ice cream samples using high performance liquid chromatography. First, important parameters on USAE and samples clean-up were investigated and optimized. Then, some effective parameters on DLLME were studied and optimized. Under the optimum conditions, good linearity (0.5–1000 µg L-1, > r2=0.99 were obtained for the dyes. Limits of detection and limits of quantization were in the range of 0.01–0.05 µg L-1 and 0.03–0.15 µg L-1, respectively. The recoveries of the five synthetic colorants ranged from 90.3 to 109.7%. Intra (1.4–6.4% and inter-day precision (3.9–9.7% expressed as relative standard deviation (RSD at 10 and 100 µg L-1 levels less than 10% were also achieved. Finally, this method has been applied successfully in the determination of the colorants in the ice cream samples.

Nanoparticle dispersion in liquid metals by electromagnetically induced acoustic cavitation

International Nuclear Information System (INIS)

Kaldre, Imants; Bojarevičs, Andris; Grants, Ilmārs; Beinerts, Toms; Kalvāns, Matīss; Milgrāvis, Mikus; Gerbeth, Gunter

2016-01-01

Aim of this study is to investigate experimentally the effect of magnetically induced cavitation applied for the purpose of nanoparticle dispersion in liquid metals. The oscillating magnetic force due to the azimuthal induction currents and the axial magnetic field excites power ultrasound in the sample. If the fields are sufficiently high then it is possible to achieve the acoustic cavitation threshold in liquid metals. Cavitation bubble collapses are known to create microscale jets with a potential to break nanoparticle agglomerates and disperse them. The samples are solidified under the contactless ultrasonic treatment and later analyzed by electron microscopy and energy-dispersive X-ray spectroscopy (EDX). It is observed that SiC nanoparticles are dispersed in an aluminum magnesium alloy, whereas in tin the same particles remain agglomerated in micron-sized clusters despite a more intense cavitation.

Rapid determination of triclosan in personal care products using new in-tube based ultrasound-assisted salt-induced liquid-liquid microextraction coupled with high performance liquid chromatography-ultraviolet detection.

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Chen, Ming-Jen; Liu, Ya-Ting; Lin, Chiao-Wen; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

2013-03-12

This paper describes the development of a novel, simple and efficient in-tube based ultrasound-assisted salt-induced liquid-liquid microextraction (IT-USA-SI-LLME) technique for the rapid determination of triclosan (TCS) in personal care products by high performance liquid chromatography-ultraviolet (HPLC-UV) detection. IT-USA-SI-LLME method is based on the rapid phase separation of water-miscible organic solvent from the aqueous phase in the presence of high concentration of salt (salting-out phenomena) under ultrasonication. In the present work, an indigenously fabricated home-made glass extraction device (8-mL glass tube inbuilt with a self-scaled capillary tip) was utilized as the phase separation device for USA-SI-LLME. After the extraction, the upper extractant layer was narrowed into the self-scaled capillary tip by pushing the plunger plug; thus, the collection and measurement of the upper organic solvent layer was simple and convenient. The effects of various parameters on the extraction efficiency were thoroughly evaluated and optimized. Under optimal conditions, detection was linear in the concentration range of 0.4-100ngmL(-1) with correlation coefficient of 0.9968. The limit of detection was 0.09ngmL(-1) and the relative standard deviations ranged between 0.8 and 5.3% (n=5). The applicability of the developed method was demonstrated for the analysis of TCS in different commercial personal care products and the relative recoveries ranged from 90.4 to 98.5%. The present method was proven to be a simple, sensitive, less organic solvent consuming, inexpensive and rapid procedure for analysis of TCS in a variety of commercially available personal care products or cosmetic preparations. Copyright © 2013 Elsevier B.V. All rights reserved.

Liquid dispersion in trickle-bed reactors with gas-liquid cocurrent downflow

International Nuclear Information System (INIS)

Chu, C.F.; Ng, K.M.

1986-01-01

The flow pattern can deviate from ideal plug flow in both trickling and pulsing flows. The liquid dispersion in those flow regimes are investigated separately, as the mechanisms causing the deviation of flow pattern from plug flow are different. In trickling flow, the dispersion of the liquid phase occurs in the flow path which is determined with computer-generated packed column. Dispersion in pulsing flow is studied with a combination of the method of characteristics and analysis of liquid dispersion in the liquid slug and gas pulse. The axial dispersion coefficients are then determined based on Monte Carlo simulation. Finally, liquid dispersion in trickle beds containing porous packings is also discussed

Ultrasound-assisted dyeing of cellulose acetate.

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Udrescu, C; Ferrero, F; Periolatto, M

2014-07-01

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

Application and optimization of microwave-assisted extraction and dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for sensitive determination of polyamines in turkey breast meat samples.

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Bashiry, Moein; Mohammadi, Abdorreza; Hosseini, Hedayat; Kamankesh, Marzieh; Aeenehvand, Saeed; Mohammadi, Zaniar

2016-01-01

A novel method based on microwave-assisted extraction and dispersive liquid-liquid microextraction (MAE-DLLME) followed by high-performance liquid chromatography (HPLC) was developed for the determination of three polyamines from turkey breast meat samples. Response surface methodology (RSM) based on central composite design (CCD) was used to optimize the effective factors in DLLME process. The optimum microextraction efficiency was obtained under optimized conditions. The calibration graphs of the proposed method were linear in the range of 20-200 ng g(-1), with the coefficient determination (R(2)) higher than 0.9914. The relative standard deviations were 6.72-7.30% (n = 7). The limits of detection were in the range of 0.8-1.4 ng g(-1). The recoveries of these compounds in spiked turkey breast meat samples were from 95% to 105%. The increased sensitivity in using the MAE-DLLME-HPLC-UV has been demonstrated. Compared with previous methods, the proposed method is an accurate, rapid and reliable sample-pretreatment method. Copyright © 2015 Elsevier Ltd. All rights reserved.

Ultrasound-assisted oxidative desulfurization and denitrogenation of liquid hydrocarbon fuels: A critical review.

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Ja'fari, Mahsa; Ebrahimi, Seyedeh Leila; Khosravi-Nikou, Mohammad Reza

2018-01-01

Nowadays, a continuously worldwide concern for development of process to produce ultra-low sulfur and nitrogen fuels have been emerged. Typical hydrodesulfurization and hydrodenitrogenation technology deals with important difficulties such as high pressure and temperature operating condition, failure to treat some recalcitrant compounds and limitations to meet the stringent environmental regulations. In contrary an advanced oxidation process that is ultrasound assisted oxidative desulfurization and denitrogenation satisfies latest environmental regulations in much milder conditions with more efficiency. The present work deals with a comprehensive review on findings and development in the ultrasound assisted oxidative desulfurization and denitrogenation (UAOD) during the last decades. The role of individual parameters namely temperature, residence time, ultrasound power and frequency, pH, initial concentration and types of sulfur and nitrogen compounds on the efficiency are described. What's more another treatment properties that is role of phase transfer agent (PTA) and solvents of extraction step, reaction kinetics, mechanism of the ultrasound, fuel properties and recovery in UAOD are reviewed. Finally, the required future works to mature this technology are suggested. Copyright © 2017 Elsevier B.V. All rights reserved.

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

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

2018-01-15

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

Simultaneous determination of phenolic compounds in Equisetum palustre L. by ultra high performance liquid chromatography with tandem mass spectrometry combined with matrix solid-phase dispersion extraction.

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Wei, Zuofu; Pan, Youzhi; Li, Lu; Huang, Yuyang; Qi, Xiaolin; Luo, Meng; Zu, Yuangang; Fu, Yujie

2014-11-01

A method based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with tandem mass spectrometry is presented for the extraction and determination of phenolic compounds in Equisetum palustre. This method combines the high efficiency of matrix solid-phase dispersion extraction and the rapidity, sensitivity, and accuracy of ultra high performance liquid chromatography with tandem mass spectrometry. The influential parameters of the matrix solid-phase dispersion extraction were investigated and optimized. The optimized conditions were as follows: silica gel was selected as dispersing sorbent, the ratio of silica gel to sample was selected to be 2:1 (400/200 mg), and 8 mL of 80% methanol was used as elution solvent. Furthermore, a fast and sensitive ultra high performance liquid chromatography with tandem mass spectrometry method was developed for the determination of nine phenolic compounds in E. palustre. This method was carried out within <6 min, and exhibited satisfactory linearity, precision, and recovery. Compared with ultrasound-assisted extraction, the proposed matrix solid-phase dispersion procedure possessed higher extraction efficiency, and was more convenient and time saving with reduced requirements on sample and solvent amounts. All these results suggest that the developed method represents an excellent alternative for the extraction and determination of active components in plant matrices. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Trace determination of safranin O dye using ultrasound assisted dispersive solid-phase micro extraction: Artificial neural network-genetic algorithm and response surface methodology.

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Dil, Ebrahim Alipanahpour; Ghaedi, Mehrorang; Asfaram, Arash; Mehrabi, Fatemeh; Bazrafshan, Ali Akbar; Ghaedi, Abdol Mohammad

2016-11-01

In this study, ultrasound assisted dispersive solid-phase micro extraction combined with spectrophotometry (USA-DSPME-UV) method based on activated carbon modified with Fe2O3 nanoparticles (Fe2O3-NPs-AC) was developed for pre-concentration and determination of safranin O (SO). It is known that the efficiency of USA-DSPME-UV method may be affected by pH, amount of adsorbent, ultrasound time and eluent volume and the extent and magnitude of their contribution on response (in term of main and interaction part) was studied by using central composite design (CCD) and artificial neural network-genetic algorithms (ANN-GA). Accordingly by adjustment of experimental conditions suggested by ANN-GA at pH 6.5, 1.1mg of adsorbent, 10min ultrasound and 150μL of eluent volume led to achievement of best operation performance like low LOD (6.3ngmL(-1)) and LOQ (17.5ngmL(-1)) in the range of 25-3500ngmL(-1). In following stage, the SO content in real water and wastewater samples with recoveries between 93.27-99.41% with RSD lower than 3% was successfully determined. Copyright © 2016 Elsevier B.V. All rights reserved.

Semiconductor nanocrystals dispersed in imidazolium-based ionic liquids: a spectroscopic and morphological investigation

International Nuclear Information System (INIS)

Panniello, Annamaria; Binetti, Enrico; Ingrosso, Chiara; Curri, M. Lucia; Agostiano, Angela; Tommasi, Raffaele; Striccoli, Marinella

2013-01-01

A growing interest is devoted to the study of imidazolium-based ionic liquids as innovative materials to combine with functional elements for advanced technological applications. Materials based on semiconductor and oxide nanocrystals in ionic liquids can be promising for their integration in lithium batteries, as well as in innovative solar cells. Although the physical chemical properties and the solvation dynamics of bare ionic liquids have been extensively studied, their combination with colloidal nanocrystals still remains almost unexplored. Here, the optical properties of organic-capped luminescent cadmium selenide nanocrystals coated by a shell of zinc sulfide (CdSe(ZnS)) dispersed in 1,3-dialkyl imidazolium ionic liquids have been investigated, also in dependence of the alkyl chain length on the imidazolium ring and of the anion nature, by using both time-integrated and time-resolved optical spectroscopy. The observed variations in decay profiles of the ionic liquid in presence of colloidal nanocrystals suggest that the dispersion of the nanostructures induces modifications in the ionic liquid structural order. Finally, atomic force microscopy analysis has provided insight into the topography of the investigated dispersions deposited as film, confirming the organization of the ionic liquids in super-structures, also upon nanocrystal incorporation.

Detection of Organophosphorus Pesticides in Wheat by Ionic Liquid-Based Dispersive Liquid-Liquid Microextraction Combined with HPLC

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Wei Liu

2018-01-01

Full Text Available Food safety issues closely related to human health have always received widespread attention from the world society. As a basic food source, wheat is the fundamental support of human survival; therefore, the detection of pesticide residues in wheat is very necessary. In this work, the ultrasonic-assisted ionic liquid-dispersive liquid-liquid microextraction (DLLME method was firstly proposed, and the extraction and analysis of three organophosphorus pesticides were carried out by combining high-performance liquid chromatography (HPLC. The extraction efficiencies of three ionic liquids with bis(trifluoromethylsulfonylimide (Tf2N anion were compared by extracting organophosphorus in wheat samples. It was found that the use of 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonylimide ([OMIM][Tf2N] had both high enrichment efficiency and appropriate extraction recovery. Finally, the method was used for the determination of three wheat samples, and the recoveries of them were 74.8–112.5%, 71.8–104.5%, and 83.8–115.5%, respectively. The results show that the method proposed is simple, fast, and efficient, which can be applied to the extraction of organic matters in wheat samples.

Experimental analysis and modeling of ultrasound assisted freezing of potato spheres.

Science.gov (United States)

Kiani, Hossein; Zhang, Zhihang; Sun, Da-Wen

2015-09-01

In recent years, innovative methods such as ultrasound assisted freezing have been developed in order to improve the freezing process. During freezing of foods, accurate prediction of the temperature distribution, phase ratios, and process time is very important. In the present study, ultrasound assisted immersion freezing process (in 1:1 ethylene glycol-water solution at 253.15K) of potato spheres (0.02 m diameter) was evaluated using experimental, numerical and analytical approaches. Ultrasound (25 kHz, 890 W m(-2)) was irradiated for different duty cycles (DCs=0-100%). A finite volume based enthalpy method was used in the numerical model, based on which temperature and liquid fraction profiles were simulated by a program developed using OpenFOAM® CFD software. An analytical technique was also employed to calculate freezing times. The results showed that ultrasound irradiation could decrease the characteristic freezing time of potatoes. Since ultrasound irradiation increased the heat transfer coefficient but simultaneously generated heat at the surface of the samples, an optimum DC was needed for the shortest freezing time which occurred in the range of 30-70% DC. DCs higher than 70% increased the freezing time. DCs lower than 30% did not provide significant effects on the freezing time compared to the control sample. The numerical model predicted the characteristic freezing time in accordance with the experimental results. In addition, analytical calculation of characteristic freezing time exhibited qualitative agreement with the experimental results. As the numerical simulations provided profiles of temperature and water fraction within potatoes frozen with or without ultrasound, the models can be used to study and control different operation situations, and to improve the understanding of the freezing process. Copyright © 2015 Elsevier B.V. All rights reserved.

In-syringe-stirring: A novel approach for magnetic stirring-assisted dispersive liquid–liquid microextraction

International Nuclear Information System (INIS)

Horstkotte, Burkhard; Suárez, Ruth; Solich, Petr; Cerdà, Víctor

2013-01-01

Graphical abstract: -- Highlights: •We propose a new automatic magnetic stirring assisted dispersive liquid–liquid microextraction. •It allows the extraction of aluminum from seawater and freshwater samples within less than 4 min. •The method was applicable to the natural samples. -- Abstract: For the first time, the use of a magnetic stirrer within the syringe of an automated syringe pump and the resulting possible analytical applications are described. A simple instrumentation following roughly the one from sequential injection analyzer systems is used in combination with an adaptor, which is placed onto the barrel of a glass syringe. Swirling around the longitudinal axis of the syringe and holding two strong neodymium magnets, it causes a rotating magnetic field and serves as driver for a magnetic stirring bar placed inside of the syringe. In a first study it was shown that this approach leads to a sealed but also automatically adaptable reaction vessel, the syringe, in which rapid and homogeneous mixing of sample with the required reagents within short time can be carried out. In a second study in-a-syringe magnetic stirring-assisted dispersive liquid–liquid microextraction (MSA-DLLME) was demonstrated by the application of the analyzer system to fluorimetric determination of aluminum in seawater samples using lumogallion. A linear working range up to 1.1 μmol L −1 and a limit of detection of 6.1 nmol L −1 were found. An average recovery of 106.0% was achieved for coastal seawaters with a reproducibility of 4.4%. The procedure lasted 210 s including syringe cleaning and only 150 μL of hexanol and 4.1 mL of sample were required

Box-Behnken design based statistical modeling for ultrasound-assisted extraction of corn silk polysaccharide.

Science.gov (United States)

Prakash Maran, J; Manikandan, S; Thirugnanasambandham, K; Vigna Nivetha, C; Dinesh, R

2013-01-30

In this study, ultrasound assisted extraction (UAE) conditions on the yield of polysaccharide from corn silk were studied using three factors, three level Box-Behnken response surface design. Process parameters, which affect the efficiency of UAE such as extraction temperature (40-60 °C), time (10-30 min) and solid-liquid ratio (1:10-1:30 g/ml) were investigated. The results showed that, the extraction conditions have significant effects on extraction yield of polysaccharide. The obtained experimental data were fitted to a second-order polynomial equation using multiple regression analysis with high coefficient of determination value (R(2)) of 0.994. An optimization study using Derringer's desired function methodology was performed and the optimal conditions based on both individual and combinations of all independent variables (extraction temperature of 56 °C, time of 17 min and solid-liquid ratio of 1:20 g/ml) were determined with maximum polysaccharide yield of 6.06%, which was confirmed through validation experiments. Copyright © 2012 Elsevier Ltd. All rights reserved.

Liquid agents for dispersion of hard alloys

International Nuclear Information System (INIS)

Putintseva, M.N.

2006-01-01

Effects of dispersant properties on granulometric, chemical, and phase composition of the products of WC hard alloy electroerosion are considered. It is established that an increase of liquid dispersant permittivity results in enhanced powder dispersity, and an increase of boiling temperature and kinematic viscosity of a hydrocarbon liquid promotes a carbon loss from WC and intensifies pyrolysis of the liquid.On electroerosion of WC base hard alloy in oil a powder particle consists of b-WC+W 2 C phases, in kerosine - of a-WC+b-WC, in distilled water - of W+W 2 C. The viscosity of liquid dispersants practically has no effect on powder particle size [ru

Ultrasound-assisted dispersive magnetic solid phase extraction based on amino-functionalized Fe3O4 adsorbent for recovery of clomipramine from human plasma and its determination by high performance liquid chromatography: Optimization by experimental design.

Science.gov (United States)

Hamidi, Fatemeh; Hadjmohammadi, Mohammad Reza; Aghaie, Ali B G

2017-09-15

The applicability of Amino-functionalized Fe 3 O 4 nanoparticles (NPs) as an effective adsorbent was developed for the extraction and determination of clomipramine (CLP) in plasma sample by ultrasound-assisted dispersive magnetic solid phase extraction (UADM-SPE) and high-performance liquid chromatography-ultraviolet (HPLC-UV) detection. Fabrication of the Fe 3 O 4 @SiO 2 -NH 2 magnetic nanoparticles confirmed by Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The effect of different extraction parameters (i.e. pH of the sample solution, the amount of magnetic nanoparticles (MNPs), sample volume, temperature and sonication time) on the extraction recovery of CLP were investigated by response surface methodology through central composite design (CCD). The optimum condition is obtained when the affecting parameters are set to: pH of the sample solution=9, the amount of MNPs=37mg, sample volume=23mL, 25°C temperature and sonication time=1min. Under the optimum condition, extraction recovery was 90.6% with relative standard deviation of 3.5%, and enrichment factor of 117. The linear range for determination of CLP was 0.017-0.70mgL -1 with a determination coefficient (R 2 ) of 0.999. Limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.0167mgL -1 , respectively. The established UADM-SPE-HPLC-UV method was rapid, simple and efficient for determination of CLP in human plasma samples. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2018-02-01

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

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

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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

Fully-automated in-syringe dispersive liquid-liquid microextraction for the determination of caffeine in coffee beverages.

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Frizzarin, Rejane M; Maya, Fernando; Estela, José M; Cerdà, Víctor

2016-12-01

A novel fully-automated magnetic stirring-assisted lab-in-syringe analytical procedure has been developed for the fast and efficient dispersive liquid-liquid microextraction (DLLME) of caffeine in coffee beverages. The procedure is based on the microextraction of caffeine with a minute amount of dichloromethane, isolating caffeine from the sample matrix with no further sample pretreatment. Selection of the relevant extraction parameters such as the dispersive solvent, proportion of aqueous/organic phase, pH and flow rates have been carefully evaluated. Caffeine quantification was linear from 2 to 75mgL(-1), with detection and quantification limits of 0.46mgL(-1) and 1.54mgL(-1), respectively. A coefficient of variation (n=8; 5mgL(-1)) of a 2.1% and a sampling rate of 16h(-1), were obtained. The procedure was satisfactorily applied to the determination of caffeine in brewed, instant and decaf coffee samples, being the results for the sample analysis validated using high-performance liquid chromatography. Copyright © 2016 Elsevier Ltd. All rights reserved.

Carbon Nanofibers-Poly-3-hydroxyalkanoates Nanocomposite: Ultrasound-Assisted Dispersion and Thermostructural Properties

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A. M. Gumel

2014-01-01

Full Text Available The conductivity and high surface-to-volume ratio of carbon nanofibers (CNFs composited with the medium-chain-length poly-3-hydroxyalkanoate (mcl-PHA have attracted much attention as smart biomaterial. However, poor CNF dispersion leads to tactoid agglomerated composite with poor crystallite morphology resulting in inferior thermomechanical properties. We employed acoustic sonication to enhance the construction of exfoliated PHA/CNFs nanocomposites. The effects of CNF loading and the insonation variables (power intensity, frequency, and time on the stability and microscopic morphology of the nanocomposites were studied. Sonication improved the dispersion of CNFs into the polymer matrix, thereby improving the physical morphology, crystallinity, and thermomechanical properties of the nanocomposites. For example, compositing the polymer with 10% w/w CNF resulted in 66% increase in crystallite size, 46% increase in micromolecular elastic strain, and 17% increase in lattice strain. Nevertheless, polymer degradation was observed following the ultrasound exposure. The constructed bionanocomposite could potentially be applied for organic electroconductive materials, biosensors and stimuli-responsive drug delivery devices.

Actuator-Assisted Calibration of Freehand 3D Ultrasound System.

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Koo, Terry K; Silvia, Nathaniel

2018-01-01

Freehand three-dimensional (3D) ultrasound has been used independently of other technologies to analyze complex geometries or registered with other imaging modalities to aid surgical and radiotherapy planning. A fundamental requirement for all freehand 3D ultrasound systems is probe calibration. The purpose of this study was to develop an actuator-assisted approach to facilitate freehand 3D ultrasound calibration using point-based phantoms. We modified the mathematical formulation of the calibration problem to eliminate the need of imaging the point targets at different viewing angles and developed an actuator-assisted approach/setup to facilitate quick and consistent collection of point targets spanning the entire image field of view. The actuator-assisted approach was applied to a commonly used cross wire phantom as well as two custom-made point-based phantoms (original and modified), each containing 7 collinear point targets, and compared the results with the traditional freehand cross wire phantom calibration in terms of calibration reproducibility, point reconstruction precision, point reconstruction accuracy, distance reconstruction accuracy, and data acquisition time. Results demonstrated that the actuator-assisted single cross wire phantom calibration significantly improved the calibration reproducibility and offered similar point reconstruction precision, point reconstruction accuracy, distance reconstruction accuracy, and data acquisition time with respect to the freehand cross wire phantom calibration. On the other hand, the actuator-assisted modified "collinear point target" phantom calibration offered similar precision and accuracy when compared to the freehand cross wire phantom calibration, but it reduced the data acquisition time by 57%. It appears that both actuator-assisted cross wire phantom and modified collinear point target phantom calibration approaches are viable options for freehand 3D ultrasound calibration.

Simultaneous determination of atorvastatin and valsartan in human plasma by solid-based disperser liquid-liquid microextraction followed by high-performance liquid chromatography-diode array detection.

Science.gov (United States)

Farajzadeh, Mir Ali; Khorram, Parisa; Pazhohan, Azar

2016-04-01

A simple, sensitive, and efficient method has been developed for simultaneous estimation of valsartan and atorvastatin in human plasma by combination of solid-based dispersive liquid-liquid microextraction and high performance liquid chromatography-diode array detection. In the proposed method, 1,2-dibromoethane (extraction solvent) is added on a sugar cube (as a solid disperser) and it is introduced into plasma sample containing the analytes. After manual shaking and centrifugation, the resultant sedimented phase is subjected to back extraction into a small volume of sodium hydrogen carbonate solution using air-assisted liquid-liquid microextraction. Then the cloudy solution is centrifuged and the obtained aqueous phase is transferred into a microtube and analyzed by the separation system. Under the optimal conditions, extraction recoveries are obtained in the range of 81-90%. Calibration curves plotted in drug-free plasma sample are linear in the ranges of 5-5000μgL(-1) for valsartan and 10-5000μgL(-1) for atorvastatin with the coefficients of determination higher than 0.997. Limits of detection and quantification of the studied analytes in plasma sample are 0.30-2.6 and 1.0-8.2μgL(-1), respectively. Intra-day (n=6) and inter-days (n=4) precisions of the method are satisfactory with relative standard deviations less than 7.4% (at three levels of 10, 500, and 2000μgL(-1), each analyte). These data suggest that the method can be successfully applied to determine trace amounts of valsartan and atorvastatin in human plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

A novel ultrasound based technique for classifying gas bubble sizes in liquids

International Nuclear Information System (INIS)

Hussein, Walid; Khan, Muhammad Salman; Zamorano, Juan; Espic, Felipe; Yoma, Nestor Becerra

2014-01-01

Characterizing gas bubbles in liquids is crucial to many biomedical, environmental and industrial applications. In this paper a novel method is proposed for the classification of bubble sizes using ultrasound analysis, which is widely acknowledged for being non-invasive, non-contact and inexpensive. This classification is based on 2D templates, i.e. the average spectrum of events representing the trace of bubbles when they cross an ultrasound field. The 2D patterns are obtained by capturing ultrasound signals reflected by bubbles. Frequency-domain based features are analyzed that provide discrimination between bubble sizes. These features are then fed to an artificial neural network, which is designed and trained to classify bubble sizes. The benefits of the proposed method are that it facilitates the processing of multiple bubbles simultaneously, the issues concerning masking interference among bubbles are potentially reduced and using a single sinusoidal component makes the transmitter–receiver electronics relatively simpler. Results from three bubble sizes indicate that the proposed scheme can achieve an accuracy in their classification that is as high as 99%. (paper)

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

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

2017-09-01

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

Ionic liquid-based dispersive microextraction of nitro toluenes in water samples

International Nuclear Information System (INIS)

Berton, Paula; Regmi, Bishnu P.; Spivak, David A.; Warner, Isiah M.

2014-01-01

We describe a method for dispersive liquid-liquid microextraction of nitrotoluene-based compounds. This method is based on use of the room temperature ionic liquid (RTIL) 1-hexyl-4-methylpyridinium bis(trifluoromethylsulfonyl)imide as the accepting phase, and is shown to work well for extraction of 4-nitrotoluene, 2,4-dinitrotoluene, and 2,4,6-trinitrotoluene. Separation and subsequent detection of analytes were accomplished via HPLC with UV detection. Several parameters that influence the efficiency of the extraction were optimized using experimental design. In this regard, a Plackett–Burman design was used for initial screening, followed by a central composite design to further optimize the influencing variables. For a 5-mL water sample, the optimized IL-DLLME procedure requires 26 mg of the RTIL as extraction solvent and 680 μL of methanol as the dispersant. Under optimum conditions, limits of detection (LODs) are lower than 1.05 μg L −1 . Relative standard deviations for 6 replicate determinations at a 4 μg L −1 analyte level are <4.3 % (calculated using peak areas). Correlation coefficients of >0.998 were achieved. This method was successfully applied to extraction and determination of nitrotoluene-based compounds in spiked tap and lake water samples. (author)

An efficient ultrasound assisted approach for the impregnation of room temperature ionic liquid onto Dowex 1 × 8 resin matrix and its application toward the enhanced adsorption of chromium (VI)

International Nuclear Information System (INIS)

Kalidhasan, S.; Santhana Krishna Kumar, A.; Vidya Rajesh; Rajesh, N.

2012-01-01

Highlights: ► Ultrasound assisted impregnation of an ionic liquid in a Dowex resin matrix is studied through various physicochemical and spectroscopic techniques. ► Chromium is adsorbed with a high adsorption capacity of 230.9 mg g −1 . ► The adsorbent is regenerated using HCl–ascorbic acid mixture. ► Chromium could be effectively detoxified from an industrial effluent and the developed method was validated with the analysis of a certified reference material. - Abstract: The work discussed in this paper is based on the utilization of ultrasound in conjunction with an ionic liquid (Aliquat 336) impregnated Dowex 1 × 8 resin for the effective adsorption of chromium. Ionic liquids are known for their selectivity toward metal extraction and ultrasonic medium offers efficient energy transfer for impregnating the ionic liquid in the resin matrix. The molecular interaction between the ionic liquid impregnated resin and chromium was studied through various physicochemical and spectroscopic techniques. The influence of various analytical parameters on the adsorption of Cr(VI) such as pH, adsorbent dosage, temperature and interference of foreign ions was studied in detail. Chromium (VI) was quantitatively adsorbed in the pH range of 3.5–4, with a high adsorption capacity of 230.9 mg g −1 in conformity with the Langmuir isotherm model. The study of thermodynamic parameters showed that the adsorption process is exothermic and spontaneous. The adsorbent could be regenerated using 1 mol L −1 HCl–0.28 mol L −1 ascorbic acid mixture. Chromium could be effectively detoxified from an industrial effluent and finally the developed method was validated with the analysis of a certified reference material (BCR-715). The obtained results indicated that the ultrasonic assisted impregnation of the room temperature ionic liquid significantly enhances and improves the removal efficiency of Cr(VI).

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

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

Science.gov (United States)

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

2018-03-02

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

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

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Kent E. Wardle

2013-01-01

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

Optimization of two different dispersive liquid-liquid microextraction methods followed by gas chromatography-mass spectrometry determination for polycyclic aromatic hydrocarbons (PAHs) analysis in water.

Science.gov (United States)

Tseng, Wan-Chi; Chen, Pai-Shan; Huang, Shang-Da

2014-03-01

Novel sample preparation methods termed "up-and-down shaker-assisted dispersive liquid-liquid microextraction (UDSA-DLLME)" and "water with low concentration of surfactant in dispersed solvent-assisted emulsion dispersive liquid-liquid microextraction (WLSEME)" coupled with gas chromatography-mass spectrometry (GC-MS) have been developed for the analysis of 11 polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. For UDSA-DLLME, an up-and-down shaker-assisted emulsification was employed. Extraction was complete in 3min. Only 14 μL of 1-heptanol was required, without a dispersive solvent. Under the optimum conditions, the linear range was 0.08-100 µg L(-1), and the LODs were in the range 0.022-0.060 µg L(-1). The enrichment factors (EFs) ranged from 392 to 766. Relative recoveries were between 84% and 113% for river, lake, and field water. In WLSEME, 9 μL of 1-nonanol as extraction solvent and 240 μL of 1 mg L(-1) Triton X-100 as surfactant were mixed in a microsyringe to form a cloudy emulsified solution, which was then injected into the samples. Compared with other surfactant-assisted emulsion methods, WLSEME uses much less surfactant. The linear range was 0.08-100 µg L(-1), and the LODs were 0.022-0.13 µg L(-1). The EFs ranged from 388 to 649. The relative recoveries were 86-114% for all three water specimens. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

The ultrasound-assisted aqueous extraction of rice bran oil.

Science.gov (United States)

Khoei, Maryam; Chekin, Fereshteh

2016-03-01

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

Ionic liquid-assisted synthesis of highly dispersive bowknot-like ZnO microrods for photocatalytic applications

International Nuclear Information System (INIS)

Zhao, Shuo; Zhang, Yiwei; Zhou, Yuming; Zhang, Chao; Sheng, Xiaoli; Fang, Jiasheng; Zhang, Mingyu; Yang, Yong

2017-01-01

Highlights: • Ionic liquid was used as template for dispersive bowknot-like ZnO microrods. • The bowknot-like ZnO consists of individual microrods whose size is about 1 μm. • The formation mechanism of the ZnO materials is tentatively elucidated. • The bowknot-like ZnO exhibited the high catalytic activity in the photodegradation. • Photocatalytic activity is a result of the combination of various factors. - Abstract: Here we present a facile method for the preparation of highly dispersive ZnO materials by using ionic liquid 1-methyl-3-[3′-(trimethoxysilyl) propyl] imidazolium chloride as the template. The influence of ionic liquid concentration and calcined atmosphere on the photoactivity is studied. The samples were characterized by X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), scanning electron microscope (SEM), N_2 gas sorption and ultraviolet-visible diffuse reflectance spectroscopy. The results showed that the as-fabricated ZnO materials consisted of individual microrods with self-assembled bowknot-like architecture whose size was about 1 μm. The formation mechanism of the bowknot-like ZnO materials which is based on the self-assembly of ionic liquid is tentatively elucidated. Moreover, the ZnO-2.6N sample exhibited the higher activity for the photodegradation of MB than the photodegradation of MO and RhB. Furthermore, it was found that the ZnO materials calcined under air atmosphere showed the better photocatalytic activities than that of samples calcined under nitrogen atmosphere in the degradation of methylene blue (MB) under UV irradiation. And the special structure, surface area, adsorption capability of dye, the separation rate of photogenerated electron–hole pairs and band gap had effects on the photocatalytic activity of ZnO photocatalysts. O_2·"− was the main active species for the photocatalytic degradation of MB. It is valuable to develop this facile route preparing

Ionic liquid-assisted synthesis of highly dispersive bowknot-like ZnO microrods for photocatalytic applications

Energy Technology Data Exchange (ETDEWEB)

Zhao, Shuo [School of Chemistry and Chemical Engineering, Southeast University, Jiangsu Optoelectronic Functional Materials and Engineering Laboratory, Nanjing 211189 (China); Zhang, Yiwei, E-mail: zhangchem@seu.edu.cn [School of Chemistry and Chemical Engineering, Southeast University, Jiangsu Optoelectronic Functional Materials and Engineering Laboratory, Nanjing 211189 (China); Zhou, Yuming, E-mail: ymzhou@seu.edu.cn [School of Chemistry and Chemical Engineering, Southeast University, Jiangsu Optoelectronic Functional Materials and Engineering Laboratory, Nanjing 211189 (China); Zhang, Chao; Sheng, Xiaoli; Fang, Jiasheng; Zhang, Mingyu [School of Chemistry and Chemical Engineering, Southeast University, Jiangsu Optoelectronic Functional Materials and Engineering Laboratory, Nanjing 211189 (China); Yang, Yong [School of Chemical Engineering, Nanjing University of Science and Technology, 200 Xiao Ling Wei St, Nanjing 210094, Jiangsu (China)

2017-04-01

Highlights: • Ionic liquid was used as template for dispersive bowknot-like ZnO microrods. • The bowknot-like ZnO consists of individual microrods whose size is about 1 μm. • The formation mechanism of the ZnO materials is tentatively elucidated. • The bowknot-like ZnO exhibited the high catalytic activity in the photodegradation. • Photocatalytic activity is a result of the combination of various factors. - Abstract: Here we present a facile method for the preparation of highly dispersive ZnO materials by using ionic liquid 1-methyl-3-[3′-(trimethoxysilyl) propyl] imidazolium chloride as the template. The influence of ionic liquid concentration and calcined atmosphere on the photoactivity is studied. The samples were characterized by X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), scanning electron microscope (SEM), N{sub 2} gas sorption and ultraviolet-visible diffuse reflectance spectroscopy. The results showed that the as-fabricated ZnO materials consisted of individual microrods with self-assembled bowknot-like architecture whose size was about 1 μm. The formation mechanism of the bowknot-like ZnO materials which is based on the self-assembly of ionic liquid is tentatively elucidated. Moreover, the ZnO-2.6N sample exhibited the higher activity for the photodegradation of MB than the photodegradation of MO and RhB. Furthermore, it was found that the ZnO materials calcined under air atmosphere showed the better photocatalytic activities than that of samples calcined under nitrogen atmosphere in the degradation of methylene blue (MB) under UV irradiation. And the special structure, surface area, adsorption capability of dye, the separation rate of photogenerated electron–hole pairs and band gap had effects on the photocatalytic activity of ZnO photocatalysts. O{sub 2}·{sup −} was the main active species for the photocatalytic degradation of MB. It is valuable to develop this facile

Analysis of drugs of abuse in human plasma by dispersive liquid-liquid microextraction and high-performance liquid chromatography.

Science.gov (United States)

Fernández, P; Regenjo, M; Bermejo, A M; Fernández, A M; Lorenzo, R A; Carro, A M

2015-04-01

Opioids and cocaine are widely used at present, both for recreational purposes and as drugs of abuse. This raises the need to develop new analytical methods specifically designed for the simultaneous detection of several drugs of abuse in biological samples. In this work, dispersive liquid-liquid microextraction (DLLME) was assessed as a new sample treatment for the simultaneous extraction of morphine (MOR), 6-acetylmorphine (6AM), cocaine (COC), benzoylecgonine (BZE) and methadone (MET) from human plasma. Preliminary assays were done before developing an experimental design based on a Uniform Network Doehlert which allowed the optimum extraction conditions to be identified, namely: a volume of extractant solvent (chloroform) and dispersant solvent (acetonitrile) of 220 µl and 3.2 ml, respectively; 0.2 g of NaCl as a salting-out additive; pH 10.6 and ultrasound stirring for 3.5 min. The resulting extracts were analyzed by high-performance liquid chromatography with photodiode array detection (HPLC-PDA), using an XBridge® RP18 column (250 × 4.6 mm i.d., 5 µm particle size). Calibration graphs were linear over the concentration range 0.1-10 µg ml⁻¹, and detection limits ranged from 13.9 to 28.5 ng ml⁻¹. Precision calculated at three different concentration levels in plasma was included in the range 0.1-6.8% RSD. Recoveries of the five drugs were all higher than 84% on average. Finally the proposed method was successfully applied to 22 plasma samples from heroin, cocaine and/or methadone users, and the most frequently detected drug was benzoylecgonine, followed by methadone, cocaine and morphine. Copyright © 2014 John Wiley & Sons, Ltd.

Ultrasound assisted extraction of bioactive compounds

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Helena Drmić

2010-01-01

Full Text Available Many novel and innovative techniques are nowadays researched and explored in order to replace or improve classical, thermal processing technologies. One of newer technique is technique of minimal food processing, under what we assume ultrasound processing. Ultrasound technology can be very useful for minimal food processing because transmission of acoustic energy through product is fast and complete, which allows reduction in total processing time, and therefore lower energy consumption. Industrial processing is growing more and more waste products, and in desire of preservation of global recourses and energy efficiency, several ways of active compounds extraction techniques are now explored. The goal is to implement novel extraction techniques in food and pharmaceutical industry as well in medicine. Ultrasound assisted extraction of bioactive compounds offers increase in yield, and reduction or total avoiding of solvent usage. Increase in temperature of treatment is controlled and restricted, thereby preserving extracted bioactive compounds. In this paper, several methods of ultrasound assisted extraction of bioactive compounds from plant materials are shown. Ultrasound can improve classic mechanisms of extraction, and thereby offer novel possibilities of commercial extraction of desired compounds. Application of sonochemistry (ultrasound chemistry is providing better yield in desired compounds and reduction in treatment time.

Extraction of acetanilides in rice using ionic liquid-based matrix solid phase dispersion-solvent flotation.

Science.gov (United States)

Zhang, Liyuan; Wang, Changyuan; Li, Zuotong; Zhao, Changjiang; Zhang, Hanqi; Zhang, Dongjie

2018-04-15

Ionic liquid-based matrix solid phase dispersion-solvent flotation coupled with high performance liquid chromatography was developed for the determination of the acetanilide herbicides, including metazachlor, propanil, alachlor, propisochlor, pretilachlor, and butachlor in rice samples. Some experimental parameters, including the type of dispersant, the mass ratio of dispersant to sample, pH of sample solution, the type of extraction solvent, the type of ionic liquid, flotation time, and flow rate of N 2 were optimized. The average recoveries of the acetanilide herbicides at spiked concentrations of 50, 125, and 250 µg/kg ranged from 89.4% to 108.7%, and relative standard deviations were equal to or lower than 7.1%, the limits of quantification were in the range of 38.0 to 84.7 µg/kg. Copyright © 2017 Elsevier Ltd. All rights reserved.

Derivation of nonlinear wave equations for ultrasound beam in nonuniform bubbly liquids

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Kanagawa, Tetsuya; Yano, Takeru; Kawahara, Junya; Kobayashi, Kazumichi; Watanabe, Masao; Fujikawa, Shigeo

2012-09-01

Weakly nonlinear propagation of diffracted ultrasound beams in a nonuniform bubbly liquid is theoretically studied based on the method of multiple scales with the set of scaling relations of some physical parameters. It is assumed that the spatial distribution of the number density of bubbles in an initial state at rest is a slowly varying function of space coordinates and the amplitude of its variation is small compared with a mean number density. As a result, a Khokhlov-Zabolotskaya-Kuznetsov (KZK) equation with dispersion and nonuniform effects for a low frequency case and a nonlinear Schrödinger (NLS) equation with dissipation, diffraction, and nonuniform effects for a high frequency case, are derived from the basic equations of bubbly flows.

Ionic liquid-assisted synthesis of highly dispersive bowknot-like ZnO microrods for photocatalytic applications

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Zhao, Shuo; Zhang, Yiwei; Zhou, Yuming; Zhang, Chao; Sheng, Xiaoli; Fang, Jiasheng; Zhang, Mingyu; Yang, Yong

2017-04-01

Here we present a facile method for the preparation of highly dispersive ZnO materials by using ionic liquid 1-methyl-3-[3‧-(trimethoxysilyl) propyl] imidazolium chloride as the template. The influence of ionic liquid concentration and calcined atmosphere on the photoactivity is studied. The samples were characterized by X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), scanning electron microscope (SEM), N2 gas sorption and ultraviolet-visible diffuse reflectance spectroscopy. The results showed that the as-fabricated ZnO materials consisted of individual microrods with self-assembled bowknot-like architecture whose size was about 1 μm. The formation mechanism of the bowknot-like ZnO materials which is based on the self-assembly of ionic liquid is tentatively elucidated. Moreover, the ZnO-2.6N sample exhibited the higher activity for the photodegradation of MB than the photodegradation of MO and RhB. Furthermore, it was found that the ZnO materials calcined under air atmosphere showed the better photocatalytic activities than that of samples calcined under nitrogen atmosphere in the degradation of methylene blue (MB) under UV irradiation. And the special structure, surface area, adsorption capability of dye, the separation rate of photogenerated electron-hole pairs and band gap had effects on the photocatalytic activity of ZnO photocatalysts. O2rad - was the main active species for the photocatalytic degradation of MB. It is valuable to develop this facile route preparing the highly dispersive bowknot-like ZnO materials and the ZnO materials can be beneficial for environmental protection.

Ultrasound-Assisted Hot Air Drying of Foods

Science.gov (United States)

Mulet, Antonio; Cárcel, Juan Andrés; García-Pérez, José Vicente; Riera, Enrique

This chapter deals with the application of power ultrasound, also named high-intensity ultrasound, in the hot air drying of foods. The aim of ultrasound-assisted drying is to overcome some of the limitations of traditional convective drying systems, especially by increasing drying rate without reducing quality attributes. The effects of ultrasound on drying rate are responsible for some of the phenomena produced in the internal and/or external resistance to mass transfer.

Fabrication of γ-MPS-Modified HNT-PMMA Nanocomposites by Ultrasound-Assisted Miniemulsion Polymerization

Science.gov (United States)

Buruga, Kezia; Kalathi, Jagannathan T.

2018-04-01

Halloysite nanotubes (HNTs) were modified with γ-methacryloxypropyltrimethoxysilane (γ-MPS) to improve their interaction with the polymer, and the modified HNTs (MHNTs) were subsequently used for the synthesis of MHNT-polymethylmethacrylate (PMMA) nanocomposites by miniemulsion polymerization assisted by ultrasound. Reduced agglomeration of HNTs due to modification with γ-MPS was evident from scanning electron microscopy analysis. Modification of HNTs and exfoliation of MHNTs in the polymer nanocomposite were confirmed by the presence of their respective characteristic peaks in Fourier-transform infrared spectra and x-ray diffraction patterns. Transmission electron microscopic analysis showed that the surface of the MHNTs differed significantly from that of unmodified HNTs. MHNT-PMMA nanocomposite exhibited significantly higher glass-transition temperature (T g) compared with neat PMMA or unmodified HNT-PMMA nanocomposite. Hence, such modification of HNTs along with miniemulsion polymerization assisted by ultrasound is a promising approach to achieve better dispersion of HNTs in the polymer and to obtain nanocomposites with enhanced properties.

Extraction of substances assisted by ultrasound (UAE)

International Nuclear Information System (INIS)

Azuola, Rocio; Vargas, Pedro

2007-01-01

Different compounds present in vegetables with functional or technological properties, have gained great importance in food, pharmaceutical and cosmetic markets. Efficient methods, economical and environment friendly are sought for the extraction of these substances. A literature review has been performanced of recent publications on different extraction methods and their comparison to the ultrasound assisted extraction (UAE) to assess their effectiveness and industrial viability. The ultrasound assisted extraction (UAE) has been found to be more efficient than traditional mining methods, and cheaper and easier than non-traditional extraction methods such as microwave-assisted extraction, so it checks its industrial viability. (author) [es

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

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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.

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

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

2016-01-29

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

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

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

2015-01-01

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

Dual-plane ultrasound flow measurements in liquid metals

International Nuclear Information System (INIS)

Büttner, Lars; Nauber, Richard; Burger, Markus; Czarske, Jürgen; Räbiger, Dirk; Franke, Sven; Eckert, Sven

2013-01-01

An ultrasound measurement system for dual-plane, two-component flow velocity measurements especially in opaque liquids is presented. Present-day techniques for measuring local flow structures in opaque liquids disclose considerable drawbacks concerning line-wise measurement of single ultrasound probes. For studying time-varying flow patterns, conventional ultrasound techniques are either limited by time-consuming mechanical traversing or by the sequential operation of single probes. The measurement system presented within this paper employs four transducer arrays with a total of 100 single elements which allows for flow mapping without mechanical traversing. A high frame rate of several 10 Hz has been achieved due to an efficient parallelization scheme using time-division multiplexing realized by a microcontroller-based electronic switching matrix. The functionality and capability of the measurement system are demonstrated on a liquid metal flow at room temperature inside a cube driven by a rotating magnetic field (RMF). For the first time, the primary and the secondary flow have been studied in detail and simultaneously using a configuration with two crossed measurement planes. The experimental data confirm predictions made by numeric simulation. After a sudden switching on of the RMF, inertial oscillations of the secondary flow were observed by means of a time-resolved measurement with a frame rate of 3.4 Hz. The experiments demonstrate that the presented measurement system is able to investigate complex and transient flow structures in opaque liquids. Due to its ability to study the temporal evolution of local flow structures, the measurement system could provide considerable progress for fluid dynamics research, in particular for applications in the food industry or liquid metal technologies. (paper)

Dual-plane ultrasound flow measurements in liquid metals

Science.gov (United States)

Büttner, Lars; Nauber, Richard; Burger, Markus; Räbiger, Dirk; Franke, Sven; Eckert, Sven; Czarske, Jürgen

2013-05-01

An ultrasound measurement system for dual-plane, two-component flow velocity measurements especially in opaque liquids is presented. Present-day techniques for measuring local flow structures in opaque liquids disclose considerable drawbacks concerning line-wise measurement of single ultrasound probes. For studying time-varying flow patterns, conventional ultrasound techniques are either limited by time-consuming mechanical traversing or by the sequential operation of single probes. The measurement system presented within this paper employs four transducer arrays with a total of 100 single elements which allows for flow mapping without mechanical traversing. A high frame rate of several 10 Hz has been achieved due to an efficient parallelization scheme using time-division multiplexing realized by a microcontroller-based electronic switching matrix. The functionality and capability of the measurement system are demonstrated on a liquid metal flow at room temperature inside a cube driven by a rotating magnetic field (RMF). For the first time, the primary and the secondary flow have been studied in detail and simultaneously using a configuration with two crossed measurement planes. The experimental data confirm predictions made by numeric simulation. After a sudden switching on of the RMF, inertial oscillations of the secondary flow were observed by means of a time-resolved measurement with a frame rate of 3.4 Hz. The experiments demonstrate that the presented measurement system is able to investigate complex and transient flow structures in opaque liquids. Due to its ability to study the temporal evolution of local flow structures, the measurement system could provide considerable progress for fluid dynamics research, in particular for applications in the food industry or liquid metal technologies.

Green ultrasound-assisted extraction of carotenoids based on the bio-refinery concept using sunflower oil as an alternative solvent.

Science.gov (United States)

Li, Ying; Fabiano-Tixier, Anne Sylvie; Tomao, Valérie; Cravotto, Giancarlo; Chemat, Farid

2013-01-01

A green, inexpensive and easy-to-use method for carotenoids extraction from fresh carrots assisted by ultrasound was designed in this work. Sunflower oil was applied as a substitute to organic solvents in this green ultrasound-assisted extraction (UAE): a process which is in line with green extraction and bio-refinery concepts. The processing procedure of this original UAE was first compared with conventional solvent extraction (CSE) using hexane as solvent. Moreover, the UAE optimal conditions for the subsequent comparison were optimized using response surface methodology (RSM) and ultra performance liquid chromatography--diode array detector--mass spectroscopy (UPLC-DAD-MS). The results showed that the UAE using sunflower as solvent has obtained its highest β-carotene yield (334.75 mg/l) in 20 min only, while CSE using hexane as solvent obtained a similar yield (321.35 mg/l) in 60 min. The green UAE performed under optimal extraction conditions (carrot to oil ratio of 2:10, ultrasonic intensity of 22.5 W cm(-2), temperature of 40 °C and sonication time of 20 min) gave the best yield of β-carotene. Copyright © 2012 Elsevier B.V. All rights reserved.

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.

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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. Copyright © 2015 Elsevier Inc. All rights reserved.

Derivation of simplified basic equations of gas-liquid two-phase dispersed flow based on two-fluid model

International Nuclear Information System (INIS)

Kataoka, Isao; Tomiyama, Akio

2004-01-01

The simplified and physically reasonable basic equations for the gas-liquid dispersed flow were developed based on some appropriate assumptions and the treatment of dispersed phase as isothermal rigid particles. Based on the local instant formulation of mass, momentum and energy conservation of the dispersed flow, time-averaged equations were obtained assuming that physical quantities in the dispersed phase are uniform. These assumptions are approximately valid when phase change rate and/or chemical reaction rate are not so large at gas-liquid interface and there is no heat generation in within the dispersed phase. Detailed discussions were made on the characteristics of obtained basic equations and physical meanings of terms consisting the basic equations. It is shown that, in the derived averaged momentum equation, the terms of pressure gradient and viscous momentum diffusion do not appear and, in the energy equation, the term of molecular thermal diffusion heat flux does not appear. These characteristics of the derived equations were shown to be very consistent concerning the physical interpretation of the gas-liquid dispersed flow. Furthermore, the obtained basic equations are consistent with experiments for the dispersed flow where most of averaged physical quantities are obtained assuming that the distributions of those are uniform within the dispersed phase. Investigation was made on the problem whether the obtained basic equations are well-posed or ill-posed for the initial value problem. The eigenvalues of the simplified mass and momentum equations are calculated for basic equations obtained here and previous two-fluid basic equations with one pressure model. Well-posedness and ill-posedness are judged whether the eigenvalues are real or imaginary. The result indicated the newly developed basic equations always constitute the well-posed initial value problem while the previous two-fluid basic equations based on one pressure model constitutes ill

Comparison of green sample preparation techniques in the analysis of pyrethrins and pyrethroids in baby food by liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Petrarca, Mateus Henrique; Ccanccapa-Cartagena, Alexander; Masiá, Ana; Godoy, Helena Teixeira; Picó, Yolanda

2017-05-12

A new selective and sensitive liquid chromatography triple quadrupole mass spectrometry method was developed for simultaneous analysis of natural pyrethrins and synthetic pyrethroids residues in baby food. In this study, two sample preparation methods based on ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and salting-out assisted liquid-liquid extraction (SALLE) were optimized, and then, compared regarding the performance criteria. Appropriate linearity in solvent and matrix-based calibrations, and suitable recoveries (75-120%) and precision (RSD values≤16%) were achieved for selected analytes by any of the sample preparation procedures. Both methods provided the analytical selectivity required for the monitoring of the insecticides in fruit-, cereal- and milk-based baby foods. SALLE, recognized by cost-effectiveness, and simple and fast execution, provided a lower enrichment factor, consequently, higher limits of quantification (LOQs) were obtained. Some of them too high to meet the strict legislation regarding baby food. Nonetheless, the combination of ultrasound and DLLME also resulted in a high sample throughput and environmental-friendly method, whose LOQs were lower than the default maximum residue limit (MRL) of 10μgkg -1 set by European Community for baby foods. In the commercial baby foods analyzed, cyhalothrin and etofenprox were detected in different samples, demonstrating the suitability of proposed method for baby food control. Copyright © 2017 Elsevier B.V. All rights reserved.

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

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

2016-01-01

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

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

Science.gov (United States)

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

2017-10-06

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

An evaporation-assisted dispersive liquid-liquid microextraction technique as a simple tool for high performance liquid chromatography tandem-mass spectrometry determination of insecticides in wine.

Science.gov (United States)

Timofeeva, Irina; Kanashina, Daria; Moskvin, Leonid; Bulatov, Andrey

2017-08-25

A sample pre-treatment technique based on evaporation-assisted dispersive liquid-liquid microextraction (EVA-DLLME), followed by HPLC-MS/MS has been developed for the determination of organophosphate insecticides (malathion, diazinon, phosalone) in wine samples. The procedure includes the addition of mixture of organic solvents (with density higher than water), consisting of the extraction (low density) and volatile (high density) solvents, to aqueous sample followed by heating of the mixture obtained, what promotes the volatile solvent evaporation and moving extraction solvent droplets from down to top of the aqueous sample and, as a consequence, microextraction of target analytes. To initiate the evaporation process an initiator is required. It was established that hexanol (extraction solvent) and dichloromethane (volatile solvent) mixture (1:1, v/v) provides effective microextraction of the insecticides from wine samples with recovery from 92 to 103%. The conditions of insecticides' microextraction such as selection of extraction solvent, ratio of hexanol/dichloromethane and hexanol/sample, type and concentration of initiator, and effect of ethanol as one of the main components of wine have been studied. Under optimal experimental conditions the linear detection ranges were found to be 10 -7 -10 -3 gL -1 for malathion, 10 -9 -10 -4 gL -1 for diazinon, and 10 -6 -10 -2 gL -1 for phosalone. The LODs, calculated from a blank test, based on 3σ, found to be 3×10 -8 gL -1 for malathion, 3×10 -10 gL -1 for diazinon and 3×10 -7 gL -1 for phosalone. The advantages of EVA-DLLME are the rapidity, simplicity, high sample throughput and low cost. As an outcome, the analytical results agreed fairly well with the results obtained by a reference GC-MS method. Copyright © 2017 Elsevier B.V. All rights reserved.

Membrane assisted liquid-liquid extraction of cerium

International Nuclear Information System (INIS)

Soldenhoff, K.M.

2000-02-01

Membrane assisted liquid-liquid extraction of cerium was investigated, with emphasis placed on the study of the reaction chemistry and the kinetics of non-dispersive solvent extraction and stripping with microporous membranes. A bulk liquid membrane process was developed for the purification of cerium(IV) from sulfate solutions containing other rare earth elements. The cerium process was studied in both a flat sheet contained liquid membrane configuration and with hollow fibre contactors. Di-2-ethylhexyl phosphoric acid (DEHPA) was identified as a suitable extractant for cerium(IV) from sulfuric acid solution, with due consideration of factors such as extraction ability, resistance to degradation, solvent selectivity and potential for sulfate transfer into a strip solution. A detailed study of the extraction of cerium(IV) with DEHPA defined the extraction reaction chemistry. The Ce/DEHPA/sulfate system was also investigated with a flat sheet bulk liquid membrane configuration, using both sulfuric and hydrochloric acid as receiver solutions. These tests identified that hydrophobic membranes provide better mass transfer for extraction and hydrophilic membranes are better for stripping. The presence of an impurity, mono 2-ethylhexyl phosphoric acid (MEHPA), was found to have a dramatic accelerating effect on the rate of the chemical extraction reaction. This was attributed to its higher interfacial activity and population compared to DEHPA, and the fact that MEHPA was also found to be an active carrier for cerium(IV). The mass transfer rate of membrane assisted extraction and stripping of cerium, using hydrophobic and hydrophilic microporous membranes, respectively, was investigated using a modified Lewis-type cell. It was quantitatively demonstrated that the extraction process was mainly controlled by membrane diffusion and the stripping process was controlled by the chemical reaction rate, with membrane diffusion becoming important at low distribution coefficients

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

Directory of Open Access Journals (Sweden)

Jianfeng Yu

2017-12-01

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

Dispersions of silica nanoparticles in ionic liquids investigated with advanced rheology

International Nuclear Information System (INIS)

Wittmar, Alexandra; Ruiz-Abad, David; Ulbricht, Mathias

2012-01-01

The colloidal stabilities of dispersions of unmodified and surface-functionalized SiO 2 nanoparticles in hydrophobic and hydrophilic imidazolium-based ionic liquids were studied with advanced rheology at three temperatures (25, 100, and 200 °C). The rheological behavior of the dispersions was strongly affected by the ionic liquids hydrophilicity, by the nanoparticles surface, by the concentration of the nanoparticles in the dispersion as well as by the temperature. The unmodified hydrophilic nanoparticles showed a better compatibility with the hydrophilic ionic liquid. The SiO 2 surface functionalization with hydrophobic groups clearly improved the colloidal stability of the dispersions in the hydrophobic ionic liquid. The temperature increase was found to lead to a destabilization in all studied systems, especially at higher concentrations. The results of this study imply that ionic liquids with tailored properties could be used in absorbers directly after reactors for gas-phase synthesis of nanoparticles or/and as solvents for their further surface functionalization without agglomeration or aggregation.

Extraction of Dihydroquercetin from Larix gmelinii with Ultrasound-Assisted and Microwave-Assisted Alternant Digestion

Directory of Open Access Journals (Sweden)

Yuangang Zu

2012-07-01

Full Text Available An ultrasound and microwave assisted alternant extraction method (UMAE was applied for extracting dihydroquercetin (DHQ from Larix gmelinii wood. This investigation was conducted using 60% ethanol as solvent, 1:12 solid to liquid ratio, and 3 h soaking time. The optimum treatment time was ultrasound 40 min, microwave 20 min, respectively, and the extraction was performed once. Under the optimized conditions, satisfactory extraction yield of the target analyte was obtained. Relative to ultrasound-assisted or microwave-assisted method, the proposed approach provides higher extraction yield. The effect of DHQ of different concentrations and synthetic antioxidants on oxidative stability in soy bean oil stored for 20 days at different temperatures (25 °C and 60 °C was compared. DHQ was more effective in restraining soy bean oil oxidation, and a dose-response relationship was observed. The antioxidant activity of DHQ was a little stronger than that of BHA and BHT. Soy bean oil supplemented with 0.08 mg/g DHQ exhibited favorable antioxidant effects and is preferable for effectively avoiding oxidation. The L. gmelinii wood samples before and after extraction were characterized by scanning electron microscopy. The results showed that the UMAE method is a simple and efficient technique for sample preparation.

The ultrasound-assisted sugar extraction from sugar beet cossettes

International Nuclear Information System (INIS)

Stasiak, D.M.

2005-01-01

The aim of this work was to study the ultrasound-assisted water extraction of sugar from sugar beet cossettes. The ultrasound bath device (25 kHz, 200 W) was used. The sonication accelerated sugar diffusion at both temperatures 18 deg C and 77.6 deg C and gave the higher level of dry matter content SS (4-6 percent) and sugar content CK (7-22 percent) in juice. The SS and CK depended on time of exposition, time and temperature of extraction. In particular, the effects of 5 min ultrasound-assisted extraction were equal to 20 min extraction in traditional conditions. The shorter time, lower temperature, higher efficiency and purity of juice could be the effects of sugar extraction with ultrasound. The change of thickness of diffusion membrane, microflows in tissue as well as it's environment caused by ultrasound was the reason of acceleration of sugar extraction

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.

Classification and management of gynecomastia: defining the role of ultrasound-assisted liposuction.

Science.gov (United States)

Rohrich, Rod J; Ha, Richard Y; Kenkel, Jeffrey M; Adams, William P

2003-02-01

Gynecomastia, or excessive male breast development, has an incidence of 32 to 65 percent in the male population. This condition has important physical and psychological impacts. Advances in elucidating the pathophysiology of gynecomastia have been made, though understanding remains limited. Recommendations for evaluation and workup have varied and are often arbitrary. A diagnostic algorithm is suggested, with emphasis on a comprehensive history, physical examination, and minimizing unnecessary diagnostic testing. Medical management has had limited success; surgical therapy, primarily through excisional techniques, has been the accepted standard. Although effective, excisional techniques subject patients to large, visible scars. Ultrasound-assisted liposuction has recently emerged as a safe and effective method for the treatment of gynecomastia. It is particularly efficient in the removal of the dense, fibrous male breast tissue while offering advantages in minimal external scarring. A new system of classification and graduated treatment is proposed, based on glandular versus fibrous hypertrophy and degree of breast ptosis (skin excess). The authors' series of 61 patients with gynecomastia from 1987 to 2000 at the University of Texas Southwestern Department of Plastic Surgery demonstrated an overall success rate of 86.9 percent using suction-assisted lipectomy (1987 to 1997) and ultrasound-assisted liposuction (1997 to 2000). The authors have found ultrasound-assisted liposuction to be effective in treating most grades of gynecomastia. Excisional techniques are reserved for severe gynecomastia with significant skin excess after attempted ultrasound-assisted liposuction.

Glucose obtained from rice bran by ultrasound-assisted enzymatic hydrolysis

Directory of Open Access Journals (Sweden)

Raquel Cristine Kuhn

2015-05-01

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

Investigation of Factors Influencing Dispersion of Liquid Hydrocarbons in Porous Media

Directory of Open Access Journals (Sweden)

Hussain Ali Baker

2016-08-01

Full Text Available An experimental work has been done to study the major factors that affect the axial dispersion of some hydrocarbons during liquid-liquid miscible displacement. Kerosene and gas oil are used as displacing phase while seven liquid hydrocarbons of high purity represent the displaced phase, three of the liquids are aromatics and the rest are of paraffinic base. In conducting the experiments, two packed beds of different porosity and permeability are used as porous media. The results showed that the displacement process is not a piston flow, breakthrough of displacing fluids are shown before one pore volume has been injected. The processes are stable with no evidence of viscous fingering. Dispersion model as adapted by Brigham et.al (1961 is used to determine the axial dispersion coefficient of displacing fluid. The results show an increasing in dispersion coefficient as the interstitial velocity and viscosity ratio increases.

An ultrasound-based liquid pressure measurement method in small diameter pipelines considering the installation and temperature.

Science.gov (United States)

Li, Xue; Song, Zhengxiang

2015-04-09

Liquid pressure is a key parameter for detecting and judging faults in hydraulic mechanisms, but traditional measurement methods have many deficiencies. An effective non-intrusive method using an ultrasound-based technique to measure liquid pressure in small diameter (less than 15 mm) pipelines is presented in this paper. The proposed method is based on the principle that the transmission speed of an ultrasonic wave in a Kneser liquid correlates with liquid pressure. Liquid pressure was calculated using the variation of ultrasonic propagation time in a liquid under different pressures: 0 Pa and X Pa. In this research the time difference was obtained by an electrical processing approach and was accurately measured to the nanosecond level through a high-resolution time measurement module. Because installation differences and liquid temperatures could influence the measurement accuracy, a special type of circuit called automatic gain control (AGC) circuit and a new back propagation network (BPN) model accounting for liquid temperature were employed to improve the measurement results. The corresponding pressure values were finally obtained by utilizing the relationship between time difference, transient temperature and liquid pressure. An experimental pressure measurement platform was built and the experimental results confirm that the proposed method has good measurement accuracy.

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

Science.gov (United States)

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

2018-01-01

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

Determination of ibuprofen enantiomers in breast milk using vortex-assisted matrix solid-phase dispersion and direct chiral liquid chromatography.

Science.gov (United States)

León-González, M E; Rosales-Conrado, N

2017-09-08

A mixture of β-cyclodextrin (β-CD) and primary and secondary amine (PSA) sorbents was employed for the extraction and quantification of ibuprofen enantiomers from human breast milk, combining a vortex-assisted matrix solid-phase dispersion method (MSPD) and direct chiral liquid chromatography (CLC) with ultraviolet detection (UV). The MSPD sample preparation procedure was optimized focusing on both the type and amount of dispersion/sorption sorbents and the nature of the elution solvent, in order to obtain acceptable recoveries and avoiding enantiomer conversion. These MSPD parameters were optimized with the aid of an experimental design approach. Hence, a factorial design was used for identification of the main variables affecting the extraction process of ibuprofen enantiomers. Under optimum selected conditions, MSPD combined with direct CLC-UV was successfully applied for ibuprofen enantiomeric determination in breast milk at enantiomer levels between 0.15 and 6.0μgg -1 . The proposed analytical method also provided good repeatability, with relative standard deviations of 6.4% and 8.3% for the intra-day and inter-day precision, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

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 CO 2 emissions. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

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

International Nuclear Information System (INIS)

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

2016-01-01

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.

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

International Nuclear Information System (INIS)

YangDai, Tianyi; Zhang, Li

2016-01-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

Energy Technology Data Exchange (ETDEWEB)

YangDai, Tianyi [Department of Engineering Physics, Tsinghua University, Beijing 100084 (China); Key Laboratory of Particle & Radiation Imaging (Tsinghua University), Ministry of Education (China); Zhang, Li, E-mail: zhangli@nuctech.com [Department of Engineering Physics, Tsinghua University, Beijing 100084 (China); Key Laboratory of Particle & Radiation Imaging (Tsinghua University), Ministry of Education (China)

2016-02-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

Science.gov (United States)

YangDai, Tianyi; Zhang, Li

2016-02-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

Ultrasound-assisted extraction of Mangiferin from Mango (Mangifera indica L.) leaves using response surface methodology.

Science.gov (United States)

Zou, Tang-Bin; Xia, En-Qin; He, Tai-Ping; Huang, Ming-Yuan; Jia, Qing; Li, Hua-Wen

2014-01-27

Mangiferin is a xanthone widely distributed in higher plants showing antioxidative, antiviral, anticancer, antidiabetic, immunomodulatory, hepatoprotective and analgesic effects. In the present study, an ultrasonic-assisted extraction method was developed for the effective extraction of mangiferin from mango leaves. Some parameters such as ethanol concentration, liquid-to-solid ratio, extraction temperature, and extraction time were optimized by single-factor experiment and response surface methodology. The optimal extraction conditions were 44% ethanol, the liquid-to-solid ratio was 38:1, and extraction for 19.2 min at 60 °C under ultrasound irradiation of 200 W. Under optimal conditions, the yield of mangiferin was 58.46 ± 1.27 mg/g. The results obtained are helpful for the full utilization of mango leaves, and also indicated that ultrasonic-assisted extraction is a very useful method for the extraction of mangiferin from plant materials.

Microalgae as feedstock for biodiesel production under ultrasound treatment - A review.

Science.gov (United States)

Sivaramakrishnan, Ramachandran; Incharoensakdi, Aran

2018-02-01

The application of ultrasound in biodiesel production has recently emerged as a novel technology. Ultrasound treatment enhances the mass transfer characteristics leading to the increased reaction rate with short reaction time and potentially reduces the production cost. In this review, application of ultrasound-assisted biodiesel production using acid, base and enzyme catalysts is presented. A critical assessment of the current status of ultrasound in biodiesel production was discussed with the emphasis on using ultrasound for efficient microalgae biodiesel production. The ultrasound in the biodiesel production enhances the emulsification of immiscible liquid reactant by microturbulence generated by cavitation bubbles. The major benefit of the ultrasound-assisted biodiesel production is a reduction in reaction time. Several different methods have been discussed to improve the biodiesel production. Overall, this review focuses on the current understanding of the application of ultrasound in biodiesel production from microalgae and to provide insights into future developments. Copyright © 2017 Elsevier Ltd. All rights reserved.

Solubilization of bovine gelatin using power ultrasound: gelation without heating.

Science.gov (United States)

Farahnaky, Asgar; Zendeboodi, Fatemeh; Azizi, Rezvan; Mesbahi, Gholamreza; Majzoobi, Mahsa

2017-04-01

The aim of this study was to investigate the efficacy of power ultrasound without using any heating stage in solubilizeing gelatin dispersions, and to characterize the mechanical and microstructural properties of the resulting gels using texture analysis and scanning electron microscopy, respectively. Usually to prepare a gel from gelatin, a primary heating stage of at about 40C or above is required to solubilize gelatin macromolecules. In this study solubilizing gelatin dispersions using power ultrasound without any heating was successfully performed. For solubilising gelatin, an ultrasound equipment with a frequency of 20 kHz, amplitude of 100% and power range of 50-150 W was used. Aqueous gelatin dispersions (4% w/v) were subjected to ultrasound for different times (40-240 s) at a constant temperature of 13C. Applying ultrasound to gelatin dispersions caused increases in water absorption and water solubility of the hydrocolloid. The textural parameters of the resulting gelatin gels, increased with increasing time and power of ultrasound. Moreover, a generalized Maxwell model with three elements was used for calculating relaxation times of the gels. The microstructural observations by SEM showed that the structural cohesiveness of the gels increased by increasing ultrasonication time. Ultrasound-assisted solubilization of gelatin can have emerging implications for industrial uses in pharmaceuticals, food and non-food systems. Usually to prepare a gel from gelatin, a primary heating stage of at about 40C or above is required to solubilize gelatin macromolecules. Therefore, the use of gelatin as a hydrocolloid in food processings or pharmaceutical formulations which lack a heating step has been a technological and practical challenge. In this study solubilizing gelatin dispersions using power ultrasound without any heating was successfully performed. Ultrasound-assisted solubilisation of gelatin can have emerging implications for industrial uses in pharmaceuticals

Ionic-liquid-based dispersive liquid-liquid microextraction combined with magnetic solid-phase extraction for the determination of aflatoxins B1 , B2 , G1 , and G2 in animal feeds by high-performance liquid chromatography with fluorescence detection.

Science.gov (United States)

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

2016-10-01

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

Glyoxal and methylglyoxal as urinary markers of diabetes. Determination using a dispersive liquid-liquid microextraction procedure combined with gas chromatography-mass spectrometry.

Science.gov (United States)

Pastor-Belda, M; Fernández-García, A J; Campillo, N; Pérez-Cárceles, M D; Motas, M; Hernández-Córdoba, M; Viñas, P

2017-08-04

Glyoxal (GO) and methylglyoxal (MGO) are α-oxoaldehydes that can be used as urinary diabetes markers. In this study, their levels were measured using a sample preparation procedure based on salting-out assisted liquid-liquid extraction (SALLE) and dispersive liquid-liquid microextraction (DLLME) combined with gas chromatography-mass spectrometry (GC-MS). The effect of the derivatization reaction with 2,3-diaminonaphthalene, the addition of acetonitrile and sodium chloride to urine, and the DLLME step using the acetonitrile extract as dispersant solvent and carbon tetrachloride as extractant solvent were carefully optimized. Quantification was performed by the internal standard method, using 5-bromo-2-chloroanisole. The intraday and interday precisions were lower than 6%. Limits of detection were 0.12 and 0.06ngmL -1 , and enrichment factors 140 and 130 for GO and MGO, respectively. The concentrations of these α-oxoaldehydes in urine were between 0.9 and 35.8ngg -1 levels (creatinine adjusted). A statistical comparison of the analyte contents of urine samples from non-diabetic and diabetic patients pointed to significant differences (P=0.046, 24 subjects investigated), particularly regarding MGO, which was higher in diabetic patients. The novelty of this study compared with previous procedures lies in the treatment of the urine sample by SALLE based on the addition of acetonitrile and sodium chloride to the urine. The DLLME procedure is performed with a sedimented drop of the extractant solvent, without a surfactant reagent, and using acetonitrile as dispersant solvent. Separation of the analytes was performed using GC-MS detection, being the analytes unequivocal identified. The proposed procedure is the first microextraction method applied to the analysis of urine samples from diabetic and non-diabetic patients that allows a clear differentiation between both groups using a simple analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Multiclass method for the determination of pharmaceuticals and personal care products in compost from sewage sludge using ultrasound and salt-assisted liquid-liquid extraction followed by ultrahigh performance liquid chromatography-tandem mass spectrometry analysis.

Science.gov (United States)

Luque-Muñoz, A; Vílchez, J L; Zafra-Gómez, A

2017-07-21

An analytical method for the analysis of 16 pharmaceuticals and personal care products in compost from sewage sludge is successfully validated. Ultrasound assisted extraction with a mixture of acetonitrile:ethyl acetate (1:1, v/v) containing 10% (v/v) of acetic acid was carried out. Two cycles of extraction of 10min were applied. A clean-up of the extracts using salt-assisted liquid-liquid extraction (SALLE) was also included. Experimental design was used for the optimization of the main parameters involved in the extraction and cleaned-up steps. The chromatographic separation was carried out by ultrahigh performance liquid chromatography using a mobile phase gradient mixture of a 13mM buffer ammonium formate solution (pH 9.25) (solvent A) and methanol (solvent B). An ACQUITY UPLC ® BEH C18 column (1.7μm; 2.1×50mm) column was used. Analytes were separated in less than 11min. The compounds were detected and quantified using single reaction monitoring electrospray tandem mass spectrometry. The limits of detection calculated ranged from 0.5 to 4ngg -1 d.w., and the limits of quantification from 2 to 13ngg -1 d.w. Recoveries from 93% to 111%, with relative standar deviations lower than 11% in all cases, were obtained. The method was applied to natural compost samples. High concentrations of some analytes were found. Ketoprofen (510ngg -1 d.w.), methylparaben (240ngg -1 d.w.), diclofenac (175ngg -1 d.w.) and flufenamic acid (128ngg -1 d.w.) were the most abundant. Copyright © 2017 Elsevier B.V. All rights reserved.

Solar assisted liquid desiccant cooling using clay based membranes

Directory of Open Access Journals (Sweden)

Priya S. Shanmuga

2018-01-01

Full Text Available The environmental concerns have led to the urge of the usage of non-conventional energy resources like solar, wind, thermal, geothermal etc. which provide enormous source of energy without causing any further diminution of the environment. Instead of the conventional HVAC systems that cause colossal environmental perils, usage of liquid desiccants in coming in vogue whereby reducing ecological threats. Moreover, solar assisted systems provide further impulse to such systems. This paper discusses about the various comparisons between liquid desiccants: Lithium chloride, Potassium formate and Calcium chloride and concludes that potassium formate is the best desiccant to be used among the three. Potassium formate (HCOOK is used which is cheaper and less corrosive as compared to the other aqueous salts, and has a negative crystallization temperature. Potassium formate is a new liquid desiccant and thus, not much research is available currently. The weather conditions of Manipal provide an appropriate condition for the experimentations of solar aided liquid desiccant evaporative cooling systems due to its humid climate and intense solar radiation obtained. The small scale experimentation also encounters the problem of liquid desiccant carryover by the air flow, with the help of clay based membranes which are again cheap, environmentally benign and obtained in a facile way. The projected system takes complete advantage of pure solar energy aimed at the regeneration of liquid desiccant.

Ultrasound-assisted dispersive solid phase extraction of cadmium(II) and lead(II) using a hybrid nanoadsorbent composed of graphene and the zeolite clinoptilolite

International Nuclear Information System (INIS)

Ghazaghi, Mehri; Mousavi, Hassan Zavvar; Shirkhanloo, Hamid; Rashidi, Ali Morad

2015-01-01

We describe a hybrid nanoadsorbent prepared by depositing graphene on the zeolite clinoptilolite by chemical vapor deposition. The resulting sorbent is well suited for the preconcentration of lead(II) and cadmium(II) by ultrasound-assisted dispersive micro solid–phase extraction. An extraction unit has been designed and manufactured that facilitates handling of small sample volumes. The effects of sample pH, amount of sorbent, concentration and volume of elution and time of ultrasonic bath were investigated. The nanoadsorbent was characterized by scanning electron microscopy, X-ray diffraction and energy dispersive X-ray microanalysis, all of which revealed the high surface area of the graphene sheets on the clinoptilolite. The extraction recoveries when using the new nanoadsorbent are 97 % (as opposed to a mere 10 % in case of clinoptilolite only). It is assumed that the graphene sheets located around the porous structure of clinoptilolite are acting as a barrier against macromolecules potentially existing in the sample matrices. The method was applied to the determination of lead and cadmium in water and human serum samples by electrothermal atomic absorption spectrometry. The detection limits were as low as 70 and 4 ng L −1 for Pb(II) and Cd(II), respectively. The accuracy of the method was underpinned by correct analysis of a standard reference material (SRM: 203105 Seronorm Trace Elements Serum L-2). (author)

Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

Science.gov (United States)

Çabuk, Hasan; Köktürk, Mustafa

2013-01-01

A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries. PMID:23853535

Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

Directory of Open Access Journals (Sweden)

Hasan Çabuk

2013-01-01

Full Text Available A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries.

Extensible automated dispersive liquid–liquid microextraction

Energy Technology Data Exchange (ETDEWEB)

Li, Songqing; Hu, Lu; Chen, Ketao; Gao, Haixiang, E-mail: hxgao@cau.edu.cn

2015-05-04

Highlights: • An extensible automated dispersive liquid–liquid microextraction was developed. • A fully automatic SPE workstation with a modified operation program was used. • Ionic liquid-based in situ DLLME was used as model method. • SPE columns packed with nonwoven polypropylene fiber was used for phase separation. • The approach was applied to the determination of benzoylurea insecticides in water. - Abstract: In this study, a convenient and extensible automated ionic liquid-based in situ dispersive liquid–liquid microextraction (automated IL-based in situ DLLME) was developed. 1-Octyl-3-methylimidazolium bis[(trifluoromethane)sulfonyl]imide ([C{sub 8}MIM]NTf{sub 2}) is formed through the reaction between [C{sub 8}MIM]Cl and lithium bis[(trifluoromethane)sulfonyl]imide (LiNTf{sub 2}) to extract the analytes. Using a fully automatic SPE workstation, special SPE columns packed with nonwoven polypropylene (NWPP) fiber, and a modified operation program, the procedures of the IL-based in situ DLLME, including the collection of a water sample, injection of an ion exchange solvent, phase separation of the emulsified solution, elution of the retained extraction phase, and collection of the eluent into vials, can be performed automatically. The developed approach, coupled with high-performance liquid chromatography–diode array detection (HPLC–DAD), was successfully applied to the detection and concentration determination of benzoylurea (BU) insecticides in water samples. Parameters affecting the extraction performance were investigated and optimized. Under the optimized conditions, the proposed method achieved extraction recoveries of 80% to 89% for water samples. The limits of detection (LODs) of the method were in the range of 0.16–0.45 ng mL{sup −1}. The intra-column and inter-column relative standard deviations (RSDs) were <8.6%. Good linearity (r > 0.9986) was obtained over the calibration range from 2 to 500 ng mL{sup −1}. The proposed

Extensible automated dispersive liquid–liquid microextraction

International Nuclear Information System (INIS)

Li, Songqing; Hu, Lu; Chen, Ketao; Gao, Haixiang

2015-01-01

Highlights: • An extensible automated dispersive liquid–liquid microextraction was developed. • A fully automatic SPE workstation with a modified operation program was used. • Ionic liquid-based in situ DLLME was used as model method. • SPE columns packed with nonwoven polypropylene fiber was used for phase separation. • The approach was applied to the determination of benzoylurea insecticides in water. - Abstract: In this study, a convenient and extensible automated ionic liquid-based in situ dispersive liquid–liquid microextraction (automated IL-based in situ DLLME) was developed. 1-Octyl-3-methylimidazolium bis[(trifluoromethane)sulfonyl]imide ([C 8 MIM]NTf 2 ) is formed through the reaction between [C 8 MIM]Cl and lithium bis[(trifluoromethane)sulfonyl]imide (LiNTf 2 ) to extract the analytes. Using a fully automatic SPE workstation, special SPE columns packed with nonwoven polypropylene (NWPP) fiber, and a modified operation program, the procedures of the IL-based in situ DLLME, including the collection of a water sample, injection of an ion exchange solvent, phase separation of the emulsified solution, elution of the retained extraction phase, and collection of the eluent into vials, can be performed automatically. The developed approach, coupled with high-performance liquid chromatography–diode array detection (HPLC–DAD), was successfully applied to the detection and concentration determination of benzoylurea (BU) insecticides in water samples. Parameters affecting the extraction performance were investigated and optimized. Under the optimized conditions, the proposed method achieved extraction recoveries of 80% to 89% for water samples. The limits of detection (LODs) of the method were in the range of 0.16–0.45 ng mL −1 . The intra-column and inter-column relative standard deviations (RSDs) were <8.6%. Good linearity (r > 0.9986) was obtained over the calibration range from 2 to 500 ng mL −1 . The proposed method opens a new avenue

Comparison of Ultrasound-Guided and Fluoroscopy-Assisted Antegrade Common Femoral Artery Puncture Techniques

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Slattery, Michael M.; Goh, Gerard S.; Power, Sarah; Given, Mark F.; McGrath, Frank P.; Lee, Michael J., E-mail: mlee@rcsi.ie [Beaumont Hospital, Department of Radiology (Ireland)

2015-06-15

PurposeTo prospectively compare the procedural time and complication rates of ultrasound-guided and fluoroscopy-assisted antegrade common femoral artery (CFA) puncture techniques.Materials and MethodsHundred consecutive patients, undergoing a vascular procedure for which an antegrade approach was deemed necessary/desirable, were randomly assigned to undergo either ultrasound-guided or fluoroscopy-assisted CFA puncture. Time taken from administration of local anaesthetic to vascular sheath insertion in the superficial femoral artery (SFA), patients’ age, body mass index (BMI), fluoroscopy radiation dose, haemostasis method and immediate complications were recorded. Mean and median values were calculated and statistically analysed with unpaired t tests.ResultsSixty-nine male and 31 female patients underwent antegrade puncture (mean age 66.7 years). The mean BMI was 25.7 for the ultrasound-guided (n = 53) and 25.3 for the fluoroscopy-assisted (n = 47) groups. The mean time taken for the ultrasound-guided puncture was 7 min 46 s and for the fluoroscopy-assisted technique was 9 min 41 s (p = 0.021). Mean fluoroscopy dose area product in the fluoroscopy group was 199 cGy cm{sup 2}. Complications included two groin haematomas in the ultrasound-guided group and two retroperitoneal haematomas and one direct SFA puncture in the fluoroscopy-assisted group.ConclusionUltrasound-guided technique is faster and safer for antegrade CFA puncture when compared to the fluoroscopic-assisted technique alone.

Intraoperative registered transrectal ultrasound guidance for robot-assisted laparoscopic radical prostatectomy.

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Mohareri, Omid; Ischia, Joseph; Black, Peter C; Schneider, Caitlin; Lobo, Julio; Goldenberg, Larry; Salcudean, Septimiu E

2015-01-01

To provide unencumbered real-time ultrasound image guidance during robot-assisted laparoscopic radical prostatectomy, we developed a robotic transrectal ultrasound system that tracks the da Vinci® Surgical System instruments. We describe our initial clinical experience with this system. After an evaluation in a canine model, 20 patients were enrolled in the study. During each procedure the transrectal ultrasound transducer was manually positioned using a brachytherapy stabilizer to provide good imaging of the prostate. Then the transrectal ultrasound was registered to the da Vinci robot by a previously validated procedure. Finally, automatic rotation of the transrectal ultrasound was enabled such that the transrectal ultrasound imaging plane safely tracked the tip of the da Vinci instrument controlled by the surgeon, while real-time transrectal ultrasound images were relayed to the surgeon at the da Vinci console. Tracking was activated during all critical stages of the surgery. The transrectal ultrasound robot was easy to set up and use, adding 7 minutes (range 5 to 14) to the procedure. It did not require an assistant or additional control devices. Qualitative feedback was acquired from the surgeons, who found transrectal ultrasound useful in identifying the urethra while passing the dorsal venous complex suture, defining the prostate-bladder interface during bladder neck dissection, identifying the seminal vesicles and their location with respect to the rectal wall, and identifying the distal prostate boundary at the apex. Real-time, registered robotic transrectal ultrasound guidance with automatic instrument tracking during robot-assisted laparoscopic radical prostatectomy is feasible and potentially useful. The results justify further studies to establish whether the approach can improve procedure outcomes. Copyright © 2015 American Urological Association Education and Research, Inc. Published by Elsevier Inc. All rights reserved.

KINETICS OF ULTRASOUND ASSISTED EXTRACTION OF WEDELOLACTONE FROM Eclipta alba

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T. W. Charpe

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

Ultrasound-assisted oxidative desulfurization of bitumen

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Kamal, Wan Mohamad Ikhwan bin Wan; Okawa, Hirokazu; Kato, Takahiro; Sugawara, Katsuyasu

2017-07-01

Bitumen contains a high percentage of sulfur (about 4.6 wt %). A hydrodesulfurization method is used to remove sulfur from bitumen. The drawback of this method is the requirement for a high temperature of >300 °C. Most of the sulfur in bitumen exists as thiophene. Oxidative desulfurization (ODS), involving oxidizing sulfur using H2O2, then removing it using NaOH, allows the removal of sulfur in thiophene at low temperatures. We removed sulfur from bitumen using ODS treatment under ultrasound irradiation, and 52% of sulfur was successfully removed. Additionally, the physical action of ultrasound assisted the desulfurization of bitumen, even at low H2O2 concentrations.

Dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Zeini Jahromi, Elham; Bidari, Araz; Assadi, Yaghoub; Milani Hosseini, Mohammad Reza; Jamali, Mohammad Reza

2007-01-01

Dispersive liquid-liquid microextraction (DLLME) technique was successfully used as a sample preparation method for graphite furnace atomic absorption spectrometry (GF AAS). In this extraction method, 500 μL methanol (disperser solvent) containing 34 μL carbon tetrachloride (extraction solvent) and 0.00010 g ammonium pyrrolidine dithiocarbamate (chelating agent) was rapidly injected by syringe into the water sample containing cadmium ions (interest analyte). Thereby, a cloudy solution formed. The cloudy state resulted from the formation of fine droplets of carbon tetrachloride, which have been dispersed, in bulk aqueous sample. At this stage, cadmium reacts with ammonium pyrrolidine dithiocarbamate, and therefore, hydrophobic complex forms which is extracted into the fine droplets of carbon tetrachloride. After centrifugation (2 min at 5000 rpm), these droplets were sedimented at the bottom of the conical test tube (25 ± 1 μL). Then a 20 μL of sedimented phase containing enriched analyte was determined by GF AAS. Some effective parameters on extraction and complex formation, such as extraction and disperser solvent type and their volume, extraction time, salt effect, pH and concentration of the chelating agent have been optimized. Under the optimum conditions, the enrichment factor 125 was obtained from only 5.00 mL of water sample. The calibration graph was linear in the rage of 2-20 ng L -1 with detection limit of 0.6 ng L -1 . The relative standard deviation (R.S.D.s) for ten replicate measurements of 20 ng L -1 of cadmium was 3.5%. The relative recoveries of cadmium in tap, sea and rivers water samples at spiking level of 5 and 10 ng L -1 are 108, 95, 87 and 98%, respectively. The characteristics of the proposed method have been compared with cloud point extraction (CPE), on-line liquid-liquid extraction, single drop microextraction (SDME), on-line solid phase extraction (SPE) and co-precipitation based on bibliographic data. Therefore, DLLME combined with

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

International Nuclear Information System (INIS)

Shirkhanloo, H.; Sedighi, K.; Mousavi, H. Z.

2014-01-01

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

Robot-assisted ultrasound imaging: overview and development of a parallel telerobotic system.

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Monfaredi, Reza; Wilson, Emmanuel; Azizi Koutenaei, Bamshad; Labrecque, Brendan; Leroy, Kristen; Goldie, James; Louis, Eric; Swerdlow, Daniel; Cleary, Kevin

2015-02-01

Ultrasound imaging is frequently used in medicine. The quality of ultrasound images is often dependent on the skill of the sonographer. Several researchers have proposed robotic systems to aid in ultrasound image acquisition. In this paper we first provide a short overview of robot-assisted ultrasound imaging (US). We categorize robot-assisted US imaging systems into three approaches: autonomous US imaging, teleoperated US imaging, and human-robot cooperation. For each approach several systems are introduced and briefly discussed. We then describe a compact six degree of freedom parallel mechanism telerobotic system for ultrasound imaging developed by our research team. The long-term goal of this work is to enable remote ultrasound scanning through teleoperation. This parallel mechanism allows for both translation and rotation of an ultrasound probe mounted on the top plate along with force control. Our experimental results confirmed good mechanical system performance with a positioning error of < 1 mm. Phantom experiments by a radiologist showed promising results with good image quality.

Progress in Imidazolium Ionic Liquids Assisted Fabrication of Carbon Nanotube and Graphene Polymer Composites

Directory of Open Access Journals (Sweden)

Xiaolin Xie

2013-06-01

Full Text Available Carbon nanotubes (CNTs and graphene sheets are the most promising fillers for polymer nanocomposites due to their superior mechanical, electrical, thermal optical and gas barrier properties, as well as high flame-retardant efficiency. The critical challenge, however, is how to uniformly disperse them into the polymer matrix to achieve a strong interface for good load transfer between the two. This problem is not new but more acute in CNTs and graphene, both because they are intrinsically insoluble and tend to aggregate into bundles and because their surfaces are atomically smooth. Over the past decade, imidazolium ionic liquids (Imi-ILs have played a multifunctional role (e.g., as solvents, dispersants, stabilizers, compatibilizers, modifiers and additives in the fabrication of polymer composites containing CNTs or graphene. In this review, we first summarize the liquid-phase exfoliation, stabilization, dispersion of CNTs and graphene in Imi-ILs, as well as the chemical and/or thermal reduction of graphene oxide to graphene with the aid of Imi-ILs. We then present a full survey of the literature on the Imi-ILs assisted fabrication of CNTs and graphene-based nanocomposites with a variety of polymers, including fluoropolymers, hydrocarbon polymers, polyacrylates, cellulose and polymeric ionic liquids. Finally, we give a future outlook in hopes of facilitating progress in this emerging area.

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

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

2011-04-01

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

Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction

International Nuclear Information System (INIS)

Chisvert, Alberto; Benedé, Juan L.; Anderson, Jared L.; Pierson, Stephen A.; Salvador, Amparo

2017-01-01

With the aim of contributing to the development and improvement of microextraction techniques, a novel approach combining the principles and advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) is presented. This new approach, termed stir bar dispersive liquid microextraction (SBDLME), involves the addition of a magnetic ionic liquid (MIL) and a neodymium-core magnetic stir bar into the sample allowing the MIL coat the stir bar due to physical forces (i.e., magnetism). As long as the stirring rate is maintained at low speed, the MIL resists rotational (centrifugal) forces and remains on the stir bar surface in a manner closely resembling SBSE. By increasing the stirring rate, the rotational forces surpass the magnetic field and the MIL disperses into the sample solution in a similar manner to DLLME. After extraction, the stirring is stopped and the MIL returns to the stir bar without the requirement of an additional external magnetic field. The MIL-coated stir bar containing the preconcentrated analytes is thermally desorbed directly into a gas chromatographic system coupled to a mass spectrometric detector (TD-GC-MS). This novel approach opens new insights into the microextraction field, by using the benefits provided by SBSE and DLLME simultaneously, such as automated thermal desorption and high surface contact area, respectively, but most importantly, it enables the use of tailor-made solvents (i.e., MILs). To prove its utility, SBDLME has been used in the extraction of lipophilic organic UV filters from environmental water samples as model analytical application with excellent analytical features in terms of linearity, enrichment factors (67–791), limits of detection (low ng L −1 ), intra- and inter-day repeatability (RSD<15%) and relative recoveries (87–113%, 91–117% and 89–115% for river, sea and swimming pool water samples, respectively). - Highlights: • A new microextraction method combining the

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.

Ultrasound-based measurement of liquid-layer thickness: A novel time-domain approach

Science.gov (United States)

Praher, Bernhard; Steinbichler, Georg

2017-01-01

Measuring the thickness of a thin liquid layer between two solid materials is important when the adequate separation of metallic parts by a lubricant film (e.g., in bearings or mechanical seals) is to be assessed. The challenge in using ultrasound-based systems for such measurements is that the signal from the liquid layer is a superposition of multiple reflections. We have developed an algorithm for reconstructing this superimposed signal in the time domain. By comparing simulated and measured signals, the time-of-flight of the ultrasonic pulse in a layer can be estimated. With the longitudinal sound velocity known, the layer thickness can then be calculated. In laboratory measurements, we validate successfully (maximum relative error 4.9%) our algorithm for layer thicknesses ranging from 30 μm to 200 μm. Furthermore, we tested our method in the high-temperature environment of polymer processing by measuring the clearance between screw and barrel in the plasticisation unit of an injection moulding machine. The results of such measurements can indicate (i) the wear status of the tribo-mechanical screw-barrel system and (ii) unsuitable process conditions.

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. Copyright © 2010 Elsevier B.V. All rights reserved.

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. Copyright 2009 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2017-01-01

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

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

Science.gov (United States)

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

2015-05-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2014-10-01

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

Rapid determination of octanol-water partition coefficient using vortex-assisted liquid-liquid microextraction.

Science.gov (United States)

Román, Iván P; Mastromichali, Anna; Tyrovola, Konstantina; Canals, Antonio; Psillakis, Elefteria

2014-02-21

Vortex-assisted liquid-liquid microextraction (VALLME) coupled with high-performance liquid chromatography (HPLC) is proposed here for the rapid determination of octanol-water partitioning coefficients (Kow). VALLME uses vortex agitation, a mild emulsification procedure, to disperse microvolumes of octanol in the aqueous phase thus increasing the interfacial contact area and ensuring faster partitioning rates. With VALLME, 2min were enough to achieve equilibrium conditions between the octanolic and aqueous phases. Upon equilibration, separation was achieved using centrifugation and the octanolic microdrop was collected and analyzed in a HPLC system. Six model compounds with logKow values ranging between ∼0.5 and 3.5 were used during the present investigations. The proposed method produced logKow values that were consistent with previously published values and the recorded uncertainty was well within the acceptable log unit range. Overall, the key features of the proposed Kow determination procedure comprised speed, reliability, simplicity, low cost and minimal solvent consumption. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Ultrasound-assisted synthesis and processing of carbon materials

Science.gov (United States)

Fortunato, Maria E.

2011-12-01

heating (˜5000 K), high pressures (˜300 atm), and enormous heating and cooling rates (>109 K/sec). In solid-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.

Ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction for the separation and determination of estrogens in water samples by high-performance liquid chromatography with fluorescence detection.

Science.gov (United States)

Zhang, Rui; Wang, Chuanliu; Yue, Qiaohong; Zhou, Tiecheng; Li, Na; Zhang, Hanqi; Hao, Xiaoke

2014-11-01

An ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction method was proposed for the extraction and concentration of 17-α-estradiol, 17-β-estradiol-benzoate, and quinestrol in environmental water samples by high-performance liquid chromatography with fluorescence detection. 1-Hexyl-3-methylimidazolium tetrafluoroborate was applied as foaming agent in the foam flotation process and dispersive solvent in microextraction. The introduction of the ion-pairing and salting-out agent NH4 PF6 was beneficial to the improvement of recoveries for the hydrophobic ionic liquid phase and analytes. Parameters of the proposed method including concentration of 1-hexyl-3-methylimidazolium tetrafluoroborate, flow rate of carrier gas, floatation time, types and concentration of ionic liquids, salt concentration in samples, extraction time, and centrifugation time were evaluated. The recoveries were between 98 and 105% with relative standard deviations lower than 7% for lake water and well water samples. The isolation of the target compounds from the water was found to be efficient, and the enrichment factors ranged from 4445 to 4632. This developing method is free of volatile organic solvents compared with regular extraction. Based on the unique properties of ionic liquids, the application of foam floatation, and dispersive liquid-liquid microextraction was widened. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous in situ derivatization and ultrasound-assisted dispersive magnetic solid phase extraction for thiamine determination by spectrofluorimetry.

Science.gov (United States)

Tarigh, Ghazale Daneshvar; Shemirani, Farzaneh

2014-06-01

A simple and rapid method for the simultaneous in situ derivatizaion, preconcentration and extraction of thiamine (vitamin B1) as a model analyte was developed by a novel quantitative method, namely ultrasound-assisted dispersive magnetic solid phase extraction spectrofluorimetry (USA-DMSPE-FL) from different real samples. This method consists of sample preparation, in situ derivatization, exhaustive extraction and clean up by a single process. High extraction efficiency and in situ derivatization in a short period of time is the main advantages of this procedure. For this purpose, the reusable magnetic multi-wall carbon nanotube (MMWCNT) nanocomposite was used as an adsorbent for preconcentration and determination of thiamine. Thiamine was, simultaneously, in situ derivatized as thiochrome by potassium hexacyanoferrate (III) and adsorbed on MMWCNT in an ultrasonic water bath. The MMWCNTs were then collected using an external magnetic field. Subsequently, the extracted thiochrome was washed from the surface of the adsorbent and determined by spectrofluorimetry. The developed method, which has been analytically characterized under its optimal operating conditions, allows the detection of the analyte in the samples with method detection limits of 0.37 µg L(-1). The repeatability of the method, expressed as the relative standard deviation (RSD, n=6), varies between 2.0% and 4.8% in different real samples, while the enhancement factor is 197. The proposed procedure has been applied for the determination of thiamine in biological (serum and urine), pharmaceutical (multivitamin tablet and B complex syrup) and foodstuff samples (cereal, wheat flour, banana and honey) with the good recoveries in the range from 90% to 105%. Copyright © 2014 Elsevier B.V. All rights reserved.

Phosphonium–based ionic liquid as dispersing agent for MWCNT in melt-mixing polystyrene blends: Rheology, electrical properties and EMI shielding effectiveness

Energy Technology Data Exchange (ETDEWEB)

Soares da Silva, Jéssica P. [Universidade Federal do Rio de Janeiro, Instituto de Macromoléculas, 21941-598, Rio de Janeiro (Brazil); Soares, Bluma G., E-mail: bluma@metalmat.ufrj.br [Universidade Federal do Rio de Janeiro, Instituto de Macromoléculas, 21941-598, Rio de Janeiro (Brazil); Universidade Federal do Rio de Janeiro, Programa de Engenharia Metalurgica e de Materiais - COPPE, Centro de Tecnologia, 21941-972, Rio de Janeiro (Brazil); Livi, Sebastien [Université de Lyon, F-69003, Lyon (France); INSA Lyon, F-69621, Villeurbanne (France); CNRS, UMR 5223, Ingénierie des Matériaux Polymères (France); Barra, Guilherme M.O. [Universidade Federal de Santa Catarina, Departamento de Engenharia Mecânica, Florianópolis, SC (Brazil)

2017-03-01

Conducting nanocomposites composed with polystyrene (PS) and multi-walled carbon nanotubes (MWCNT) were prepared by melt mixing procedure assisted by trihexyl-(tetradecyl)-phosphonium combined with bis(trifluoromethylsulfonyl) amide counteranion (TFSI) as the ionic liquid (IL). The non-covalent functionalization of MWCNT with the IL was confirmed by Raman spectroscopy and thermogravimetric analysis. The functionalized MWCNT provided better dispersion of the MWCNT within PS matrix, as indicated by transmission electron microscopy (TEM), and also an electrical conductivity as high as 10{sup −1} S/m with 0.66 m% of MWCNT combined with 3.34 m% of IL. This value is around four orders of magnitude higher when compared to nanocomposites with similar amount of untreated MWCNT. From rheological studies, it was observed that the transition between liquid-like to solid-like behavior occurred at lower frequencies for the systems containing functionalized MWCNT. Moreover, an improvement of around 170% in the electromagnetic interference shielding effectiveness (EMI SE) in the X-band frequency range was observed for the nanocomposites containing 1% of MWCNT non-covalently functionalized with the IL, that is, 1% of MWCNT and 5% of IL. - Highlights: • MWCNT well dispersed in PS matrix, in the presence of ionic liquid. • Outstanding electric conductivity of PS/MWCNT nanocomposite. • Improved EMI shielding effectiveness by addition of ionic liquid in PS/MWCNT nanocomposite.

Centrifugeless dispersive liquid-liquid microextraction based on salting-out phenomenon followed by high performance liquid chromatography for determination of Sudan dyes in different species.

Science.gov (United States)

Bazregar, Mohammad; Rajabi, Maryam; Yamini, Yadollah; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

2018-04-01

In this work, a novel method, namely centrifugeless dispersive liquid-liquid microextraction, is introduced for the efficient extraction of banned Sudan dyes from foodstuff and water samples. In this method, which is based upon the salting-out phenomenon, in order to accelerate the extraction process, the extraction solvent (1-undecanol, 75 μL) is dispersed into the sample solution. Then the mixture is passed through a small column filled with 5 g sodium chloride, used as a separating reagent. In this condition, fine droplets of the extraction solvent are floated on the mixture, and the phase separation is simply achieved. This method is environmentally friendly, simple, and very fast, so that the overall extraction time is only 7 min. Under the optimal experimental conditions, the preconcentration factors in the range of 90-121 were obtained for the analytes. Also good linearities were obtained in the range of 2.5-1200 ng mL -1 (r 2  ≥ 0.993). Copyright © 2017 Elsevier Ltd. All rights reserved.

Overcoming the challenges of conventional dispersive liquid-liquid microextraction: analysis of THMs in chlorinated swimming pools.

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Faraji, Hakim; Helalizadeh, Masoumeh; Kordi, Mohammad Reza

2018-01-01

A rapid, simple, and sensitive approach to the analysis of trihalomethanes (THMs) in swimming pool water samples has been developed. The main goal of this study was to overcome or to improve the shortcomings of conventional dispersive liquid-liquid microextraction (DLLME) and to maximize the realization of green analytical chemistry principles. The method involves a simple vortex-assisted microextraction step, in the absence of the dispersive solvent, followed by salting-out effect for the elimination of the centrifugation step. A bell-shaped device and a solidifiable solvent were used to simplify the extraction solvent collection after phase separation. Optimization of the independent variables was performed by using chemometric methods in three steps. The method was statistically validated based on authentic guidance documents. The completion time for extraction was less than 8 min, and the limits of detection were in the range between 4 and 72 ng L -1 . Using this method, good linearity and precision were achieved. The results of THMs determination in different real samples showed that in some cases the concentration of total THMs was more than threshold values of THMs determined by accredited healthcare organizations. This method indicated satisfactory analytical figures of merit. Graphical Abstract A novel green microextraction technique for overcoming the challenges of conventional DLLME. The proposed procedure complies with the principles of green/sustainable analytical chemistry, comprising decreasing the sample size, making easy automation of the process, reducing organic waste, diminishing energy consumption, replacing toxic reagents with safer reagents, and enhancing operator safety.

Temperature-assisted On-column Solute Focusing: A General Method to Reduce Pre-column Dispersion in Capillary High Performance Liquid Chromatography

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Groskreutz, Stephen R.; Weber, Stephen G.

2014-01-01

Solvent-based on-column focusing is a powerful and well known approach for reducingthe impact of pre-column dispersion in liquid chromatography. Here we describe an orthogonal temperature-based approach to focusing called temperature-assisted on-column solute focusing (TASF). TASF is founded on the same principles as the more commonly used solvent-based method wherein transient conditions are created thatlead to high solute retention at the column inlet. Combining the low thermal mass of capillary columns and the temperature dependence of solute retentionTASF is used effectivelyto compress injection bands at the head of the column through the transient reduction in column temperature to 5 °C for a defined 7 mm segment of a 6 cm long 150 μm I.D. column. Following the 30 second focusing time, the column temperature is increased rapidly to the separation temperature of 60 °C releasing the focused band of analytes. We developed a model tosimulate TASF separations based on solute retention enthalpies, focusing temperature, focusing time, and column parameters. This model guides the systematic study of the influence of sample injection volume on column performance.All samples have solvent compositions matching the mobile phase. Over the 45 to 1050 nL injection volume range evaluated, TASF reducesthe peak width for all soluteswith k’ greater than or equal to 2.5, relative to controls. Peak widths resulting from injection volumes up to 1.3 times the column fluid volume with TASF are less than 5% larger than peak widths from a 45 nL injection without TASF (0.07 times the column liquid volume). The TASF approach reduced concentration detection limits by a factor of 12.5 relative to a small volume injection for low concentration samples. TASF is orthogonal to the solvent focusing method. Thus, it canbe used where on-column focusing is required, but where implementation of solvent-based focusing is difficult. PMID:24973805

Ultrasound-assisted extraction for total sulphur measurement in mine tailings

International Nuclear Information System (INIS)

Khan, Adnan Hossain; Shang, Julie Q.; Alam, Raquibul

2012-01-01

Highlights: ► We develop a total sulphur measuring procedure of mine tailings. ► Ultrasound is used in the sample pre-treatment process. ► Full factorial design is applied to identify the best level of effecting factors. - Abstract: A sample preparation method for percentage recovery of total sulphur (%S) in reactive mine tailings based on ultrasound-assisted digestion (USAD) and inductively coupled plasma-optical emission spectroscopy (ICP-OES) was developed. The influence of various methodological factors was screened by employing a two-level and three-factor (2 3 ) full factorial design and using KZK-1, a sericite schist certified reference material (CRM), to find the optimal combination of studied factors and %S. Factors such as the sonication time, temperature and acid combination were studied, with the best result identified as 20 min of sonication, 80 °C temperature and 1 ml of HNO 3 :1 ml of HCl, which can achieve 100% recovery for the selected CRM. Subsequently a fraction of the 2 3 full factorial design was applied to mine tailings. The percentage relative standard deviation (%RSD) for the ultrasound method is less than 3.0% for CRM and less than 6% for the mine tailings. The investigated method was verified by X-ray diffraction analysis. The USAD method compared favorably with existing methods such as hot plate assisted digestion method, X-ray fluorescence and LECO™-CNS method.

The role for peer-assisted ultrasound teaching in medical school.

Science.gov (United States)

Dickerson, Jonathan; Paul, Katie; Vila, Pierre; Whiticar, Rebecca

2017-06-01

Bedside ultrasonography has an increasing role in medicine yet medical students have limited exposure. Although countless hours are devoted to plain radiograph and electrocardiogram (ECG) interpretation, ultrasound is frequently glossed over. Yet this imaging modality could enhance students' understanding of anatomy, physiology and pathology, and may increase their integration into hospital teams. We aimed to investigate whether a peer-assisted ultrasound course has a place within the undergraduate medical curriculum. We describe the implementation of a course and discuss its acceptability and utility in student education. Bedside ultrasonography has an increasing role in medicine yet medical students have limited exposure METHODS: Following consultation with the medical school, an improved ultrasonography course was developed with expert guidance from an ultrasonographer and with new equipment. Sessions involved peer-tutors teaching ultrasonography techniques to medical students during emergency medicine placements. Tutees completed questionnaires to assess the quality and perceived benefits of the course and of learning ultrasonography. Both quantitative and thematic analyses of the responses were conducted by the authors. Over a period of 8 months, 105 medical students received teaching across four sessions. A total of 103 students (98%) returned questionnaires on their evaluation of the course and tutors, and on their confidence in using ultrasound. Ninety-eight per cent felt that the teaching was well delivered, 100 per cent felt that their knowledge of ultrasound had improved and 100 per cent would recommend the course. The peer-assisted ultrasound course described here enabled the majority of students to feel confident gaining elementary ultrasound views, and performing abdominal aneurysm screening and trauma assessments: techniques that they could hopefully put to use during their placements. The peer-assisted model has an acceptable role in teaching

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).

Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction.

Science.gov (United States)

Chisvert, Alberto; Benedé, Juan L; Anderson, Jared L; Pierson, Stephen A; Salvador, Amparo

2017-08-29

With the aim of contributing to the development and improvement of microextraction techniques, a novel approach combining the principles and advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) is presented. This new approach, termed stir bar dispersive liquid microextraction (SBDLME), involves the addition of a magnetic ionic liquid (MIL) and a neodymium-core magnetic stir bar into the sample allowing the MIL coat the stir bar due to physical forces (i.e., magnetism). As long as the stirring rate is maintained at low speed, the MIL resists rotational (centrifugal) forces and remains on the stir bar surface in a manner closely resembling SBSE. By increasing the stirring rate, the rotational forces surpass the magnetic field and the MIL disperses into the sample solution in a similar manner to DLLME. After extraction, the stirring is stopped and the MIL returns to the stir bar without the requirement of an additional external magnetic field. The MIL-coated stir bar containing the preconcentrated analytes is thermally desorbed directly into a gas chromatographic system coupled to a mass spectrometric detector (TD-GC-MS). This novel approach opens new insights into the microextraction field, by using the benefits provided by SBSE and DLLME simultaneously, such as automated thermal desorption and high surface contact area, respectively, but most importantly, it enables the use of tailor-made solvents (i.e., MILs). To prove its utility, SBDLME has been used in the extraction of lipophilic organic UV filters from environmental water samples as model analytical application with excellent analytical features in terms of linearity, enrichment factors (67-791), limits of detection (low ng L -1 ), intra- and inter-day repeatability (RSD<15%) and relative recoveries (87-113%, 91-117% and 89-115% for river, sea and swimming pool water samples, respectively). Copyright © 2017 Elsevier B.V. All rights reserved.

Combination of in situ metathesis reaction with a novel "magnetic effervescent tablet-assisted ionic liquid dispersive microextraction" for the determination of endogenous steroids in human fluids.

Science.gov (United States)

Wu, Jia; Xu, Zilin; Pan, Yixuan; Shi, Yi; Bao, Xiujie; Li, Jun; Tong, Yu; Tang, Han; Ma, Shuyan; Wang, Xuedong; Lyu, Jianxin

2018-05-01

Herein, a novel magnetic effervescence tablet-assisted microextraction coupled to in situ metathesis reaction of ionic liquid (IS-META-ILDM) is presented for the determination of four endogenous steroids in human urine, pregnant women's blood, and fetal umbilical cord blood. The magnetic effervescent tablets, which were composed of Fe 3 O 4 nanoparticles, sodium carbonate (alkaline source), and tartaric acid (acidic source), were used to disperse the extractant and for convenient magnetic separation. After the effervescent reaction, in situ reaction between NH 4 PF 6 and [C 6 MIM]BF 4 was adopted to change hydrophilic ionic liquid to hydrophobic liquid, which could be separated from the aqueous phase. The newly developed method has three obvious advantages: (1) combination of effervescent dispersion and magnetic nanoparticles' retrieval is cost-effective and the dispersion and collection of the extractant can be completed almost simultaneously; (2) as compared to temperature-controlled ionic liquid dispersive microextraction and cold-induced solidified microextraction, this method avoids a heating and cooling process which significantly reduces the extraction time and energy cost; and (3) the combination of adsorption by magnetic nanoparticles with extraction by in situ metathesis reaction easily produces high recoveries for target analytes. The optimized composition of effervescent tablet and experimental parameters are as follows: 0.64 g mixture of sodium carbonate and tartaric acid, 7 mg of Fe 3 O 4 (20 nm) as magnetic sorbents, 40 μL of [C 6 MIM]BF 4 as the extraction solvent, 0.15 g NH 4 PF 6 , and 300 μL of elution solvent. Under the optimized conditions, the newly developed method provided high extraction recoveries (90.0-118.5%) and low LODs (0.14-0.17 μg L -1 ) in urine and blood samples. In total, this IS-META-ILDM method provided high extraction efficiency, fast and convenient separation, and underutilization of any organic solvent, and thus

Ultrasound assisted evaluation of chest pain in the emergency department.

Science.gov (United States)

Colony, M Deborah; Edwards, Frank; Kellogg, Dylan

2018-04-01

Chest pain is a commonly encountered emergency department complaint, with a broad differential including several life-threatening possible conditions. Ultrasound-assisted evaluation can potentially be used to rapidly and accurately arrive at the correct diagnosis. We propose an organized, ultrasound assisted evaluation of the patient with chest pain using a combination of ultrasound, echocardiography and clinical parameters. Basic echo techniques which can be mastered by residents in a short time are used plus standardized clinical questions and examination. Information is kept on a checklist. We hypothesize that this will result in a quicker, more accurate evaluation of chest pain in the ED leading to timely treatment and disposition of the patient, less provider anxiety, a reduction in the number of diagnostic errors, and the removal of false assumptions from the diagnostic process. Copyright © 2017 Elsevier Inc. All rights reserved.

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

Science.gov (United States)

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

2018-01-01

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

Effect of silica nanoparticles on the phase inversion of liquid-liquid dispersions

International Nuclear Information System (INIS)

Asadabadi, Maliheh Raji; Abolghasemi, Hossein; Nasab, Payman Davoodi; Maragheh, Mohammad Ghannadi

2013-01-01

The effect of silica nanoparticles on phase inversion of liquid-liquid dispersions in a stirred vessel was investigated. The studied systems were toluene dispersed in water and vice versa. In the first set of experiments, phase inversion behavior of systems without Silica nanoparticles was evaluated and subsequent experiments were conducted in the presence of the nanoparticles. For this purpose, Silica nanoparticles of different concentrations (0.01, 0.03, 0.05, 0.07 wt%) were dispersed in water. The nanofluid stability was examined using an ultraviolet-visible (UV-vis) spectrophotometer. The results indicated that increase in silica nanoparticle concentrations up to 0.07 wt% led to increase in agitation speed of phase inversion 43-53.5% and 38.5-45% in the case of O/W and W/O dispersions, respectively. Consequently, the tendency of dispersions to inversion diminished as nanoparticle concentrations increased. Finally, 0.05 wt% of silica nanoparticle was selected as the optimum on the range studied

Tracked "Pick-Up" Ultrasound for Robot-Assisted Minimally Invasive Surgery.

Science.gov (United States)

Schneider, Caitlin; Nguan, Christopher; Rohling, Robert; Salcudean, Septimiu

2016-02-01

We present a novel "pick-up" ultrasound transducer for intraabdominal robot-assisted minimally invasive surgery. Such a "pick-up" ultrasound transducer is inserted through an abdominal incision at the beginning of the procedure and remains in the abdominal cavity throughout, eliminating the need for a dedicated port or a patient bedside surgical assistant. The transducer has a handle that can be grasped in a repeatable manner using a da Vinci Prograsp tool, allowing the transducer to be accurately manipulated by the surgeon using the da Vinci Robot. This is one way to enable 3-D tracking of the transducer, and, thus, mapping of the vasculature. The 3-D vascular images can be used to register preoperative CT to intraoperative camera images. To demonstrate the feasibility of the approach, we use an ultrasound vessel phantom to register a CT surface model to extracted ultrasound vessel models. The 3-D vascular phantom images are generated by segmenting B-mode images and tracking the pick-up ultrasound transducer with the da Vinci kinematics, internal electromagnetic sensor, or visible fiducials suitable for camera tracking. Reconstruction results using da Vinci kinematics for tracking give a target registration error of 5.4 ± 1.7 mm.

Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

Science.gov (United States)

Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

2015-08-01

A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L- 1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L- 1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract.

Ultrasound assisted PTC catalyzed saponification of vegetable oils using aqueous alkali.

Science.gov (United States)

Bhatkhande, B S; Samant, S D

1998-03-01

A few vegetable oils were saponified using aqueous KOH and different PTCs at room temperature in the presence of ultrasound. The extent of saponification was studied using the saponification value as a reference. Optimizations of various parameters such as time, selection of PTC, quantity of PTC, quantity of KOH and quantity of water were carried out using soyabean oil as a sample oil under sonication with stirring. To study the effect of ultrasound, the saponification was also carried out at 35 +/- 2 degrees C under different conditions, namely stirring, sonication, stirring and sonication, and heating at 100 degrees C. It was found that the heterogeneous liquid-liquid phase saponification of different vegetable oils using aq. KOH/CTAB was remarkably accelerated at 35 +/- 2 degrees C in the presence of ultrasound along with stirring.

Application of dispersive liquid-liquid microextraction and dispersive micro-solid-phase extraction for the determination of quinolones in swine muscle by high-performance liquid chromatography with diode-array detection

International Nuclear Information System (INIS)

Tsai, Wen-Hsien; Chuang, Hung-Yi; Chen, Ho-Hsien; Huang, Joh-Jong; Chen, Hwi-Chang; Cheng, Shou-Hsun; Huang, Tzou-Chi

2009-01-01

Dispersive liquid-liquid microextraction (DLLME) and dispersive micro-solid-phase extraction (DMSPE) are two simple and low-cost sample preparation methods for liquid samples. In this work, these two methods were applied to solid tissue sample for the determination of seven quinolones by high-performance liquid chromatography with diode-array detection (HPLC-DAD). After the homogenization of the swine muscle with acetonitrile and salt-promoted partitioning, small amounts of the extract were used for the DLLME and DMSPE methods. In the DLLME approach, the target analytes in the extraction solvent were rapidly extracted into a small volume of dichloromethane for drying and the residue was reconstituted for HPLC-DAD analysis. In the DMSPE approach, the target analytes in the extraction solvent were trapped by dispersive silica-based PSA (primary and secondary amine) sorbents and desorbed into a small amount of desorption solution for HPLC-DAD analysis. Under the optimal conditions, relative recoveries were determined for swine muscle spiked 50-200 μg kg -1 and quantification was achieved by matrix-matched calibration. The calibration curves of seven quinolones showed linearity with a correlation coefficient value above 0.998 for both approaches. Relative recoveries ranged from 93.0 to 104.7% and from 95.5 to 111.0% for DLLME and DMSPE, respectively. Limits of detection (LODs) ranged from 5.6 to 23.8 μg kg -1 and from 7.5 to 26.3 μg kg -1 for DLLME and DMSPE, respectively.

Ultrasound assisted synthesis of iron doped TiO2 catalyst.

Science.gov (United States)

Ambati, Rohini; Gogate, Parag R

2018-01-01

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

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.

Ultrasound-assisted extraction for total sulphur measurement in mine tailings

Energy Technology Data Exchange (ETDEWEB)

Khan, Adnan Hossain, E-mail: ad_li2@yahoo.com [Department of Civil and Environmental Engineering, University of Western Ontario (Canada); Shang, Julie Q.; Alam, Raquibul [Department of Civil and Environmental Engineering, University of Western Ontario (Canada)

2012-10-15

Highlights: Black-Right-Pointing-Pointer We develop a total sulphur measuring procedure of mine tailings. Black-Right-Pointing-Pointer Ultrasound is used in the sample pre-treatment process. Black-Right-Pointing-Pointer Full factorial design is applied to identify the best level of effecting factors. - Abstract: A sample preparation method for percentage recovery of total sulphur (%S) in reactive mine tailings based on ultrasound-assisted digestion (USAD) and inductively coupled plasma-optical emission spectroscopy (ICP-OES) was developed. The influence of various methodological factors was screened by employing a two-level and three-factor (2{sup 3}) full factorial design and using KZK-1, a sericite schist certified reference material (CRM), to find the optimal combination of studied factors and %S. Factors such as the sonication time, temperature and acid combination were studied, with the best result identified as 20 min of sonication, 80 Degree-Sign C temperature and 1 ml of HNO{sub 3}:1 ml of HCl, which can achieve 100% recovery for the selected CRM. Subsequently a fraction of the 2{sup 3} full factorial design was applied to mine tailings. The percentage relative standard deviation (%RSD) for the ultrasound method is less than 3.0% for CRM and less than 6% for the mine tailings. The investigated method was verified by X-ray diffraction analysis. The USAD method compared favorably with existing methods such as hot plate assisted digestion method, X-ray fluorescence and LECO Trade-Mark-Sign -CNS method.

Preconcentration of valsartan by dispersive liquid-liquid microextraction based on solidification of floating organic drop and its determination in urine sample: Central composite design.

Science.gov (United States)

Pebdani, Arezou Amiri; Shabani, Ali Mohammad Haji; Dadfarnia, Shayesteh; Talebianpoor, Mohammad Sharif; Khodadoust, Saeid

2016-05-01

In this work, a fast, easy, and efficient dispersive liquid-liquid microextraction method based on solidification of floating organic drop followed by high-performance liquid chromatography with UV detection was developed for the separation/preconcentration and determination of the drug valsartan. Experimental design was applied for the optimization of the effective variables (such as volume of extracting and dispersing solvents, ionic strength, and pH) on the extraction efficiency of valsartan from urine samples. The optimized values were 250.0 μL ethanol, 65.0 μL 1-dodecanol, 4.0% w/v NaCl, pH 3.8, 1.0 min extraction time, and 4.0 min centrifugation at 4000 rpm min(-1) . The linear response (r(2) = 0.997) was obtained in the range of 0.013-10.0 μg mL(-1) with a limit of detection of 4.0 ng mL(-1) and relative standard deviations of less than 5.0 % (n = 6). © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Science.gov (United States)

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

2014-10-01

Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction was developed and applied to the extraction of pesticides in high fatty matrices. The herbicides were ultrasonically extracted from peanut using ethyl acetate as extraction solvent. The separation of the analytes from a large amount of co-extractive fat was achieved by dispersive solid-phase extraction using MIL-101(Cr) as sorbent. In this step, the analytes were adsorbed on MIL-101(Cr) and the fat remained in bulk. The herbicides were separated and determined by high-performance liquid chromatography. The experimental parameters, including type and volume of extraction solvent, ultrasonication time, volume of hexane and eluting solvent, amount of MIL-101(Cr) and dispersive solid phase extraction time, were optimized. The limits of detection for herbicides range from 0.98 to 1.9 μg/kg. The recoveries of the herbicides are in the range of 89.5-102.7% and relative standard deviations are equal or lower than 7.0%. The proposed method is simple, effective and suitable for treatment of the samples containing high content of fat. Copyright © 2014 Elsevier B.V. All rights reserved.

Ultrasound assisted, thermally activated persulfate oxidation of coal tar DNAPLs.

Science.gov (United States)

Peng, Libin; Wang, Li; Hu, Xingting; Wu, Peihui; Wang, Xueqing; Huang, Chumei; Wang, Xiangyang; Deng, Dayi

2016-11-15

The feasibility of ultrasound assisted, thermally activated persulfate for effective oxidation of twenty 2-6 ringed coal tar PAHs in a biphasic tar/water system and a triphasic tar/soil/water system were investigated and established. The results indicate that ultrasonic assistance, persulfate and elevated reaction temperature are all required to achieve effective oxidation of coal tar PAHs, while the heating needed can be provided by ultrasonic induced heating as well. Further kinetic analysis reveals that the oxidation of individual PAH in the biphasic tar/water system follows the first-order kinetics, and individual PAH oxidation rate is primary determined by the mass transfer coefficients, tar/water interfacial areas, the aqueous solubility of individual PAH and its concentration in coal tar. Based on the kinetic analysis and experimental results, the contributions of ultrasound, persulfate and elevated reaction temperature to PAHs oxidation were characterized, and the effects of ultrasonic intensity and oxidant dosage on PAHs oxidation efficiency were investigated. In addition, the results indicate that individual PAH degradability is closely related to its reactivity as well, and the high reactivity of 4-6 ringed PAHs substantially improves their degradability. Copyright © 2016 Elsevier B.V. All rights reserved.

Ultrasound-Assisted Oxidative Desulfurization of Diesel

OpenAIRE

Niran K. Ibrahim; Walla A. Noori; Jaffar M. Khasbag

2016-01-01

Due to the dramatic environmental impact of sulfur emissions associated with the exhaust of diesel engines, last environmental regulations for ultra-low-sulfur diesel require a very deep desulfurization (up to 15 ppm), which cannot be met by the conventional hydrodesulfurization units alone. The proposed method involves a batch ultrasound-assisted oxidative desulfurization (UAODS) of a previously hydrotreated diesel (containing 480 ppm sulfur) so as to convert the residual sulfur-bearing comp...

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

Science.gov (United States)

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

2018-01-01

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

Recovery of anthocyanins from residues of Rubus fruticosus, Vaccinium myrtillus and Eugenia brasiliensis by ultrasound assisted extraction, pressurized liquid extraction and their combination.

Science.gov (United States)

Machado, Ana Paula Da Fonseca; Pereira, Ana Luiza Duarte; Barbero, Gerardo Fernández; Martínez, Julian

2017-09-15

This work investigated the extraction efficiency of polyphenols (anthocyanins) from blackberry, blueberry and grumixama residues using combined ultrasonic assisted extraction (UAE) and pressurized liquid extraction (PLE) (UAE+PLE). The performance of UAE+PLE was compared to those achieved by the isolated PLE and UAE methods and conventional Soxhlet extraction. The effects of the extraction methods and solvents (acidified water pH 2.0, ethanol+water 50% v/v and ethanol+water 70% ethanol v/v) on total phenolics content, anthocyanin composition and antioxidant capacity of extracts were investigated by a full factorial design. The extraction efficiency for total phenolics and antioxidant capacity in decreasing order was: UAE+PLE>PLE≈Soxhlet>UAE, and for anthocyanins it was: Soxhlet≈UAE>UAE+PLE>PLE, using hydroethanolic mixtures as solvents. Extractions with acidified water and ultrasound were not effective to recover phenolics. Two, four and fourteen anthocyanins were identified in the extracts from grumixama, blackberry and blueberry, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

Ultrasound assisted co-precipitation of nanostructured CuO-ZnO-Al2O3 over HZSM-5: effect of precursor and irradiation power on nanocatalyst properties and catalytic performance for direct syngas to DME.

Science.gov (United States)

Allahyari, Somaiyeh; Haghighi, Mohammad; Ebadi, Amanollah; Hosseinzadeh, Shahin

2014-03-01

Nanostructured CuO-ZnO-Al2O3/HZSM-5 was synthesized from nitrate and acetate precursors using ultrasound assisted co-precipitation method under different irradiation powers. The CuO-ZnO-Al2O3/HZSM-5 nanocatalysts were characterized using XRD, FESEM, BET, FTIR and EDX Dot-mapping analyses. The results indicated precursor type and irradiation power have significant influences on phase structure, morphology, surface area and functional groups. It was observed that the acetate formulated CuO-ZnO-Al2O3/HZSM-5 nanocatalyst have smaller CuO crystals with better dispersion and stronger interaction between components in comparison to nitrate based nanocatalysts. Ultrasound assisted co-precipitation synthesis method resulted in nanocatalyst with more uniform morphology compared to conventional method and increasing irradiation power yields smaller particles with better dispersion and higher surface area. Additionally the crystallinity of CuO is lower at high irradiation powers leading to stronger interaction between metal oxides. The nanocatalysts performance were tested at 200-300 °C, 10-40 bar and space velocity of 18,000-36,000 cm(3)/g h with the inlet gas composition of H2/CO = 2/1 in a stainless steel autoclave reactor. The acetate based nanocatalysts irradiated with higher levels of power exhibited better reactivity in terms of CO conversion and DME yield. While there is an optimal temperature for CO conversion and DME yield in direct synthesis of DME, CO conversion and DME yield both increase with the pressure increase. Furthermore ultrasound assisted co-precipitation method yields more stable CuO-ZnO-Al2O3/HZSM-5 nanocatalyst while conventional precipitated nanocatalyst lost their activity ca. 18% and 58% in terms of CO conversion and DME yield respectively in 24 h time on stream test.

Organic solvent-free air-assisted liquid-liquid microextraction for optimized extraction of illegal azo-based dyes and their main metabolite from spices, cosmetics and human bio-fluid samples in one step.

Science.gov (United States)

Barfi, Behruz; Asghari, Alireza; Rajabi, Maryam; Sabzalian, Sedigheh

2015-08-15

Air-assisted liquid-liquid microextraction (AALLME) has unique capabilities to develop as an organic solvent-free and one-step microextraction method, applying ionic-liquids as extraction solvent and avoiding centrifugation step. Herein, a novel and simple eco-friendly method, termed one-step air-assisted liquid-liquid microextraction (OS-AALLME), was developed to extract some illegal azo-based dyes (including Sudan I to IV, and Orange G) from food and cosmetic products. A series of experiments were investigated to achieve the most favorable conditions (including extraction solvent: 77μL of 1-Hexyl-3-methylimidazolium hexafluorophosphate; sample pH 6.3, without salt addition; and extraction cycles: 25 during 100s of sonication) using a central composite design strategy. Under these conditions, limits of detection, linear dynamic ranges, enrichment factors and consumptive indices were in the range of 3.9-84.8ngmL(-1), 0.013-3.1μgmL(-1), 33-39, and 0.13-0.15, respectively. The results showed that -as well as its simplicity, fastness, and use of no hazardous disperser and extraction solvents- OS-AALLME is an enough sensitive and efficient method for the extraction of these dyes from complex matrices. After optimization and validation, OS-AALLME was applied to estimate the concentration of 1-amino-2-naphthol in human bio-fluids as a main reductive metabolite of selected dyes. Levels of 1-amino-2-naphthol in plasma and urinary excretion suggested that this compound may be used as a new potential biomarker of these dyes in human body. Copyright © 2015 Elsevier B.V. All rights reserved.

Heterocyclic aramid nanoparticle-assisted graphene exfoliation for fabrication of pristine graphene-based composite paper

Energy Technology Data Exchange (ETDEWEB)

Mo, Yao; Liu, Qi; Fan, Jinchen, E-mail: Jinchen.fan@shiep.edu.cn; Shi, Penghui; Min, Yulin, E-mail: ahaqmylin@126.com; Xu, Qunjie [Shanghai University of Electric Power, Shanghai Key Laboratory of Materials Protection and Advanced Materials in Electric Power, College of Environmental and Chemical Engineering (China)

2015-07-15

Mechanically strong, electrically conductive, and flexible pristine graphene-based composite paper was prepared based on heterocyclic aramid nanoparticle-assisted liquid-phase exfoliation of graphite. The macroscopic heterocyclic aramid yarns were split and assembled into heterocyclic aramid nanoparticles with the size of ∼30 nm by deprotonation in dimethylsulfoxide in the presence of potassium hydroxide. The obtained heterocyclic aramid nanoparticles dimethylsulfoxide dispersion was used as good medium solvent for highly efficiency liquid-phase exfoliation of graphite. The results demonstrated that the concentration of exfoliated graphene can facile reaches ∼2.72 mg/mL after direct sonication of 7 h with assist of heterocyclic aramid nanoparticles. After exfoliation, the self-assembled pristine graphene-based composite paper was fabricated by vacuum-assisted filtration. Due to the introduction of heterocyclic aramid nanoparticles, the self-assembled pristine graphene/heterocyclic aramid nanoparticles composite paper exhibited good mechanical property with tensile strength of ∼129.7 MPa, meantime, has a high electrical conductivity of ∼1.42 × 10{sup 4} S/m.

Heterocyclic aramid nanoparticle-assisted graphene exfoliation for fabrication of pristine graphene-based composite paper

International Nuclear Information System (INIS)

Mo, Yao; Liu, Qi; Fan, Jinchen; Shi, Penghui; Min, Yulin; Xu, Qunjie

2015-01-01

Mechanically strong, electrically conductive, and flexible pristine graphene-based composite paper was prepared based on heterocyclic aramid nanoparticle-assisted liquid-phase exfoliation of graphite. The macroscopic heterocyclic aramid yarns were split and assembled into heterocyclic aramid nanoparticles with the size of ∼30 nm by deprotonation in dimethylsulfoxide in the presence of potassium hydroxide. The obtained heterocyclic aramid nanoparticles dimethylsulfoxide dispersion was used as good medium solvent for highly efficiency liquid-phase exfoliation of graphite. The results demonstrated that the concentration of exfoliated graphene can facile reaches ∼2.72 mg/mL after direct sonication of 7 h with assist of heterocyclic aramid nanoparticles. After exfoliation, the self-assembled pristine graphene-based composite paper was fabricated by vacuum-assisted filtration. Due to the introduction of heterocyclic aramid nanoparticles, the self-assembled pristine graphene/heterocyclic aramid nanoparticles composite paper exhibited good mechanical property with tensile strength of ∼129.7 MPa, meantime, has a high electrical conductivity of ∼1.42 × 10 4  S/m.

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

Science.gov (United States)

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

2018-01-01

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

Maghemite nanoparticle-decorated hollow fiber electromembrane extraction combined with dispersive liquid-liquid microextraction for the determination of thymol from Carum copticum

DEFF Research Database (Denmark)

Khajeh, Mostafa; Pedersen-Bjergaard, Stig; Bohlooli, Mousa

2017-01-01

BACKGROUND A novel technique using maghemite nanoparticle-decorated hollow fibers to assist electromembrane extraction is proposed. Electromembrane extraction combined with dispersive liquid–liquid microextraction (EME-DLLME) was applied for the extraction of thymol from Carum copticum, followed...... by gas chromatography with flame ionization detection (GC-FID). RESULTS The use of maghemite nanoparticle-decorated hollow fibers was found to improve the extraction efficiency of thymol significantly. Important operational parameters, including pH of acceptor phase, extraction time, voltage...

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

Science.gov (United States)

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

2014-01-01

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

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

Rapid pretreatment and determination of bisphenol A in water samples based on vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection.

Science.gov (United States)

Yang, Xiao; Diao, Chun-Peng; Sun, Ai-Ling; Liu, Ren-Min

2014-10-01

A method for the rapid pretreatment and determination of bisphenol A in water samples based on vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection was proposed in this paper. A simple apparatus consisting of a test tube and a cut-glass dropper was designed and applied to collect the floating extraction drop in liquid-liquid microextraction when low-density organic solvent was used as the extraction solvent. Solidification and melting steps that were tedious but necessary once the low-density organic solvent used as extraction solvent could be avoided by using this apparatus. Bisphenol A was selected as model pollutant and vortex-assisted liquid-liquid microextraction was employed to investigate the usefulness of the apparatus. High-performance liquid chromatography with fluorescence detection was selected as the analytical tool for the detection of bisphenol A. The linear dynamic range was from 0.10 to 100 μg/L for bisphenol A, with good squared regression coefficient (r(2) = 0.9990). The relative standard deviation (n = 7) was 4.7% and the limit of detection was 0.02 μg/L. The proposed method had been applied to the determination of bisphenol A in natural water samples and was shown to be economical, fast, and convenient. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Morphological studies of polymer dispersed liquid crystal materials

International Nuclear Information System (INIS)

Han, Jin-Woo

2006-01-01

In this work, we have studied the morphologies of polymer dispersed liquid crystals (PDLCs) based on E7/NOA61. Scanning electron microscope studies show that the PDLC morphology is strongly affected by the LC concentration and the cure temperature. A typical PDLC morphology with isolated LC droplets dispersed in a polymer matrix is only observed at low LC compositions and at low cure temperatures. Increasing either the LC composition or the cure temperature results in a polymer ball morphology, in which LCs exist in irregularly shaped voids in the polymer network structure. It is shown that the transition between these two morphologies can be qualitatively explained using a pseudo-binary phase diagram.

Microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid for the determination of sulfonamides in environmental water samples.

Science.gov (United States)

Song, Ying; Wu, Lijie; Lu, Chunmei; Li, Na; Hu, Mingzhu; Wang, Ziming

2014-12-01

An easy, quick, and green method, microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid, was first developed and applied to the extraction of sulfonamides in environmental water samples. 1-Ethy-3-methylimidazolium hexafluorophosphate, which is a solid-state ionic liquid at room temperature, was used as extraction solvent in the present method. After microwave irradiation for 90 s, the solid-state ionic liquid was melted into liquid phase and used to finish the extraction of the analytes. The ionic liquid and sample matrix can be separated by freezing and centrifuging. Several experimental parameters, including amount of extraction solvent, microwave power and irradiation time, pH of sample solution, and ionic strength, were investigated and optimized. Under the optimum experimental conditions, good linearity was observed in the range of 2.00-400.00 μg/L with the correlation coefficients ranging from 0.9995 to 0.9999. The limits of detection for sulfathiazole, sulfachlorpyridazine, sulfamethoxazole, and sulfaphenazole were 0.39, 0.33, 0.62, and 0.85 μg/L, respectively. When the present method was applied to the analysis of environmental water samples, the recoveries of the analytes ranged from 75.09 to 115.78% and relative standard deviations were lower than 11.89%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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

Science.gov (United States)

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

2016-01-01

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

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

Science.gov (United States)

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

2014-07-01

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

Ultrasound-assisted sol-gel synthesis of ZrO2.

Science.gov (United States)

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

2017-03-01

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

Long-range dipolar order and dispersion forces in polar liquids

Science.gov (United States)

Besford, Quinn Alexander; Christofferson, Andrew Joseph; Liu, Maoyuan; Yarovsky, Irene

2017-11-01

Complex solvation phenomena, such as specific ion effects, occur in polar liquids. Interpretation of these effects in terms of structure and dispersion forces will lead to a greater understanding of solvation. Herein, using molecular dynamics, we probe the structure of polar liquids through specific dipolar pair correlation functions that contribute to the potential of mean force that is "felt" between thermally rotating dipole moments. It is shown that unique dipolar order exists at separations at least up to 20 Å for all liquids studied. When the structural order is compared with a dipolar dispersion force that arises from local co-operative enhancement of dipole moments, a strong agreement is found. Lifshitz theory of dispersion forces was compared with the structural order, where the theory is validated for all liquids that do not have significant local dipole correlations. For liquids that do have significant local dipole correlations, specifically liquid water, Lifshitz theory underestimates the dispersion force by a factor of 5-10, demonstrating that the force that leads to the increased structure in liquid water is missed by Lifshitz theory of van der Waals forces. We apply similar correlation functions to an ionic aqueous system, where long-range order between water's dipole moment and a single chloride ion is found to exist at 20 Å of separation, revealing a long-range perturbation of water's structure by an ion. Furthermore, we found that waters within the 1st, 2nd, and 3rd solvation shells of a chloride ion exhibit significantly enhanced dipolar interactions, particularly with waters at larger distances of separation. Our results provide a link between structures, dispersion forces, and specific ion effects, which may lead to a more robust understanding of solvation.

Separation/preconcentration and determination of vanadium with dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) and electrothermal atomic absorption spectrometry.

Science.gov (United States)

Asadollahi, Tahereh; Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji

2010-06-30

A novel dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) for separation/preconcentration of ultra trace amount of vanadium and its determination with the electrothermal atomic absorption spectrometry (ETAAS) was developed. The DLLME-SFO behavior of vanadium (V) using N-benzoyl-N-phenylhydroxylamine (BPHA) as complexing agent was systematically investigated. The factors influencing the complex formation and extraction by DLLME-SFO method were optimized. Under the optimized conditions: 100 microL, 200 microL and 25 mL of extraction solvent (1-undecanol), disperser solvent (acetone) and sample volume, respectively, an enrichment factor of 184, a detection limit (based on 3S(b)/m) of 7 ng L(-1) and a relative standard deviation of 4.6% (at 500 ng L(-1)) were obtained. The calibration graph using the preconcentration system for vanadium was linear from 20 to 1000 ng L(-1) with a correlation coefficient of 0.9996. The method was successfully applied for the determination of vanadium in water and parsley. Copyright 2010 Elsevier B.V. All rights reserved.

MLESAC Based Localization of Needle Insertion Using 2D Ultrasound Images

Science.gov (United States)

Xu, Fei; Gao, Dedong; Wang, Shan; Zhanwen, A.

2018-04-01

In the 2D ultrasound image of ultrasound-guided percutaneous needle insertions, it is difficult to determine the positions of needle axis and tip because of the existence of artifacts and other noises. In this work the speckle is regarded as the noise of an ultrasound image, and a novel algorithm is presented to detect the needle in a 2D ultrasound image. Firstly, the wavelet soft thresholding technique based on BayesShrink rule is used to denoise the speckle of ultrasound image. Secondly, we add Otsu’s thresholding method and morphologic operations to pre-process the ultrasound image. Finally, the localization of the needle is identified and positioned in the 2D ultrasound image based on the maximum likelihood estimation sample consensus (MLESAC) algorithm. The experimental results show that it is valid for estimating the position of needle axis and tip in the ultrasound images with the proposed algorithm. The research work is hopeful to be used in the path planning and robot-assisted needle insertion procedures.

Ionic liquid-based microwave-assisted extraction of flavonoids from Bauhinia championii (Benth.) Benth.

Science.gov (United States)

Xu, Wei; Chu, Kedan; Li, Huang; Zhang, Yuqin; Zheng, Haiyin; Chen, Ruilan; Chen, Lidian

2012-12-03

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.

Ultrasound-assisted extraction for total sulphur measurement in mine tailings.

Science.gov (United States)

Khan, Adnan Hossain; Shang, Julie Q; Alam, Raquibul

2012-10-15

A sample preparation method for percentage recovery of total sulphur (%S) in reactive mine tailings based on ultrasound-assisted digestion (USAD) and inductively coupled plasma-optical emission spectroscopy (ICP-OES) was developed. The influence of various methodological factors was screened by employing a two-level and three-factor (2(3)) full factorial design and using KZK-1, a sericite schist certified reference material (CRM), to find the optimal combination of studied factors and %S. Factors such as the sonication time, temperature and acid combination were studied, with the best result identified as 20 min of sonication, 80°C temperature and 1 ml of HNO(3):1 ml of HCl, which can achieve 100% recovery for the selected CRM. Subsequently a fraction of the 2(3) full factorial design was applied to mine tailings. The percentage relative standard deviation (%RSD) for the ultrasound method is less than 3.0% for CRM and less than 6% for the mine tailings. The investigated method was verified by X-ray diffraction analysis. The USAD method compared favorably with existing methods such as hot plate assisted digestion method, X-ray fluorescence and LECO™-CNS method. Copyright © 2012 Elsevier B.V. All rights reserved.

Control of liquid crystal molecular orientation using ultrasound vibration

Energy Technology Data Exchange (ETDEWEB)

Taniguchi, Satoki [Faculty of Life and Medical Sciences, Doshisha University, 1-3 Tataramiyakodani, Kyotanabe, Kyoto 610-0321 (Japan); Wave Electronics Research Center, Doshisha University, 1-3 Tataramiyakodani, Kyotanabe, Kyoto 610-0321 (Japan); Koyama, Daisuke; Matsukawa, Mami [Wave Electronics Research Center, Doshisha University, 1-3 Tataramiyakodani, Kyotanabe, Kyoto 610-0321 (Japan); Faculty of Science and Engineering, Doshisha University, 1-3 Tataramiyakodani, Kyotanabe, Kyoto 610-0321 (Japan); Shimizu, Yuki; Emoto, Akira [Faculty of Science and Engineering, Doshisha University, 1-3 Tataramiyakodani, Kyotanabe, Kyoto 610-0321 (Japan); Nakamura, Kentaro [Precision and Intelligence Laboratory, Tokyo Institute of Technology, 4259-R2-26, Nagatsuta-cho, Midori-ku, Yokohama 226-8503 (Japan)

2016-03-07

We propose a technique to control the orientation of nematic liquid crystals using ultrasound and investigate the optical characteristics of the oriented samples. An ultrasonic liquid crystal cell with a thickness of 5–25 μm and two ultrasonic lead zirconate titanate transducers was fabricated. By exciting the ultrasonic transducers, the flexural vibration modes were generated on the cell. An acoustic radiation force to the liquid crystal layer was generated, changing the molecular orientation and thus the light transmission. By modulating the ultrasonic driving frequency and voltage, the spatial distribution of the molecular orientation of the liquid crystals could be controlled. The distribution of the transmitted light intensity depends on the thickness of the liquid crystal layer because the acoustic field in the liquid crystal layer is changed by the orientational film.

Modified dispersive liquid-liquid microextraction for pre-concentration of benzene, toluene, ethylbenzene and xylenes prior to their determination by GC

International Nuclear Information System (INIS)

Faraji, Hakim; Feizbakhsh, Alireza; Helalizadeh, Masoumeh

2013-01-01

We have developed a modified method for the extraction and preconcentration of benzene, toluene, ethylbenzene and xylenes (BTEX) in aqueous samples. It based on dispersive liquid-liquid microextraction along with solidification of floating organic microdrops. The dispersion of microvolumes of an extracting solvent into the aqueous occurs without dispersive solvent. Various parameters have been optimized. BTEX were quantified via GC with FID detection. Under optimized conditions, the preconcentration factors range from 301 to 514, extraction efficiencies from 60 to 103 %, repeatabilities from 2.2 to 4.1 %, and intermediate precisions from 3.5 to 7.0 %. The relative recovery for each analyte in water samples at three spiking levels is >85.6 %, with a relative standard deviation of <7.4 %. (author)

Dispersion relations of the acoustic modes in divalent liquid metals

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Inui Masanori

2017-01-01

Full Text Available Collective dynamics in liquid Ca and liquid Cd was studied by inelastic x-ray scattering (IXS. Using our experimental technique to prepare proper sample cells and high performance of an IXS beamline (BL35XU at SPring-8 in Japan, the dynamic structure factor with reasonable statistics was obtained for these divalent liquid metals. For both liquids, the dynamic structure factor at low Q exhibits a central peak with a shoulder or small hump clearly visible on each side, and the inelastic excitation energy determined using the model function composed of Lorentzian and the damped harmonic oscillator function disperses with increasing Q. The dispersion curves of these liquids were compared with that of the longitudinal acoustic phonon in each crystalline phase. From these results, clear difference in the interatomic interaction be- tween liquid Ca and liquid Cd was inferred.

Rapid determination of hydrophilic phenols in olive oil by vortex-assisted reversed-phase dispersive liquid-liquid microextraction and screen-printed carbon electrodes.

Science.gov (United States)

Fernández, Elena; Vidal, Lorena; Canals, Antonio

2018-05-01

A novel approach is presented to determine hydrophilic phenols in olive oil samples, employing vortex-assisted reversed-phase dispersive liquid-liquid microextraction (RP-DLLME) for sample preparation and screen-printed carbon electrodes for voltammetric analysis. The oxidation of oleuropein, hydroxytyrosol, caffeic acid, ferulic acid and tyrosol was investigated, being caffeic acid and tyrosol selected for quantification. A matrix-matching calibration using sunflower oil as analyte-free sample diluted with hexane was employed to compensate matrix effects. Samples were analyzed under optimized RP-DLLME conditions, i.e., extractant phase, 1M HCl; extractant volume, 100µL; extraction time, 2min; centrifugation time, 10min; centrifugation speed, 4000rpm. The working range showed a good linearity between 0.075 and 2.5mgL -1 (r = 0.998, N = 7) for caffeic acid, and between 0.075 and 3mgL -1 (r = 0.999, N = 8) for tyrosol. The methodological limit of detection was empirically established at 0.022mgL -1 for both analytes, which is significantly lower than average contents found in olive oil samples. The repeatability was evaluated at two different spiking levels (i.e., 0.5mgL -1 and 2mgL -1 ) and coefficients of variation ranged from 8% to 11% (n = 5). The applicability of the proposed method was tested in olive oil samples of different quality (i.e., refined olive oil, virgin olive oil and extra virgin olive oil). Relative recoveries varied between 83% and 108% showing negligible matrix effects. Finally, fifteen samples were analyzed by the proposed method and a high correlation with the traditional Folin-Ciocalteu spectrophotometric method was obtained. Thereafter, the concentrations of the fifteen oil samples were employed as input variables in linear discriminant analysis in order to distinguish between olive oils of different quality. Copyright © 2017 Elsevier B.V. All rights reserved.

Binary Solvents Dispersive Liquid-Liquid Microextraction (BS-DLLME) Method for Determination of Tramadol in Urine Using High-Performance Liquid Chromatography.

Science.gov (United States)

Kiarostami, Vahid; Rouini, Mohamad-Reza; Mohammadian, Razieh; Lavasani, Hoda; Ghazaghi, Mehri

2014-02-03

Tramadol is an opioid, synthetic analog of codeine and has been used for the treatment of acute or chronic pain may be abused. In this work, a developed Dispersive liquid liquid microextraction (DLLME) as binary solvents-based dispersive liquid-liquid microextraction (BS-DLLME) combined with high performance liquid chromatography (HPLC) with fluorescence detection (FD) was employed for determination of tramadol in the urine samples. This procedure involves the use of an appropriate mixture of binary extraction solvents (70 μL CHCl3 and 30 μL ethyl acetate) and disperser solvent (600 μL acetone) for the formation of cloudy solution in 5 ml urine sample comprising tramadol and NaCl (7.5%, w/v). After centrifuging, the small droplets of extraction solvents were precipitated. In the final step, the HPLC with fluorescence detection was used for determination of tramadol in the precipitated phase. Various factors on the efficiency of the proposed procedure were investigated and optimized. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively. The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6). The relative recoveries of tramadol from urine samples at spiking levels of 10, 30 and 60 μg/L were in the range of 95.6 - 99.6%. Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories.

Entrapment of curcumin into monoolein-based liquid crystalline nanoparticle dispersion for enhancement of stability and anticancer activity

Directory of Open Access Journals (Sweden)

Baskaran R

2014-06-01

Full Text Available Rengarajan Baskaran,1 Thiagarajan Madheswaran,2 Pasupathi Sundaramoorthy,1 Hwan Mook Kim,1 Bong Kyu Yoo1 1College of Pharmacy, Gachon University, Incheon, South Korea; 2College of Pharmacy Yeungnam University, Gyeongsan, South Korea Abstract: Despite the promising anticancer potential of curcumin, its therapeutic application has been limited, owing to its poor solubility, bioavailability, and chemical fragility. Therefore, various formulation approaches have been attempted to address these problems. In this study, we entrapped curcumin into monoolein (MO-based liquid crystalline nanoparticles (LCNs and evaluated the physicochemical properties and anticancer activity of the LCN dispersion. The results revealed that particles in the curcumin-loaded LCN dispersion were discrete and monodispersed, and that the entrapment efficiency was almost 100%. The stability of curcumin in the dispersion was surprisingly enhanced (about 75% of the curcumin survived after 45 days of storage at 40°C, and the in vitro release of curcumin was sustained (10% or less over 15 days. Fluorescence-activated cell sorting (FACS analysis using a human colon cancer cell line (HCT116 exhibited 99.1% fluorescence gating for 5 µM curcumin-loaded LCN dispersion compared to 1.36% for the same concentration of the drug in dimethyl sulfoxide (DMSO, indicating markedly enhanced cellular uptake. Consistent with the enhanced cellular uptake of curcumin-loaded LCNs, anticancer activity and cell cycle studies demonstrated apoptosis induction when the cells were treated with the LCN dispersion; however, there was neither noticeable cell death nor significant changes in the cell cycle for the same concentration of the drug in DMSO. In conclusion, entrapping curcumin into MO-based LCNs may provide, in the future, a strategy for overcoming the hurdles associated with both the stability and cellular uptake issues of the drug in the treatment of various cancers. Keywords: liquid

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

International Nuclear Information System (INIS)

Rodriguez Chanfrau, Jorge Enrique; Lopez Armas, Marilyn

2014-01-01

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

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

Science.gov (United States)

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

2015-05-01

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

Ligandless-dispersive liquid-liquid microextraction of trace amount of copper ions

International Nuclear Information System (INIS)

Mohammadi, Sayed Zia; Afzali, Daryoush; Baghelani, Yar Mohammad

2009-01-01

In the present work, a new ligandless-dispersive liquid-liquid microextraction (LL-DLLME) method has been developed for preconcentration trace amounts of copper as a prior step to its determination by flame atomic absorption spectrometry. In the proposed approach 1,2-dicholorobenzene and ethanol were used as extraction and dispersive solvents, respectively. Some factors influencing on the extraction efficiency of copper and its subsequent determination were studied and optimized, such as the extraction and dispersive solvent type and volume, pH of sample solution, extraction time and salting out effect. Under the optimal conditions, the calibration curve was linear in the range of 1.0 ng mL -1 -0.6 μg mL -1 of copper with R 2 = 0.9985. Detection limit was 0.5 ng mL -1 in original solution (3S b /m) and the relative standard deviation for seven replicate determination of 0.2 μg mL -1 copper was ±1.4%. The proposed method has been applied for determination of copper in standard and water samples with satisfactory results.

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

Science.gov (United States)

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

2014-11-26

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

Simultaneous multi-mycotoxin determination in nutmeg by ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection.

Science.gov (United States)

Kong, Wei-Jun; Liu, Shu-Yu; Qiu, Feng; Xiao, Xiao-He; Yang, Mei-Hua

2013-05-07

A simple and sensitive analytical method based on ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with high performance liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection (USLE-IAC-HPLC-PCD-FLD) has been developed for simultaneous multi-mycotoxin determination of aflatoxins B1, B2, G1, G2 (AFB1, AFB2, AFG1, AFG2) and ochratoxin A (OTA) in 13 edible and medicinal nutmeg samples marketed in China. AFs and OTA were extracted from nutmeg samples by ultrasonication using a methanol : water (80 : 20, v/v) solution, followed by an IAC clean-up step. Different USL extraction conditions, pre-processing ways for nutmeg sample and clean-up columns for mycotoxins, as well as HPLC-PCD-FLD parameters (mobile phase, column temperature, elution procedure, excitation and emission wavelengths) were optimized. This method, which was appraised for analyzing nutmeg samples, showed satisfactory results with reference to limits of detection (LODs) (from 0.02 to 0.25 μg kg(-1)), limits of quantification (LOQs) (from 0.06 to 0.8 μg kg(-1)), linear ranges (up to 30 ng mL(-1) for AFB1, AFG1 and OTA and 9 ng mL(-1) for AFB2 and AFG2), intra- and inter-day variability (all application of developed method in nutmeg samples have elucidated that four samples were detected with contamination of AFs and one with OTA. AFB1 was the most frequently found mycotoxin in 30.8% of nutmeg samples at contamination levels of 0.73-16.31 μg kg(-1). At least two different mycotoxins were co-occurred in three samples, and three AFs were simultaneously detected in one sample.

Ultrasonic absorption and velocity dispersion of binary mixture liquid crystal MBBA/EBBA

International Nuclear Information System (INIS)

Choi, K.

1979-01-01

The effect of phase transitions and the partial magnetic alignment for liquid crystal molecules on the ultrasonic absorption and velocity dispersion has been investigated. The binary mixture of Shiff base liquid crystals MBBA/EBBA (55:45 mole %) showed anomalous ultrasonic absorption and velocity dispersion at eutectic (Tsub(m) = -20 0 C) and clearing point (Tsub(c) = 50 0 C) at the frequency range of 5 MHz, 10MHz, 15MHz and 30 MHz. The experimental data were analyzed in terms of relaxation time and Fixman theory. The anisotropy of the propagation velocity due to the magnetic alignment was about 0.9% (the deviation between velocities propagating parallel and perpendicular to the applied field). (author)

2-Naphthalenthiol derivatization followed by dispersive liquid-liquid microextraction as an efficient and sensitive method for determination of acrylamide in bread and biscuit samples using high-performance liquid chromatography.

Science.gov (United States)

Faraji, Mohammad; Hamdamali, Mohammadrezza; Aryanasab, Fezzeh; Shabanian, Meisam

2018-07-13

In this research, an ultrasonic-assisted extraction followed by 2-naphthalenthiol derivatization and dispersive liquid-liquid microextraction of acrylamide (AA) was developed as simple and sensitive sample preparation method for AA in bread and biscuit samples using high performance liquid chromatography. Influence of derivatization and microextraction parameters were evaluated and optimized. Results showed that the derivatization of AA leads to improve its hydrophobicity and chromatographic behavior. Under optimum conditions of derivatization and microextraction, the method yielded a linear calibration curve ranging from 10 to 1000 μg L -1 with a determination coefficient (R 2 ) of 0.9987. Limit of detection (LOD) and limit of quantification (LOQ) were 3.0 and 9.0 μg L -1 , respectively. Intra-day (n = 6) and inter-day (n = 3) precisions based on relative standard deviation percent (RSD%) for extraction and determination of AA at 50 and 500 μg L -1 levels were less than 9.0%. Finally, the performance of proposed method was investigated for determination of AA in some bread and biscuit samples, and satisfactory results were obtained (relative recovery ≥ 90%). Copyright © 2018. Published by Elsevier B.V.

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

Energy Technology Data Exchange (ETDEWEB)

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

2014-07-01

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

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

International Nuclear Information System (INIS)

Khajeh, Mostafa; Nemch, Tabandeh Karimi

2014-01-01

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

Evolution of Robot-assisted ultrasound-guided breast biopsy systems

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Mustafa Z. Mahmoud

2018-01-01

Full Text Available Robot-assisted ultrasound-guided breast biopsy combines ultrasound (US imaging with a robotic system for medical interventions. This study was designed to provide a literature review of a robotic US-guided breast biopsy system to delineate its efficacious impact on current medical practice. In addition, the strengths and limitations of this approach were also addressed. Articles published in the English language between 2000 and 2016 were appraised in this review. A wide range of systems that bind robotics with US imaging and guided breast biopsy were examined in this article. The fundamental safety and real-time imaging capabilities of US, together with the accuracy and maneuverability of robotic devices, is clearly an effective association with unmatched capabilities. Numerous experimental systems have obvious benefits over old-fashioned techniques, and the future of robot-assisted US-guided breast biopsy will be characterized by increasing levels of automation, and they hold tremendous possibility to impact doctor achievement, patient recovery, and clinical management.

In-syringe magnetic-stirring-assisted liquid-liquid microextraction for the spectrophotometric determination of Cr(VI) in waters.

Science.gov (United States)

Henríquez, Camelia; Horstkotte, Burkhard; Solich, Petr; Cerdà, Víctor

2013-08-01

A fully automated method for the determination of chromate is described. It is based on the selective reaction of Cr(VI) with diphenylcarbazide in acidic media to form a colored complex of Cr(III) with the oxidation product diphenylcarbazone. The reaction was performed within the syringe of an automatic burette containing a magnetic stirrer for homogenization of the sample and the required reagents. In-syringe stirring was made possible using a specially designed driving device placed around the syringe barrel to achieve a rotating magnetic field in the syringe, forcing the stirrer to spin. In a second step, the reaction mixture in the syringe was neutralized to allow in-syringe magnetic-stirring-assisted dispersive liquid-liquid microextraction of the complex into 125 μL of n-hexanol. After phase separation by droplet flotation over 30 s, the organic phase was propelled into a coupled spectrophotometric detection cell. The entire multistep procedure including in-system standard preparation was done within 270 s. The method was used for the analysis of natural waters, achieving average analyte recovery of 103%, a limit of detection of 0.26 μg L(-1), and a repeatability of less than 4% relative standard deviation.

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.

Microbubbles-Assisted Ultrasound Triggers the Release of Extracellular Vesicles

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Yuana Yuana

2017-07-01

Full Text Available Microbubbles-assisted ultrasound (USMB has shown promise in improving local drug delivery. The formation of transient membrane pores and endocytosis are reported to be enhanced by USMB, and they contribute to cellular drug uptake. Exocytosis also seems to be linked to endocytosis upon USMB treatment. Based on this rationale, we investigated whether USMB triggers exocytosis resulting in the release of extracellular vesicles (EVs. USMB was performed on a monolayer of head-and-neck cancer cells (FaDu with clinically approved microbubbles and commonly used ultrasound parameters. At 2, 4, and 24 h, cells and EV-containing conditioned media from USMB and control conditions (untreated cells, cells treated with microbubbles and ultrasound only were harvested. EVs were measured using flow cytometric immuno-magnetic bead capture assay, immunogold electron microscopy, and western blotting. After USMB, levels of CD9 exposing-EVs significantly increased at 2 and 4 h, whereas levels of CD63 exposing-EVs increased at 2 h. At 24 h, EV levels were comparable to control levels. EVs released after USMB displayed a heterogeneous size distribution profile (30–1200 nm. Typical EV markers CD9, CD63, and alix were enriched in EVs released from USMB-treated FaDu cells. In conclusion, USMB treatment triggers exocytosis leading to the release of EVs from FaDu cells.

Analysis of chlorpheniramine in human urine samples using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography

Directory of Open Access Journals (Sweden)

Mehdi Maham

2014-09-01

Full Text Available A simple and environmentally friendly microextraction technique was used for determination of chlorpheniramine (CPM, an antihistamine drug, in human urine samples using dispersive liquid-liquid microextraction (DLLME followed by high performance liquid chromatography with diode array detection (HPLC-DAD. In this extraction technique, an appropriate mixture of acetonitrile (disperser solvent and carbon tetrachloride (extraction solvent was rapidly injected into the urine sample containing the target analyte. Tiny droplets of extractant were formed and dispersed into the sample solution and then sedimented at the bottom of the conical test tube by centrifugation. Under optimal conditions, the calibration curve was linear in the range of 0.055-5.5 µg mL-1, with a detection limit of 16.5 ng mL-1. This proposed method was successfully applied to the analysis of real urine samples. Low consumption of toxic organic solvents, simplicity of operation, low cost and acceptable figures of merit are the main advantages of the proposed technique.

Recent Advances in Discotic Liquid Crystal-Assisted Nanoparticles

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Ashwathanarayana Gowda

2018-03-01

Full Text Available This article primarily summarizes recent advancement in the field of discotic liquid crystal (DLC nanocomposites. Discotic liquid crystals are nanostructured materials, usually 2 to 6 nm size and have been recognized as organic semiconducting materials. Recently, it has been observed that the dispersion of small concentration of various functionalized zero-, one- and two-dimensional nanomaterials in the supramolecular order of mesophases of DLCs imparts negligible impact on liquid crystalline properties but enhances their thermal, supramolecular and electronic properties. Synthesis, characterization and dispersion of various nanoparticles in different discotics are presented.

Ultrasound-Assisted Extraction: Effect of Extraction Time and Solvent ...

African Journals Online (AJOL)

Purpose: To investigate the influence of extraction conditions assisted by ultrasound on the quality of extracts obtained from Mesembryanthemum edule shoots. Methods: The extraction procedure was carried out in an ultrasonic bath. The effect of two solvents (methanol and ethanol) and two extraction times (5 and 10 min) ...

Vortex-assisted liquid-liquid microextraction for the rapid screening of short-chain chlorinated paraffins in water.

Science.gov (United States)

Chang, Chia-Yu; Chung, Wu-Hsun; Ding, Wang-Hsien

2016-01-01

The rapid screening of trace levels of short-chain chlorinated paraffins in various aqueous samples was performed by a simple and reliable procedure based on vortex-assisted liquid-liquid microextraction combined with gas chromatography and electron capture negative ionization mass spectrometry. The optimal vortex-assisted liquid-liquid microextraction conditions for 20 mL water sample were as follows: extractant 400 μL of dichloromethane; vortex extraction time of 1 min at 2500 × g; centrifugation of 3 min at 5000 × g; and no ionic strength adjustment. Under the optimum conditions, the limit of quantitation was 0.05 μg/L. Precision, as indicated by relative standard deviations, was less than 9% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was above 91%. The vortex-assisted liquid-liquid microextraction with gas chromatography and electron capture negative ionization mass spectrometry method was successfully applied to quantitatively extract short-chain chlorinated paraffins from samples of river water and the effluent of a wastewater treatment plant, and the concentrations ranged from 0.8 to 1.6 μg/L. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Recent developments on ultrasound-assisted organic synthesis in aqueous medium

Directory of Open Access Journals (Sweden)

Banerjee Bubun

2017-01-01

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

Liquid-liquid and liquid-solid phase separation and flocculation for a charged colloidal dispersion

International Nuclear Information System (INIS)

Lai, S.K.; Wu, K.L.

2002-01-01

We model the intercolloidal interaction by a hard-sphere Yukawa repulsion to which is added the long-range van der Waals attraction. In comparison with the Derjaguin-Landau-Verwey-Overbeek repulsion, the Yukawa repulsion explicitly incorporates the spatial correlations between colloids and small ions. As a result, the repulsive part can be expressed analytically and has a coupling strength depending on the colloidal volume fraction. By use of this two-body potential of mean force and in conjunction with a second-order thermodynamic perturbation theory, we construct the colloidal Helmholtz free energy and use it to calculate the thermodynamic quantities, pressure and chemical potential, needed in the determination of the liquid-liquid and liquid-solid phase diagrams. We examine, in an aqueous charged colloidal dispersion, the effects of the Hamaker constant and particle size on the conformation of a stable liquid-liquid phase transition calculated with respect to the liquid-solid coexistence phases. We find that there exists a threshold Hamaker constant or particle size whose value demarcates the stable liquid-liquid coexistence phases from their metastable counterparts. Applying the same technique and using the energetic criterion, we extend our calculations to study the flocculation phenomenon in aqueous charged colloids. Here, we pay due attention to determining the loci of a stability curve stipulated for a given temperature T 0 , and obtain the parametric phase diagram of the Hamaker constant vs the coupling strength or, at given surface potential, the particle size. By imposing T 0 to be the critical temperature T c , i.e., setting k B T 0 (=k B T c ) equal to a reasonable potential barrier, we arrive at the stability curve that marks the irreversible reversible phase transition. The interesting result is that there occurs a minimum size for the colloidal particles below (above) which the colloidal dispersion is driven to an irreversible (reversible) phase

Chromatic dispersion of liquid crystal infiltrated capillary tubes and photonic crystal fibers

DEFF Research Database (Denmark)

Rasmussen, Per Dalgaard; Lægsgaard, Jesper; Bang, Ole

2006-01-01

We consider chromatic dispersion of capillary tubes and photonic crystal fibers infiltrated with liquid crystals. A perturbative scheme for inclusion of material dispersion of both liquid crystal and the surrounding waveguide material is derived. The method is used to calculate the chromatic...

Biomolecule-assisted exfoliation and dispersion of graphene and other two-dimensional materials: a review of recent progress and applications.

Science.gov (United States)

Paredes, J I; Villar-Rodil, S

2016-08-25

Direct liquid-phase exfoliation of layered materials by means of ultrasound, shear forces or electrochemical intercalation holds enormous promise as a convenient, cost-effective approach to the mass production of two-dimensional (2D) materials, particularly in the form of colloidal suspensions of high quality and micrometer- and submicrometer-sized flakes. Of special relevance due to environmental and practical reasons is the production of 2D materials in aqueous medium, which generally requires the use of certain additives (surfactants and other types of dispersants) to assist in the exfoliation and colloidal stabilization processes. In this context, biomolecules have received, in recent years, increasing attention as dispersants for 2D materials, as they provide a number of advantages over more conventional, synthetic surfactants. Here, we review research progress in the use of biomolecules as exfoliating and dispersing agents for the production of 2D materials. Although most efforts in this area have focused on graphene, significant advances have also been reported with transition metal dichalcogenides (MoS2, WS2, etc.) or hexagonal boron nitride. Particular emphasis is placed on the specific merits of different types of biomolecules, including proteins and peptides, nucleotides and nucleic acids (RNA, DNA), polysaccharides, plant extracts and bile salts, on their role as efficient colloidal dispersants of 2D materials, as well as on the potential applications that have been explored for such biomolecule-exfoliated materials. These applications are wide-ranging and encompass the fields of biomedicine (photothermal and photodynamic therapy, bioimaging, biosensing, etc.), energy storage (Li- and Na-ion batteries), catalysis (e.g., catalyst supports for the oxygen reduction reaction or electrocatalysts for the hydrogen evolution reaction), or composite materials. As an incipient area of research, a number of knowledge gaps, unresolved issues and novel future

Effects of Ultrasound Assistance on Dehydration Processes and Bioactive Component Retention of Osmo-Dried Sour Cherries.

Science.gov (United States)

Siucińska, Karolina; Mieszczakowska-Frąc, Monika; Połubok, Aleksandra; Konopacka, Dorota

2016-07-01

Despite having numerous health benefits, dried sour cherries have proven to be more acceptable to consumers when infused with sugar or other sweeteners to enhance their flavor, which, in turn, leads to serious anthocyanin losses. For this reason, a consideration was made for the application of ultrasound to accelerate solid gain and shorten drying time, thus favoring bioactive component retention. To determine the usefulness of ultrasound as a tool for sour cherry osmotic infusion enhancement, the effect of sonication time on dehydration effectiveness, as well as the stability of bioactive components during osmotic treatment and consecutive convective drying, was investigated. Fruits were osmo-dehydrated using a 60% sucrose solution for 120 min (40 °C), during which, ultrasound of 25 kHz (0.4 W/cm(2) ), was applied for 0, 30, 60, 90, and 120 min, after which, the fruits were convectively dried. In the range of the applied ultrasound energy no significant effect of sonication on mass transfer intensification was observed; moreover, longer acoustic treatment seemed to retard moisture removal during subsequent convective drying, which can be related to the breakdown of the parenchyma cell walls caused by the prolonged ultrasound (US) action. It was concluded that although US assistance could be considered neutral for bioactive component retention, excessive sonication time can lead to some anthocyanin deterioration. According to high-performance liquid chromatography analysis, the particular anthocyanin alterations, both during dehydration and final drying, occurred in a similar way. Sonication time prolongation caused approximately 10% more bioactive compound deterioration, than earlier, shorter trials. © 2016 Institute of Food Technologists®

An approach of ionic liquids/lithium salts based microwave irradiation pretreatment followed by ultrasound-microwave synergistic extraction for two coumarins preparation from Cortex fraxini.

Science.gov (United States)

Liu, Zaizhi; Gu, Huiyan; Yang, Lei

2015-10-23

Ionic liquids/lithium salts solvent system was successfully introduced into the separation technique for the preparation of two coumarins (aesculin and aesculetin) from Cortex fraxini. Ionic liquids/lithium salts based microwave irradiation pretreatment followed by ultrasound-microwave synergy extraction (ILSMP-UMSE) procedure was developed and optimized for the sufficient extraction of these two analytes. Several variables which can potentially influence the extraction yields, including pretreatment time and temperature, [C4mim]Br concentration, LiAc content, ultrasound-microwave synergy extraction (UMSE) time, liquid-solid ratio, and UMSE power were optimized by Plackett-Burman design. Among seven variables, UMSE time, liquid-solid ratio, and UMSE power were the statistically significant variables and these three factors were further optimized by Box-Behnken design to predict optimal extraction conditions and find out operability ranges with maximum extraction yields. Under optimum operating conditions, ILSMP-UMSE showed higher extraction yields of two target compounds than those obtained by reference extraction solvents. Method validation studies also evidenced that ILSMP-UMSE is credible for the preparation of two coumarins from Cortex fraxini. This study is indicative of the proposed procedure that has huge application prospects for the preparation of natural products from plant materials. Copyright © 2015 Elsevier B.V. All rights reserved.

Ultrasound-responsive gene-activated matrices for osteogenic gene therapy using matrix-assisted sonoporation.

Science.gov (United States)

Nomikou, N; Feichtinger, G A; Saha, S; Nuernberger, S; Heimel, P; Redl, H; McHale, A P

2018-01-01

Gene-activated matrix (GAM)-based therapeutics for tissue regeneration are limited by efficacy, the lack of spatiotemporal control and availability of target cells, all of which impact negatively on their translation to the clinic. Here, an advanced ultrasound-responsive GAM is described containing target cells that facilitates matrix-assisted sonoporation (MAS) to induce osteogenic differentiation. Ultrasound-responsive GAMs consisting of fibrin/collagen hybrid-matrices containing microbubbles, bone morphogenetic protein BMP2/7 coexpression plasmids together with C2C12 cells were treated with ultrasound either in vitro or following parenteral intramuscular implantation in vivo. Using direct measurement for alkaline phosphatase activity, von Kossa staining and immunohistochemical analysis for osteocalcin expression, MAS-stimulated osteogenic differentiation was confirmed in the GAMs in vitro 7 days after treatment with ultrasound. At day 30 post-treatment with ultrasound, ectopic osteogenic differentiation was confirmed in vivo using X-ray microcomputed tomography and histological analysis. Osteogenic differentiation was indicated by the presence of ectopic bone structures in all animals treated with MAS. In addition, bone volumes in this group were statistically greater than those in the control groups. This novel approach of incorporating a MAS capability into GAMs could be exploited to facilitate ex vivo gene transfer with subsequent surgical implantation or alternatively provide a minimally invasive means of stimulating in situ transgene delivery for osteoinductive gene-based therapies. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Ligandless-dispersive liquid-liquid microextraction of trace amount of copper ions

Energy Technology Data Exchange (ETDEWEB)

Mohammadi, Sayed Zia, E-mail: szmohammadi@yahoo.com [Department of Chemistry, Payame Noor University (PNU), Kerman (Iran, Islamic Republic of); Afzali, Daryoush [Environment Department, Institute Research of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Baghelani, Yar Mohammad [Department of Chemistry, Payame Noor University (PNU), Kerman (Iran, Islamic Republic of)

2009-10-27

In the present work, a new ligandless-dispersive liquid-liquid microextraction (LL-DLLME) method has been developed for preconcentration trace amounts of copper as a prior step to its determination by flame atomic absorption spectrometry. In the proposed approach 1,2-dicholorobenzene and ethanol were used as extraction and dispersive solvents, respectively. Some factors influencing on the extraction efficiency of copper and its subsequent determination were studied and optimized, such as the extraction and dispersive solvent type and volume, pH of sample solution, extraction time and salting out effect. Under the optimal conditions, the calibration curve was linear in the range of 1.0 ng mL{sup -1}-0.6 {mu}g mL{sup -1} of copper with R{sup 2} = 0.9985. Detection limit was 0.5 ng mL{sup -1} in original solution (3S{sub b}/m) and the relative standard deviation for seven replicate determination of 0.2 {mu}g mL{sup -1} copper was {+-}1.4%. The proposed method has been applied for determination of copper in standard and water samples with satisfactory results.

Ultra-trace determination of gold nanoparticles in environmental water by surfactant assisted dispersive liquid liquid microextraction coupled with electrothermal vaporization-inductively coupled plasma-mass spectrometry

Science.gov (United States)

Liu, Ying; He, Man; Chen, Beibei; Hu, Bin

2016-08-01

A new method by coupling surfactant assisted dispersive liquid liquid microextraction (SA-DLLME) with electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) was proposed for the analysis of gold nanoparticles (AuNPs) in environmental water samples. Effective separation of AuNPs from ionic gold species was achieved by using sodium thiosulphate as a complexing agent. Various experimental parameters affecting SA-DLLME of AuNPs, such as the organic solvent, organic solvent volume, pH of the sample, the kind of surfactant, surfactant concentration, vortex time, speed of centrifugation, centrifugation time, and different coating as well as sizes of AuNPs were investigated carefully. Furthermore, the interference of coexisting ions, dissolved organic matter (DOM) and other metal nanoparticles (NPs) were studied. Under the optimal conditions, a detection limit of 2.2 ng L- 1 and an enrichment factor of 152-fold was achieved for AuNPs, and the original morphology of the AuNPs could be maintained during the extraction process. The developed method was successfully applied for the analysis of AuNPs in environmental water samples, including tap water, the East Lake water, and the Yangtze River water, with recoveries in the range of 89.6-102%. Compared with the established methods for metal NPs analysis, the proposed method has the merits of simple and fast operation, low detection limit, high selectivity, good tolerance to the sample matrix and no digestion or dilution required. It provides an efficient quantification methodology for monitoring AuNPs' pollution in the environmental water and evaluating its toxicity.

Ultrasound-guided, vacuum-assisted biopsy in evaluation of breast lesions

International Nuclear Information System (INIS)

Luczynska, E.; Kocurek, A.; Dyczek, S.; Skotnicki, P.; Stelmach, A.; Herman, K.

2008-01-01

Aim. Evaluation of the efficacy of ultrasound-guided vacuum-assisted biopsy for the verification of breast lesions. Introduction. Ultrasound breast examination is a noninvasive method of breast imaging. It is adjunct to mammography and physical examination and, in women under 30 years of age, pregnant and lactating, it is the basic examination used for the detection and diagnosing of breast diseases. It allows also to obtain cells or tissue samples with such minimally invasive techniques as fine-needle biopsy, core needle biopsy or vacuum-assisted biopsy. Material and methods. The study group consisted of 138 women, aged from 20 to 76 years, who underwent ultrasound guided vacuum-assisted biopsy between March and December 2006. Because double lesions were diagnosed in 6 patients, this resulted in 144 performed procedures. Each patient underwent ultrasound examination, performed with a 10-12 MHz transducer. Biopsies were guided by a 12 MHz transducer and performed with the Mammotome System using an 11G or an 8G needle, depending upon the size and site of the lesion. Obtained data were compared using the Chi-square test; p values of less than 0.05 were considered indicative of a significant difference. Results. The average size of the biopted lesions was estimated as 11±3,8 mm (range: 4-30 mm). However, lesions described by radiologists as apparently suspicious were not qualified for the vacuum-assisted biopsy, in the tested material 4 lesions appeared to be carcinomas (3 were invasive breast carcinomas and 1 was ductal carcinoma in situ). When compared with other changes, these lesions were most frequently equivocal (3 vs 1 determined as benign, p=0.014). There was no statistically significant difference in echogenicity (3 hypoechoic vs 1 with mixed echogenicity) nor in the shape (1 oval change, 2 lobulated and 1 irregular). Pathological examination revealed 86 cases of fibroadenoma within the tested material. Those lesions were mostly benign (77 vs 9 equivocal

Ultrasound assisted dispersion of different amount of Ni over ZSM-5 used as nanostructured catalyst for hydrogen production via CO2 reforming of methane

International Nuclear Information System (INIS)

Vafaeian, Yaser; Haghighi, Mohammad; Aghamohammadi, Sogand

2013-01-01

Graphical abstract: A series of Ni/ZSM-5 nanocatalysts with different amount of Ni were prepared via ultrasound assisted method and characterized with XRD, FESEM, TEM, BET and FTIR techniques. The research deals with catalyst development for dry reforming of methane with the aim of reaching the most stable catalyst specifically over nano-sized catalysts. About more than 99% of Ni particles size is less than 100 nm for the sample prepared with 8% Ni, which is essential to the relative suppression of the carbon formation on catalysts. Catalyst prepared with 8% Ni content showed superior activity in process expected due to its better catalytic properties. - Highlights: • Using ZSM-5 zeolite in dry reforming of methane. • Employing ultrasound energy in synthesis of Ni/ZSM-5 nanocatalyst. • Enhancement of Ni particles size to meet desired catalyst at lower amount of Ni loading. • Dry reforming of methane over Ni/ZSM-5 nanocatalyst with different Ni-loading. • Superior activity of Ni/ZSM-5 nanocatalyst synthesized with 8% Ni content. - Abstract: Carbon dioxide reforming of methane is an interesting route for synthesis gas production especially over nanostructured catalysts. The present research deals with nanocatalyst development by sonochemical method for dry reforming of methane with the aim of reaching the most efficient nanocatalyst. Effect of Ni metal content, one of the most significant variables, on the properties of the ZSM-5 supported nanocatalysts was taken into account. The Ni/ZSM-5 nanocatalysts were prepared via assisted traditional impregnation method via ultrasound irradiation and characterized with XRD, FESEM, TEM, BET and FTIR techniques. Comparison of XRD patterns implies that the peaks related to NiO become sharper by increasing metal content over the support. In the case of nanocatalysts with lower metal content (3% and 8%), the beneficial influence of ultrasound assisted procedure become more pronounced and the observed reduction in

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.

Rapid determination of 226Ra in drinking water samples using dispersive liquid-liquid microextraction coupled with liquid scintillation counting

International Nuclear Information System (INIS)

Sadi, B.K.; Chunsheng Li; Kramer, G.H.; Johnson, C.L.; Queenie Ko; Lai, E.P.C.

2011-01-01

A new radioanalytical method was developed for rapid determination of 226 Ra in drinking water samples. The method is based on extraction and preconcentration of 226 Ra from a water sample to an organic solvent using a dispersive liquid-liquid microextraction (DLLME) technique followed by radiometric measurement using liquid scintillation counting. In DLLME for 226 Ra, a mixture of an organic extractant (toluene doped with dibenzo-21-crown-7 and 2-theonyltrifluoroacetone) and a disperser solvent (acetonitrile) is rapidly injected into the water sample resulting in the formation of an emulsion. Within the emulsion, 226 Ra reacts with dibenzo-21-crown-7 and 2-theonyltrifluoroacetone and partitions into the fine droplets of toluene. The water/toluene phases were separated by addition of acetonitrile as a de-emulsifier solvent. The toluene phase containing 226 Ra was then measured by liquid scintillation counting. Several parameters were studied to optimize the extraction efficiency of 226 Ra, including water immiscible organic solvent, disperser and de-emulsifier solvent type and their volume, chelating ligands for 226 Ra and their concentrations, inorganic salt additive and its concentration, and equilibrium pH. With the optimized DLLME conditions, the accuracy (expressed as relative bias, B r ) and method repeatability (expressed as relative precision, S B ) were determined by spiking 226 Ra at the maximum acceptable concentration level (0.5 Bq L -1 ) according to the Guidelines for Canadian Drinking Water Quality. Accuracy and repeatability were found to be less than -5% (B r ) and less than 6% (S B ), respectively, for both tap water and bottled natural spring water samples. The minimum detectable activity and sample turnaround time for determination of 226 Ra was 33 mBq L -1 and less than 3 h, respectively. The DLLME technique is selective for extraction of 226 Ra from its decay progenies. (author)

Minimally invasive registration for computer-assisted orthopedic surgery: combining tracked ultrasound and bone surface points via the P-IMLOP algorithm.

Science.gov (United States)

Billings, Seth; Kang, Hyun Jae; Cheng, Alexis; Boctor, Emad; Kazanzides, Peter; Taylor, Russell

2015-06-01

We present a registration method for computer-assisted total hip replacement (THR) surgery, which we demonstrate to improve the state of the art by both reducing the invasiveness of current methods and increasing registration accuracy. A critical element of computer-guided procedures is the determination of the spatial correspondence between the patient and a computational model of patient anatomy. The current method for establishing this correspondence in robot-assisted THR is to register points intraoperatively sampled by a tracked pointer from the exposed proximal femur and, via auxiliary incisions, from the distal femur. In this paper, we demonstrate a noninvasive technique for sampling points on the distal femur using tracked B-mode ultrasound imaging and present a new algorithm for registering these data called Projected Iterative Most-Likely Oriented Point (P-IMLOP). Points and normal orientations of the distal bone surface are segmented from ultrasound images and registered to the patient model along with points sampled from the exposed proximal femur via a tracked pointer. The proposed approach is evaluated using a bone- and tissue-mimicking leg phantom constructed to enable accurate assessment of experimental registration accuracy with respect to a CT-image-based model of the phantom. These experiments demonstrate that localization of the femur shaft is greatly improved by tracked ultrasound. The experiments further demonstrate that, for ultrasound-based data, the P-IMLOP algorithm significantly improves registration accuracy compared to the standard ICP algorithm. Registration via tracked ultrasound and the P-IMLOP algorithm has high potential to reduce the invasiveness and improve the registration accuracy of computer-assisted orthopedic procedures.

Fabrication of Microcapsules for Dye-Doped Polymer-Dispersed Liquid Crystal-Based Smart Windows.

Science.gov (United States)

Kim, Mingyun; Park, Kyun Joo; Seok, Seunghwan; Ok, Jong Min; Jung, Hee-Tae; Choe, Jaehoon; Kim, Do Hyun

2015-08-19

A dye-doped polymer-dispersed liquid crystal (PDLC) is an attractive material for application in smart windows. Smart windows using a PDLC can be operated simply and have a high contrast ratio compared to those of other devices that employed photochromic or thermochromic material. However, in conventional dye-doped PDLC methods, dye contamination can cause problems and has a limited degree of commercialization of electric smart windows. Here, we report on an approach to resolve dye-related problems by encapsulating the dye in monodispersed capsules. By encapsulation, a fabricated dye-doped PDLC had a contrast ratio of >120 at 600 nm. This fabrication method of encapsulating the dye in a core-shell structured microcapsule in a dye-doped PDLC device provides a practical platform for dye-doped PDLC-based smart windows.

Ionic liquid – Assisted emulsion polymerization of aniline in organic medium

Energy Technology Data Exchange (ETDEWEB)

Calheiros, Loan F. [Universidade Federal do Rio de Janeiro, Instituto de Macromoléculas, 21941-598, Rio de Janeiro (Brazil); Soares, Bluma G., E-mail: bluma@metalmat.ufrj.br [Universidade Federal do Rio de Janeiro, PEMM-COPPE, Centro de Tecnologia, 21941-972, Rio de Janeiro (Brazil); Universidade Federal do Rio de Janeiro, Instituto de Macromoléculas, 21941-598, Rio de Janeiro (Brazil); Barra, Guilherme M.O. [Universidade Federal de Santa Catarina, Mechanical Engineering Department, Florianópolis, SC (Brazil); Livi, Sébastien [Université de Lyon, F-69003, Lyon (France); INSA Lyon, F-69621, Villeurbanne (France); CNRS, UMR 5223, Ingénierie des Matériaux Polymères (France)

2016-08-15

Polyaniline doped with dodecylbenzene sulfonic acid (PAni.DBSA) with different conductivities and morphologies was prepared by inverted emulsion polymerization, in toluene using ammonium peroxydisulfate as the oxidizing agent, in the presence of two different imidazolium – based ionic liquids, such as, 1-methyl-3-butyl imidazolium tetrafluorate (bmim.BF{sub 4}) and 1-(11-carboxyundecyl)-3-methylimidazolium bromide (mimC{sub 10}COOH.Br). The influence of ionic liquid on the morphology and particle size of formed PAni.DBSA samples was investigated by field emission - scanning electron microscopy (FEG-SEM) and dynamic light scattering (DLS) measurements. Ultraviolet–visible measurements were also employed to confirm the structure of the conducting polymer. PAni.DBSA samples were also characterized by thermogravimetric analysis, cyclic voltammetry and X-ray photoelectron spectroscopy (XPS). PAni.DBSA samples prepared in the presence of ionic liquids have shown improved dispersability in epoxy resin as indicated by optical micrograph. - Highlights: • Imidazolium-based ionic liquids as soft templates for polyaniline synthesis. • PAni with higher conductivity and different morphologies was achieved in the presence of IL. • Good IL/aniline salt interaction resulted in confinement inside PAni particles. • IL confinement confirmed by TGA and XPS analyses. • Excellent dispersability of PAni. DBSA prepared with ionic liquids, in epoxy matrix.

Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar

2015-08-01

A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L{sup −1} and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L{sup −1} of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic.

Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

2015-01-01

A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L −1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L −1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic

Organic-Inorganic Hybrid Hollow Mesoporous Organosilica Nanoparticles for Efficient Ultrasound-Based Imaging and Controlled Drug Release

Directory of Open Access Journals (Sweden)

Xiaoqin Qian

2014-01-01

Full Text Available A novel anticancer drug delivery system with contrast-enhanced ultrasound-imaging performance was synthesized by a typical hard-templating method using monodispersed silica nanoparticles as the templates, which was based on unique molecularly organic/inorganic hybrid hollow periodic mesoporous organosilicas (HPMOs. The highly dispersed HPMOs show the uniform spherical morphology, large hollow interior, and well-defined mesoporous structures, which are very beneficial for ultrasound-based theranostics. The obtained HPMOs exhibit excellent performances in contrast-enhanced ultrasonography both in vitro and in vivo and can be used for the real-time determination of the progress of lesion tissues during the chemotherapeutic process. Importantly, hydrophobic paclitaxel- (PTX- loaded HPMOs combined with ultrasound irradiation show fast ultrasound responsiveness for controlled drug release and higher in vitro and in vivo tumor inhibition rates compared with free PTX and PTX-loaded HPMOs, which is due to the enhanced ultrasound-triggered drug release and ultrasound-induced cavitation effect. Therefore, the achieved novel HPMOs-based nanoparticle systems will find broad application potentials in clinically ultrasound-based imaging and auxiliary tumor chemotherapy.

Fabrication and imaging study of ultrasound/fluorescence bi-modal contrast agent based on polymeric microbubbles

International Nuclear Information System (INIS)

Xing Zhanwen; Ke Hengte; Wang Jinrui; Zhao Bo; Qu Enze; Yue Xiuli; Dai Zhifei

2013-01-01

Objective: To fabricate an ultrasound/fluorescence bi-modal contrast agent by encapsulating fluorescent quantum dots into polymeric ultrasound contrast agent microbubbles. Methods: Polylactic acid (PLA, 500 mg), (1R)-(+)-camphor (50 mg) and CdSe/ZnS quantum dots (0.5 ml, 2.3 μmol/L)were dissolved or dispersed in dichloromethane (10 ml) to form in an organic phase. Ammonium carbonate solution and poly (vinyl alcohol) solution were employed as the internal and external water phase, respectively. The fluorescent microbubbles were generated using double emulsion solvent evaporation and lyophilization methods. The morphology and illumination were characterized by scanning electron microscopy (SEM) and fluorescence spectrophotometry. Synchronized contrast-enhanced ultrasound and fluorescence imaging was acquired by injecting fluorescent microbubbles into the silicone tube coupled to a self-made ultrasound/fluorescence imaging device. Ultrasound/fluorescence bi-modal in vivo imaging was acquired on the kidney of New Zealand rabbits and suckling mice. Results: The fluorescent microbubbles were hollow spheres with an averaged diameter of (1.62 ± 1.47) μm. More than 99% of these microbubbles were less than 8 μm in diameter, which met the size criteria for ultrasound contrast agents. The fluorescence emission peak of the microbubbles appeared at 632 nm, indicating that good luminescence properties of quantum dots were maintained. In vitro ultrasound/fluorescence imaging showed no echoic signal when the silicone tube was filled with saline, but there was a strong echo when filled with fluorescent microbubbles. The liquid column with fluorescent microbubbles emitted red luminescence under ultraviolet irradiation. The kidney of the rabbit was remarkably enhanced after the administration of fluorescent microbubbles. Bright fluorescence could be observed at the injection site of the suckling mice via subcutaneous injection. Conclusions: A bi-modal but single contrast agent

Ultrasound-assisted endoscopic partial plantar fascia release.

Science.gov (United States)

Ohuchi, Hiroshi; Ichikawa, Ken; Shinga, Kotaro; Hattori, Soichi; Yamada, Shin; Takahashi, Kazuhisa

2013-01-01

Various surgical treatment procedures for plantar fasciitis, such as open surgery, percutaneous release, and endoscopic surgery, exist. Skin trouble, nerve disturbance, infection, and persistent pain associated with prolonged recovery time are complications of open surgery. Endoscopic partial plantar fascia release offers the surgeon clear visualization of the anatomy at the surgical site. However, the primary medial portal and portal tract used for this technique have been shown to be in close proximity to the posterior tibial nerves and their branches, and there is always the risk of nerve damage by introducing the endoscope deep to the plantar fascia. By performing endoscopic partial plantar fascia release under ultrasound assistance, we could dynamically visualize the direction of the endoscope and instrument introduction, thus preventing nerve damage from inadvertent insertion deep to the fascia. Full-thickness release of the plantar fascia at the ideal position could also be confirmed under ultrasound imaging. We discuss the technique for this new procedure.

Faraday rotation dispersion microscopy imaging of diamagnetic and chiral liquids with pulsed magnetic field.

Science.gov (United States)

Suwa, Masayori; Nakano, Yusuke; Tsukahara, Satoshi; Watarai, Hitoshi

2013-05-21

We have constructed an experimental setup for Faraday rotation dispersion imaging and demonstrated the performance of a novel imaging principle. By using a pulsed magnetic field and a polarized light synchronized to the magnetic field, quantitative Faraday rotation images of diamagnetic organic liquids in glass capillaries were observed. Nonaromatic hydrocarbons, benzene derivatives, and naphthalene derivatives were clearly distinguished by the Faraday rotation images due to the difference in Verdet constants. From the wavelength dispersion of the Faraday rotation images in the visible region, it was found that the resonance wavelength in the UV region, which was estimated based on the Faraday B-term, could be used as characteristic parameters for the imaging of the liquids. Furthermore, simultaneous acquisition of Faraday rotation image and natural optical rotation image was demonstrated for chiral organic liquids.

Efficacy evaluation of laparoscopy assisted ultrasound guided radiofrequency ablation in the treatment of hepatocellular carcinoma beneath the diaphragm

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Song WANG

2017-06-01

Full Text Available Objective To explore the feasibility, safety and efficacy of laparoscopy assisted ultrasound guided radiofrequency ablation (RFA in the treatment of hepatocellular carcinoma (HCC beneath the diaphragm. Methods Twenty- three consecutive patients with solitary HCC beneath the diaphragm were treated by laparoscopy assisted ultrasound guided RFA in the Chinese PLA General Hospital from January 2013 to March 2016. We observed the perioperative complications and followed- up long-term effect. Results All the 23 patients successfully underwent laparoscopy assisted ultrasound guided radiofrequency ablation. No serious complications such as massive hemorrhage, biliary fistula and severe pleural effusion, hemopneumothorax occurred in the patients during perioperative period. CT examination 2-3 days after the operation revealed that the tumor was completely covered by the ablation area. Besides, the survival condition was satisfactory during follow-up period of 9-38 months. Conclusion Laparoscopy-assisted ultrasound-guided radiofrequency ablation is effective and safe for HCC beneath the diaphragm. DOI: 10.11855/j.issn.0577-7402.2017.05.16

Entrapment of curcumin into monoolein-based liquid crystalline nanoparticle dispersion for enhancement of stability and anticancer activity

Science.gov (United States)

Baskaran, Rengarajan; Madheswaran, Thiagarajan; Sundaramoorthy, Pasupathi; Kim, Hwan Mook; Yoo, Bong Kyu

2014-01-01

Despite the promising anticancer potential of curcumin, its therapeutic application has been limited, owing to its poor solubility, bioavailability, and chemical fragility. Therefore, various formulation approaches have been attempted to address these problems. In this study, we entrapped curcumin into monoolein (MO)-based liquid crystalline nanoparticles (LCNs) and evaluated the physicochemical properties and anticancer activity of the LCN dispersion. The results revealed that particles in the curcumin-loaded LCN dispersion were discrete and monodispersed, and that the entrapment efficiency was almost 100%. The stability of curcumin in the dispersion was surprisingly enhanced (about 75% of the curcumin survived after 45 days of storage at 40°C), and the in vitro release of curcumin was sustained (10% or less over 15 days). Fluorescence-activated cell sorting (FACS) analysis using a human colon cancer cell line (HCT116) exhibited 99.1% fluorescence gating for 5 μM curcumin-loaded LCN dispersion compared to 1.36% for the same concentration of the drug in dimethyl sulfoxide (DMSO), indicating markedly enhanced cellular uptake. Consistent with the enhanced cellular uptake of curcumin-loaded LCNs, anticancer activity and cell cycle studies demonstrated apoptosis induction when the cells were treated with the LCN dispersion; however, there was neither noticeable cell death nor significant changes in the cell cycle for the same concentration of the drug in DMSO. In conclusion, entrapping curcumin into MO-based LCNs may provide, in the future, a strategy for overcoming the hurdles associated with both the stability and cellular uptake issues of the drug in the treatment of various cancers. PMID:25061290

The role of ultrasound in controlling the liquid-liquid phase separation and nucleation of vanillin polymorphs I and II

Science.gov (United States)

Parimaladevi, P.; Supriya, S.; Srinivasan, K.

2018-02-01

The influence of ultrasound on liquid-liquid phase separation (LLPS) and polymorphism of vanillin in aqueous solution has been investigated for the first time by varying the ultrasonic parameters such as power, pulse rate and insonation time at ambient condition. Results reveal that the application of ultrasound controls the impact of LLPS and accelerates the nucleation of vanillin within a short period at lower levels of ultrasonic process parameters, and also enhances the quality of the nucleated crystals. Moreover, the application of ultrasound induces the nucleation of rare and metastable polymorph of vanillin Form II in aqueous solution. But, at higher levels of power, pulse rate and insonation time, the rate of LLPS is found increased and the quality of the crystals becomes deteriorated. Morphology of the nucleated polymorphs were identified through optical microscopy and confirmed by optical goniometry. The internal structure and thermal stability of the grown stable Form I and metastable Form II of vanillin were confirmed through powder X-ray diffraction (PXRD) and differential scanning calorimetry (DSC) analyses. Further, results suggest that the ultrasound has profound effect in controlling the LLPS and nucleation of vanillin polymorphs in aqueous solution.

Dispersive liquid-liquid microextraction of copper ions as neocuproine complex in environmental aqueous samples.

Science.gov (United States)

Shariati, Shahab; Golshekan, Mostafa

2011-06-01

In the present study, a simple and efficient extraction method based on dispersive liquid-liquid microextraction prior to UV-Vis spectrophotometry was developed for the preconcentration and determination of copper ions in environmental samples. Briefly, cupric ions (Cu II) were reduced to cuprous (Cu I) with addition of hydroxyl amine hydrochloride and formed hydrophobic chelates with neocuproine. Then, a proper mixture of acetonitrile (as dispersive solvent) and choloroform (as extraction solvent) was rapidly injected into the solution and a cloudy solution was formed. After centrifuging, choloroform was sedimented at the bottom of a conical tube and diluted with 100 µL of methanol for further UV-Vis spectrophotometry measurement. An orthogonal array design (OAD) was employed to study the effects of different parameters on the extraction efficiency. Under the optimum experimental conditions, a preconcentration factor up to 63.6 was achieved for extraction from 5.0 mL of sample solution. The limit of detection (LOD) based on S/N = 3 was 0.33 µg L-1 and the calibration curve was linear in the range of 1-200 µg L-1 with reasonable linearity (r2 > 0.997). Finally, the accuracy of the proposed method was successfully evaluated by determination of trace amounts of copper ions in different water samples and satisfactory results were obtained.

Efficient sample preparation method based on solvent-assisted dispersive solid-phase extraction for the trace detection of butachlor in urine and waste water samples.

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Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

2016-10-01

In this work, an efficient sample preparation method termed solvent-assisted dispersive solid-phase extraction was applied. The used sample preparation method was based on the dispersion of the sorbent (benzophenone) into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the butachlor, the cloudy solution was centrifuged and butachlor in the sediment phase dissolved in ethanol and determined by gas chromatography with flame ionization detection. Under the optimized conditions (solution pH = 7.0, sorbent: benzophenone, 2%, disperser solvent: ethanol, 500 μL, centrifuged at 4000 rpm for 3 min), the method detection limit for butachlor was 2, 3 and 3 μg/L for distilled water, waste water, and urine sample, respectively. Furthermore, the preconcentration factor was 198.8, 175.0, and 174.2 in distilled water, waste water, and urine sample, respectively. Solvent-assisted dispersive solid-phase extraction was successfully used for the trace monitoring of butachlor in urine and waste water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of statin drugs in hospital effluent with dispersive liquid-liquid microextraction and quantification by liquid chromatography.

Science.gov (United States)

Martins, Ayrton F; Frank, Carla da S; Altissimo, Joseline; de Oliveira, Júlia A; da Silva, Daiane S; Reichert, Jaqueline F; Souza, Darliana M

2017-08-24

Statins are classified as being amongst the most prescribed agents for treating hypercholesterolaemia and preventing vascular diseases. In this study, a rapid and effective liquid chromatography method, assisted by diode array detection, was designed and validated for the simultaneous quantification of atorvastatin (ATO) and simvastatin (SIM) in hospital effluent samples. The solid phase extraction (SPE) of the analytes was optimized regarding sorbent material and pH, and the dispersive liquid-liquid microextraction (DLLME), in terms of pH, ionic strength, type and volume of extractor/dispersor solvents. The performance of both extraction procedures was evaluated in terms of linearity, quantification limits, accuracy (recovery %), precision and matrix effects for each analyte. The methods proved to be linear in the concentration range considered; the quantification limits were 0.45 µg L -1 for ATO and 0.75 µg L -1 for SIM; the matrix effect was almost absent in both methods and the average recoveries remained between 81.5-90.0%; and the RSD values were <20%. The validated methods were applied to the quantification of the statins in real samples of hospital effluent; the concentrations ranged from 18.8 µg L -1 to 35.3 µg L -1 for ATO, and from 30.3 µg L -1 to 38.5 µg L -1 for SIM. Since the calculated risk quotient was ≤192, the occurrence of ATO and SIM in hospital effluent poses a potential serious risk to human health and the aquatic ecosystem.

Comparison of two novel in-syringe dispersive liquid-liquid microextraction techniques for the determination of iodide in water samples using spectrophotometry.

Science.gov (United States)

Kaykhaii, Massoud; Sargazi, Mona

2014-01-01

Two new, rapid methodologies have been developed and applied successfully for the determination of trace levels of iodide in real water samples. Both techniques are based on a combination of in-syringe dispersive liquid-liquid microextraction (IS-DLLME) and micro-volume UV-Vis spectrophotometry. In the first technique, iodide is oxidized with nitrous acid to the colorless anion of ICl2(-) at high concentration of hydrochloric acid. Rhodamine B is added and by means of one step IS-DLLME, the ion-pair formed was extracted into toluene and measured spectrophotometrically. Acetone is used as dispersive solvent. The second method is based on the IS-DLLME microextraction of iodide as iodide/1, 10-phenanthroline-iron((II)) chelate cation ion-pair (colored) into nitrobenzene. Methanol was selected as dispersive solvent. Optimal conditions for iodide extraction were determined for both approaches. Methods are compared in terms of analytical parameters such as precision, accuracy, speed and limit of detection. Both methods were successfully applied to determining iodide in tap and river water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Dispersion of breakdown voltage of liquid helium

International Nuclear Information System (INIS)

Ishii, Itaru; Noguchi, Takuya

1978-01-01

As for the electrical insulation characteristics of liquid helium, the discrepancy among the measured values by each person is very large even in the fundamental DC breakdown voltage in uniform electric field. The dispersion of experimental values obtained in the experiments by the same person is also large. Hereafter, the difference among the mean values obtained by each experimenter will be referred to as ''deviation of mean values'', and the dispersion of measured values around the mean value obtained by the same person as ''deviation around the man value''. The authors have mainly investigated on the latter experimentally. The cryostat was made of stainless steel, and the innermost helium chamber was of 500 mm I.D. and approximately 1200 mm deep. The high voltage electrode was of brass sphere of 25 mm diameter, and the low voltage electrode was of brass plate. The experiment was conducted for liquid helium boiling at 4.2 K and 1 atm, and the breakdown voltage and time lag were measured by applying the approximately square wave impulses of fast rise and long tail, ramp and DC voltages. The cause of the deviation of mean values may be the presence of impurity particles or the effect of electrode shape. As for the deviation around the mean value, the dispersion is large, and its standard deviation may amount to 10 to 20% of the man value. The dispersion is not due to the statistical time lag, but is due to parameters that vary with breakdown. (Wakatsuki, Y.)

Kinetic Study on Ultrasound Assisted Biodiesel Production from Waste Cooking Oil

Directory of Open Access Journals (Sweden)

Widayat

2015-09-01

Full Text Available The objective of this research was to study a kinetic model of biodiesel production from waste cooking oil assisted by ultrasound power. The model considered the biodiesel production process as a 2nd order reversible reaction, while its kinetic parameters were estimated using MATLAB, based on data extracted from Hingu, et al. [1]. The data represented experiments under low-frequency ultrasonic wave (20 kHz and variations of temperature, power, catalyst concentration, and alcohol-oil molar ratio. Statistical analysis showed that the proposed model fits well to the experimental data with a determination coefficient (R2 higher than 0.9.

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.

Ultrasound-Assisted Extraction of Stilbenes from Grape Canes.

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Piñeiro, Zulema; Marrufo-Curtido, Almudena; Serrano, Maria Jose; Palma, Miguel

2016-06-16

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.

Optimization of dispersive liquid-phase microextraction based on solidified floating organic drop combined with high-performance liquid chromatography for the analysis of glucocorticoid residues in food.

Science.gov (United States)

Huang, Yuan; Zheng, Zhiqun; Huang, Liying; Yao, Hong; Wu, Xiao Shan; Li, Shaoguang; Lin, Dandan

2017-05-10

A rapid, simple, cost-effective dispersive liquid-phase microextraction based on solidified floating organic drop (SFOD-LPME) was developed in this study. Along with high-performance liquid chromatography, we used the developed approach to determine and enrich trace amounts of four glucocorticoids, namely, prednisone, betamethasone, dexamethasone, and cortisone acetate, in animal-derived food. We also investigated and optimized several important parameters that influenced the extraction efficiency of SFOD-LPME. These parameters include the extractant species, volumes of extraction and dispersant solvents, sodium chloride addition, sample pH, extraction time and temperature, and stirring rate. Under optimum experimental conditions, the calibration graph exhibited linearity over the range of 1.2-200.0ng/ml for the four analytes, with a reasonable linearity(r 2 : 0.9990-0.9999). The enrichment factor was 142-276, and the detection limits was 0.39-0.46ng/ml (0.078-0.23μg/kg). This method was successfully applied to analyze actual food samples, and good spiked recoveries of over 81.5%-114.3% were obtained. Copyright © 2017. Published by Elsevier B.V.

Ultrasound-assisted oxidative process for sulfur removal from petroleum product feedstock.

Science.gov (United States)

Mello, Paola de A; Duarte, Fábio A; Nunes, Matheus A G; Alencar, Mauricio S; Moreira, Elizabeth M; Korn, Mauro; Dressler, Valderi L; Flores, Erico M M

2009-08-01

A procedure using ultrasonic irradiation is proposed for sulfur removal of a petroleum product feedstock. The procedure involves the combination of a peroxyacid and ultrasound-assisted treatment in order to comply with the required sulfur content recommended by the current regulations for fuels. The ultrasound-assisted oxidative desulfurization (UAOD) process was applied to a petroleum product feedstock using dibenzothiophene as a model sulfur compound. The influence of ultrasonic irradiation time, oxidizing reagents amount, kind of solvent for the extraction step and kind of organic acid were investigated. The use of ultrasonic irradiation allowed higher efficiency for sulfur removal in comparison to experiments performed without its application, under the same reactional conditions. Using the optimized conditions for UAOD, the sulfur removal was about 95% after 9min of ultrasonic irradiation (20kHz, 750W, run at 40%), using hydrogen peroxide and acetic acid, followed by extraction with methanol.

Effervescence-assisted dispersive solid-phase extraction using ionic-liquid-modified magnetic β-cyclodextrin/attapulgite coupled with high-performance liquid chromatography for fungicide detection in honey and juice.

Science.gov (United States)

Wu, Xiaoling; Yang, Miyi; Zeng, Haozhe; Xi, Xuefei; Zhang, Sanbing; Lu, Runhua; Gao, Haixiang; Zhou, Wenfeng

2016-11-01

In this study, a simple effervescence-assisted dispersive solid-phase extraction method was developed to detect fungicides in honey and juice. Most significantly, an innovative ionic-liquid-modified magnetic β-cyclodextrin/attapulgite sorbent was used because its large specific surface area enhanced the extraction capacity and also led to facile separation. A one-factor-at-a-time approach and orthogonal design were employed to optimize the experimental parameters. Under the optimized conditions, the entire extraction procedure was completed within 3 min. In addition, the calibration curves exhibited good linearity, and high enrichment factors were achieved for pure water and honey samples. For the honey samples, the extraction efficiencies for the target fungicides ranged from 77.0 to 94.3% with relative standard deviations of 2.3-5.44%. The detection and quantitation limits were in the ranges of 0.07-0.38 and 0.23-1.27 μg/L, respectively. Finally, the developed technique was successfully applied to real samples, and satisfactory results were achieved. This analytical technique is cost-effective, environmentally friendly, and time-saving. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Measurement of the ultrasound attenuation and dispersion in whole human blood and its components from 0-70 MHz.

Science.gov (United States)

Treeby, Bradley E; Zhang, Edward Z; Thomas, Alison S; Cox, Ben T

2011-02-01

The ultrasound attenuation coefficient and dispersion from 0-70 MHz in whole human blood and its components (red blood cells and plasma) at 37°C is reported. The measurements are made using a fixed path substitution technique that exploits optical mechanisms for the generation and detection of ultrasound. This allows the measurements to cover a broad frequency range with a single source and receiver. The measured attenuation coefficient and dispersion in solutions of red blood cells and physiological saline for total haemoglobin concentrations of 10, 15 and 20 g/dL are presented. The attenuation coefficient and dispersion in whole human blood taken from four healthy volunteers by venipuncture is also reported. The power law dependence of the attenuation coefficient is shown to vary across the measured frequency range. This is due to the varying frequency dependence of the different mechanisms responsible for the attenuation. The attenuation coefficient measured at high frequencies is found to be significantly higher than that predicted by historical power law parameters. A review of the attenuation mechanisms in blood along with previously reported experimental measurements is given. Values for the sound speed and density in the tested samples are also presented. Copyright © 2011 World Federation for Ultrasound in Medicine & Biology. Published by Elsevier Inc. All rights reserved.

Modified Dispersive Liquid-Liquid Micro Extraction Using Green Solvent for Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Vegetable Samples

International Nuclear Information System (INIS)

Kin, C.M.; Shing, W.L.

2016-01-01

According to International Agency for Research on Cancer (IARC), most of Polycyclic Aromatic Hydrocarbons (PAHs) known as genotoxic human carcinogen and mutagenic. PAHs represent as poorly degradable pollutants that exist in soils, sediments, surface water and atmosphere. A simple, rapid and sensitive extraction method termed modified Dispersive Liquid-Liquid Micro extraction (DLLME) using green solvent was developed to determine PAHs in vegetable samples namely radish, cabbage and cucumber prior to Gas Chromatography Flame Ionization Detection (GC-FID). The extraction method is based on replacing chlorinated organic extraction solvent in the conventional DLLME with low toxic solvent, 1-bromo-3-methylbutane without using dispersive solvent. Several experimental factors such as type and volume of extraction solvents, extraction time, confirmation of 12 PAHs by GC-MS, recovery percentages on vegetable samples and the comparative analysis with conventional DLLME were carried out. Both DLLME were successfully extracted 12 types of PAHs. In modified DLLME, the recoveries of the analytes obtained were in a range of 72.72 - 88.07 % with RSD value below 7.5 % which is comparable to the conventional DLLME. The use of microliter of low toxic extraction solvent without addition of dispersive solvent caused the method is economic and environmental friendly which is fulfill the current requirement, green chemistry based analytical method. (author)

Resistive sensing of gaseous nitrogen dioxide using a dispersion of single-walled carbon nanotubes in an ionic liquid

Energy Technology Data Exchange (ETDEWEB)

Mishra, Prabhash [Solidstate Electronics Research Laboratory (SERL), Faculty of Engineering and Technology, Jamia Millia Islamia, Jamia Nagar, New Delhi 110025 (India); Department of Nanoengineering, Samara State Aerospace University, 443086 Samara (Russian Federation); Pavelyev, V.S. [Department of Nanoengineering, Samara State Aerospace University, 443086 Samara (Russian Federation); Patel, Rajan [Center for Interdisciplinary Research in Basic Sciences (CIRBSc), Jamia Millia Islamia, Jamia Nagar, New Delhi 110025 (India); Islam, S.S., E-mail: sislam@jmi.ac.in [Solidstate Electronics Research Laboratory (SERL), Faculty of Engineering and Technology, Jamia Millia Islamia, Jamia Nagar, New Delhi 110025 (India)

2016-06-15

Graphical abstract: Ionic liquid ([C6-mim]PF6) used as dispersant agent for SWCNTs: An investigations were carried out to find the structural quality and surface modification for sensor application. - Highlights: • An effective technique based on Ionic liquids (IL) and their use as a dispersant. • Electron microscopy and spectroscopy for structure characterization. • Covalent linkage of ILs with SWNTs and dispersion of SWCNTs. • The IL-wrapped sensing film, capable for detecting trace levels of gas. - Abstract: Single-walled carbon nanotubes (SWCNTs) were dispersed in an imidazolium-based ionic liquid (IL) and investigated in terms of structural quality, surface functionalization and inter-CNT force. Analysis by field emission electron microscopy and transmission electron microscopy shows the IL layer to coat the SWNTs, and FTIR and Raman spectroscopy confirm strong binding of the ILs to the SWNTs. Two kinds of resistive sensors were fabricated, one by drop casting of IL-wrapped SWCNTs, the other by conventional dispersion of SWCNTs. Good response and recovery to NO{sub 2} is achieved with the IL-wrapped SWCNTs material upon UV-light exposure, which is needed because decrease the desorption energy barrier to increase the gas molecule desorption. NO{sub 2} can be detected in the 1–20 ppm concentration range. The sensor is not interfered by humidity due to the hydrophobic tail of PF6 (ionic liquid) that makes our sensor highly resistant to moisture.

Using Power Ultrasound to Accelerate Food Freezing Processes: Effects on Freezing Efficiency and Food Microstructure.

Science.gov (United States)

Zhang, Peizhi; Zhu, Zhiwei; Sun, Da-Wen

2018-05-31

Freezing is an effective way of food preservation. However, traditional freezing methods have the disadvantages of low freezing efficiency and generation of large ice crystals, leading to possible damage of food quality. Power ultrasound assisted freezing as a novel technique can effectively reduce the adverse effects during freezing process. This paper gives an overview on recent researches of power ultrasound technique to accelerate the food freezing processes and illustrates the main principles of power ultrasound assisted freezing. The effects of power ultrasound on liquid food, model solid food as well as fruit and vegetables are discussed, respectively, from the aspects of increasing freezing rate and improving microstructure. It is shown that ultrasound assisted freezing can effectively improve the freezing efficiency and promote the formation of small and evenly distributed ice crystals, resulting in better food quality. Different inherent properties of food samples affect the effectiveness of ultrasound application and optimum ultrasound parameters depend on the nature of the samples. The application of ultrasound to the food industry is more likely on certain types of food products and more efforts are still needed to realize the industrial translation of laboratory results.

Treatment of tanneries waste water by ultrasound assisted electrolysis process

International Nuclear Information System (INIS)

Farooq, R.; Ahmed, Z.; Gilani, M. A.; Durrani, M.; Mahmood, Q.; Shaukat, S. F.; Choima, N.

2013-01-01

The leather industry is a major producer of wastewater and solid waste containing potential water and soil contaminants. Considering the large amount and variety of chemical agents used in skin processing, the wastewaters generated by tanneries are very complex. Therefore, the development of treatment methods for these effluents is extremely necessary. In this work the electrochemical treatment of a tannery wastewater by ultrasound assisted electrochemical process, using stainless steel and lead cathode and titanium anodes was studied. Effect of ultrasound irradiation at various ultrasonic intensities 0, 40, 60 and 80% on electrochemical removal of chromium was investigated. Experiments were conducted at two pH conditions of pH 3 and 9. Significant removal of chromium was found at pH 3 and it was also noticed that by increasing ultrasonic intensities, percentage removal of chromium and sulfate also increases. The optimum removal of chromium and sulfate ions was observed at 80% ultrasonic intensity. The technique of electrolysis assisted with ultrasonic waves can be further improved and can be the future waste water treatment process for industries. (author)

Luminescence screening of enrofloxacin and ciprofloxacin residues in swine liver after dispersive liquid - liquid microextraction cleanup

Science.gov (United States)

A rapid luminescence method was developed to screen residues of enrofloxacin (ENRO) and its metabolite, ciprofloxacin (CIPRO), in swine liver. Target analytes were extracted in acetonitrile-2.5% trifluoroacetic acid-NaCl, cleaned up by dispersive liquid-liquid microextraction (DLLME), and finally de...

Mechanisms of dispersion during liquid hydrogen leakage

International Nuclear Information System (INIS)

Proust, C.; Gaston, D.

2000-01-01

INERIS conducts research programs with a mission of assessing and preventing accidental and chronic risks to people and the environment due to industrial plants, chemical substances and underground operation. This paper is a study of the dispersion mechanism of cryogenic hydrogen and the mechanisms of flame propagation in clouds of hydrogen. The objective is to contribute to the industrial control implementation of significant storage of hydrogen liquid that has pressure close to the atmospheric pressure. Within the framework of this program, the only interest is with the risk presented by escape of significant flow. This corresponds to accidental ruptures in tanks. The following four phases are looked at: the escape incident and the determination of the leak flow; the formation of the liquid layer and the vaporization of the hydrogen; the formation of the Hydrogen cloud in air; and the explosive ignition in the atmosphere, propagation of the explosive flame and evaluation of the pressure wave. This situation has been limited to dispersion in free air and does not consider the impact of containment

Carbon nanotubes: are they dispersed or dissolved in liquids?

Directory of Open Access Journals (Sweden)

Premkumar Thathan

2011-01-01

Full Text Available Abstract Carbon nanotubes (CNTs constitute a novel class of nanomaterials with remarkable applications in diverse domains. However, the main intrincsic problem of CNTs is their insolubility or very poor solubility in most of the common solvents. The basic key question here is: are carbon nanotubes dissolved or dispersed in liquids, specifically in water? When analyzing the scientific research articles published in various leading journals, we found that many researchers confused between "dispersion" and "solubilization" and use the terms interchangeably, particularly when stating the interaction of CNTs with liquids. In this article, we address this fundamental issue to give basic insight specifically to the researchers who are working with CNTs as well asgenerally to scientists who deal with nano-related research domains.

Dichroic dye-dependent studies in guest-host polymer-dispersed liquid crystal films

Energy Technology Data Exchange (ETDEWEB)

Malik, Praveen, E-mail: pmalik100@yahoo.co [Department of Physics, Dr. B.R. Ambedkar National Institute of Technology, Jalandhar 144011, Punjab (India); Raina, K.K. [Liquid Crystal Group, Materials Research Laboratory, School of Physics and Materials Science, Thapar University, Patiala 147004, Punjab (India)

2010-01-01

Guest-host polymer-dispersed liquid crystal (GHPDLC) films were prepared using a nematic liquid crystal, photo-curable polymer and dichroic dye (anthraquinone blue) by polymerization-induced phase separation (PIPS) technique. Non-ionic dichroic dye (1%, 2% and 4% wt./wt. ratio) was taken as guest in PDLC host. Polarizing microscopy shows that in the absence of electric field, liquid crystal (LC) droplets in polymer matrix mainly exhibit bipolar configuration, however, relatively at higher field, maltese-type crosses were observed. Our results show that approx1% dye-doped PDLC film shows better transmission and faster response times over pure polymer-dispersed nematic liquid crystal (PDNLC) and higher concentrated (2% and 4%) GHPDLC films.

Dichroic dye-dependent studies in guest-host polymer-dispersed liquid crystal films

International Nuclear Information System (INIS)

Malik, Praveen; Raina, K.K.

2010-01-01

Guest-host polymer-dispersed liquid crystal (GHPDLC) films were prepared using a nematic liquid crystal, photo-curable polymer and dichroic dye (anthraquinone blue) by polymerization-induced phase separation (PIPS) technique. Non-ionic dichroic dye (1%, 2% and 4% wt./wt. ratio) was taken as guest in PDLC host. Polarizing microscopy shows that in the absence of electric field, liquid crystal (LC) droplets in polymer matrix mainly exhibit bipolar configuration, however, relatively at higher field, maltese-type crosses were observed. Our results show that ∼1% dye-doped PDLC film shows better transmission and faster response times over pure polymer-dispersed nematic liquid crystal (PDNLC) and higher concentrated (2% and 4%) GHPDLC films.

Optimization of ultrasound-assisted extraction of phenolic compounds from grapefruit (Citrus paradisi Macf.) leaves via D-optimal design and artificial neural network design with categorical and quantitative variables.

Science.gov (United States)

Ciğeroğlu, Zeynep; Aras, Ömür; Pinto, Carlos A; Bayramoglu, Mahmut; Kırbaşlar, Ş İsmail; Lorenzo, José M; Barba, Francisco J; Saraiva, Jorge A; Şahin, Selin

2018-03-06

The extraction of phenolic compounds from grapefruit leaves assisted by ultrasound-assisted extraction (UAE) was optimized using response surface methodology (RSM) by means of D-optimal experimental design and artificial neural network (ANN). For this purpose, five numerical factors were selected: ethanol concentration (0-50%), extraction time (15-60 min), extraction temperature (25-50 °C), solid:liquid ratio (50-100 g L -1 ) and calorimetric energy density of ultrasound (0.25-0.50 kW L -1 ), whereas ultrasound probe horn diameter (13 or 19 mm) was chosen as categorical factor. The optimized experimental conditions yielded by RSM were: 10.80% for ethanol concentration; 58.52 min for extraction time; 30.37 °C for extraction temperature; 52.33 g L -1 for solid:liquid ratio; 0.457 kW L -1 for ultrasonic power density, with thick probe type. Under these conditions total phenolics content was found to be 19.04 mg gallic acid equivalents g -1 dried leaf. The same dataset was used to train multilayer feed-forward networks using different approaches via MATLAB, with ANN exhibiting superior performance to RSM (differences included categorical factor in one model and higher regression coefficients), while close values were obtained for the extraction variables under study, except for ethanol concentration and extraction time. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

Ultrasound-Assisted Extraction of Stilbenes from Grape Canes

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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.

Model-based ultrasound temperature visualization during and following HIFU exposure.

Science.gov (United States)

Ye, Guoliang; Smith, Penny Probert; Noble, J Alison

2010-02-01

This paper describes the application of signal processing techniques to improve the robustness of ultrasound feedback for displaying changes in temperature distribution in treatment using high-intensity focused ultrasound (HIFU), especially at the low signal-to-noise ratios that might be expected in in vivo abdominal treatment. Temperature estimation is based on the local displacements in ultrasound images taken during HIFU treatment, and a method to improve robustness to outliers is introduced. The main contribution of the paper is in the application of a Kalman filter, a statistical signal processing technique, which uses a simple analytical temperature model of heat dispersion to improve the temperature estimation from the ultrasound measurements during and after HIFU exposure. To reduce the sensitivity of the method to previous assumptions on the material homogeneity and signal-to-noise ratio, an adaptive form is introduced. The method is illustrated using data from HIFU exposure of ex vivo bovine liver. A particular advantage of the stability it introduces is that the temperature can be visualized not only in the intervals between HIFU exposure but also, for some configurations, during the exposure itself. 2010 World Federation for Ultrasound in Medicine & Biology. Published by Elsevier Inc. All rights reserved.

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

International Nuclear Information System (INIS)

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

2012-01-01

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

Ultrasound-assisted extraction of Ca, K and Mg from in vitro citrus culture

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Arruda Sandra C. C.

2003-01-01

Full Text Available An ultrasound extraction procedure for Ca, K and Mg from in vitro plant cultures is proposed, comparing cultures of different embryogenic levels of Citrus sinensis and Citrus limonia, employing ultrasound energy. Parameters related to metals extraction, such as plant material sampling, acid concentration and sonication time were investigated. For accuracy check, the proposed ultrasound extraction procedure was compared with a microwave-assisted digestion procedure and no differences in the results were verified at 95% of the confidence level. With this simple and accurate extraction procedure, it was possible to determine differences in Ca, K and Mg concentrations during Citrus embryo formation/development and between cultures (embryogenic and non-embryogenic. Finally, the ultrasound extraction method demonstrated to be an excellent alternative for handless sampling and operational costs.

Automation-assisted cervical cancer screening in manual liquid-based cytology with hematoxylin and eosin staining.

Science.gov (United States)

Zhang, Ling; Kong, Hui; Ting Chin, Chien; Liu, Shaoxiong; Fan, Xinmin; Wang, Tianfu; Chen, Siping

2014-03-01

Current automation-assisted technologies for screening cervical cancer mainly rely on automated liquid-based cytology slides with proprietary stain. This is not a cost-efficient approach to be utilized in developing countries. In this article, we propose the first automation-assisted system to screen cervical cancer in manual liquid-based cytology (MLBC) slides with hematoxylin and eosin (H&E) stain, which is inexpensive and more applicable in developing countries. This system consists of three main modules: image acquisition, cell segmentation, and cell classification. First, an autofocusing scheme is proposed to find the global maximum of the focus curve by iteratively comparing image qualities of specific locations. On the autofocused images, the multiway graph cut (GC) is performed globally on the a* channel enhanced image to obtain cytoplasm segmentation. The nuclei, especially abnormal nuclei, are robustly segmented by using GC adaptively and locally. Two concave-based approaches are integrated to split the touching nuclei. To classify the segmented cells, features are selected and preprocessed to improve the sensitivity, and contextual and cytoplasm information are introduced to improve the specificity. Experiments on 26 consecutive image stacks demonstrated that the dynamic autofocusing accuracy was 2.06 μm. On 21 cervical cell images with nonideal imaging condition and pathology, our segmentation method achieved a 93% accuracy for cytoplasm, and a 87.3% F-measure for nuclei, both outperformed state of the art works in terms of accuracy. Additional clinical trials showed that both the sensitivity (88.1%) and the specificity (100%) of our system are satisfyingly high. These results proved the feasibility of automation-assisted cervical cancer screening in MLBC slides with H&E stain, which is highly desirable in community health centers and small hospitals. © 2013 International Society for Advancement of Cytometry.

Functional Smart Dispersed Liquid Crystals for Nano- and Biophotonic Applications: Nanoparticles-Assisted Optical Bioimaging

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N. V. Kamanina

2016-01-01

Full Text Available Functional nematic liquid crystal structures doped with nano- and bioobjects have been investigated. The self-assembling features and the photorefractive parameters of the structured liquid crystals have been comparatively studied via microscopy and laser techniques. Fullerene, quantum dots, carbon nanotubes, DNA, and erythrocytes have been considered as the effective nano- and biosensitizers of the LC mesophase. The holographic recording technique based on four-wave mixing of the laser beams has been used to investigate the laser-induced change of the refractive index in the nano- and bioobjects-doped liquid crystal cells. The special accent has been given to novel nanostructured relief with vertically aligned carbon nanotubes at the interface: solid substrate-liquid crystal mesophase. It has been shown that this nanostructured relief influences the orienting ability of the liquid crystal molecules with good advantage. As a result, it provokes the orientation of the DNA. The modified functional liquid crystal materials have been proposed as the perspective systems for both the photonics and biology as well as the medical applications.

Rayleigh theory of ultrasound scattering applied to liquid-filled contrast nanoparticles.

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Flegg, M B; Poole, C M; Whittaker, A K; Keen, I; Langton, C M

2010-06-07

We present a novel modified theory based upon Rayleigh scattering of ultrasound from composite nanoparticles with a liquid core and solid shell. We derive closed form solutions to the scattering cross-section and have applied this model to an ultrasound contrast agent consisting of a liquid-filled core (perfluorooctyl bromide, PFOB) encapsulated by a polymer shell (poly-caprolactone, PCL). Sensitivity analysis was performed to predict the dependence of the scattering cross-section upon material and dimensional parameters. A rapid increase in the scattering cross-section was achieved by increasing the compressibility of the core, validating the incorporation of high compressibility PFOB; the compressibility of the shell had little impact on the overall scattering cross-section although a more compressible shell is desirable. Changes in the density of the shell and the core result in predicted local minima in the scattering cross-section, approximately corresponding to the PFOB-PCL contrast agent considered; hence, incorporation of a lower shell density could potentially significantly improve the scattering cross-section. A 50% reduction in shell thickness relative to external radius increased the predicted scattering cross-section by 50%. Although it has often been considered that the shell has a negative effect on the echogeneity due to its low compressibility, we have shown that it can potentially play an important role in the echogeneity of the contrast agent. The challenge for the future is to identify suitable shell and core materials that meet the predicted characteristics in order to achieve optimal echogenity.

A novel separation/preconcentration technique based on ultrasonic dispersion liquid-liquid microextraction for determination of trace cobalt by flame atomic absorption spectrometry

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Jingci Li

2012-12-01

Full Text Available An improved method for the determination of trace cobalt in water samples has been developed using ultrasonic dispersion liquid-liquid microextraction (US-DLLME prior to flame atomic absorption spectrometry (FAAS analysis. In this method, cobalt was extracted into the fine droplets of carbon tetrachloride after chelate formation with the water soluble ligand, ammonium pyrrolidine dithiocarbamate (APDC. The fine droplets of carbon tetrachloride were formed and dispersed in the aqueous sample with the help of ultrasonic waves which accelerated the formation of the fine cloudy solution without using disperser solvents. Under optimum conditions, the calibration curve was linear in the range of 2.5-500 μg L-1, with a detection limit of 0.8 μg L-1. The relative standard deviation (RSD for ten replicate measurements of 20 and 500 μg L-1 of cobalt were 3.3 and 2.2%. This proposed method was successfully applied to tap water, river water, and sea water, and accuracy was assessed through the analysis of certified reference water or recovery experiments. Operation simplicity, low cost, high enrichment factor, and low consumption of the extraction solvent are the main advantages of the proposed method.DOI: http://dx.doi.org/10.4314/bcse.v26i1.2

Memory effect of polymer dispersed liquid crystal by hybridization with nanoclay

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2010-01-01

Full Text Available The electro-optical performances of polymer dispersed liquid crystal (PDLC were investigated in the presence of organically modified clays. With the addition and increasing amount of modified clay, driving voltage and memory effect, viz. transparent state of the film after the electricity is off simultaneously increased due most likely to the increased viscosity. Among the two types of modifier, 4-(4-aminophenyl benzonitrile having greater chemical affinity with LC than hexylamine, gave finer dispersion of clay in liquid crystal, greater viscosity, larger driving voltage and response time, and greater memory effect.

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

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F. Arabi

2012-11-01

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

Preconcentration procedure using vortex-assisted liquid-liquid microextraction for the fast determination of trace levels of thorium in water samples

International Nuclear Information System (INIS)

Ehsan Zolfonoun; Maryam Salahinejad

2013-01-01

A new simple and rapid vortex-assisted liquid-liquid microextraction method was applied for the determination of thorium in water samples. In this method, chloroform used as extraction solvent was directly injected into the water sample solution. The extraction solvent was dispersed into the aqueous phase under vigorously shaking with the vortex. After centrifuging, the fine droplets of extractant phase were settled to the bottom of the conical-bottom centrifuge tube. The effect of different experimental parameters on the performance of the method were studied and discussed. Under the optimum conditions, the detection limit for Th(IV) was 7.5 ng mL -1 . The precision of the method, evaluated as the relative standard deviation obtained by analyzing of 10 replicates, was 2.8 %. The practical applicability of the developed method was examined using natural water and monazite sand samples. (author)

Robot-assisted automatic ultrasound calibration.

Science.gov (United States)

Aalamifar, Fereshteh; Cheng, Alexis; Kim, Younsu; Hu, Xiao; Zhang, Haichong K; Guo, Xiaoyu; Boctor, Emad M

2016-10-01

Ultrasound (US) calibration is the process of determining the unknown transformation from a coordinate frame such as the robot's tooltip to the US image frame and is a necessary task for any robotic or tracked US system. US calibration requires submillimeter-range accuracy for most applications, but it is a time-consuming and repetitive task. We provide a new framework for automatic US calibration with robot assistance and without the need for temporal calibration. US calibration based on active echo (AE) phantom was previously proposed, and its superiority over conventional cross-wire phantom-based calibration was shown. In this work, we use AE to guide the robotic arm motion through the process of data collection; we combine the capability of the AE point to localize itself in the frame of the US image with the automatic motion of the robotic arm to provide a framework for calibrating the arm to the US image automatically. We demonstrated the efficacy of the automated method compared to the manual method through experiments. To highlight the necessity of frequent ultrasound calibration, it is demonstrated that the calibration precision changed from 1.67 to 3.20 mm if the data collection is not repeated after a dismounting/mounting of the probe holder. In a large data set experiment, similar reconstruction precision of automatic and manual data collection was observed, while the time was reduced by 58 %. In addition, we compared ten automatic calibrations with ten manual ones, each performed in 15 min, and showed that all the automatic ones could converge in the case of setting the initial matrix as identity, while this was not achieved by manual data sets. Given the same initial matrix, the repeatability of the automatic was [0.46, 0.34, 0.80, 0.47] versus [0.42, 0.51, 0.98, 1.15] mm in the manual case for the US image four corners. The submillimeter accuracy requirement of US calibration makes frequent data collections unavoidable. We proposed an automated

Use of dispersive liquid-liquid microextraction for simultaneous preconcentration of samarium, europium, gadolinium and dysprosium

International Nuclear Information System (INIS)

Mallah, M.H.; Atomic Energy Organization of Iran, Tehran; Shemirani, F.; Ghannadi Maragheh, M.

2008-01-01

A new preconcentration method of dispersive liquid-liquid microextraction (DLLME) was developed for simultaneous preconcentration of samarium, europium, gadolinium and dysprosium. DLLME technique was successfully used as a sample preparation method. In this preconcentration method, an appropriate mixture of extraction solvent, disperser solvent was injected rapidly into an aqueous solution containing Sm, Eu, Gd and Dy after complex formation using chelating reagent of the 1-(2-pyridylazo)-2-naphthol (PAN). After phase separation, 0.5 mL of the settled phase containing enriched analytes was determined by inductively coupled plasma optical emission spectrometry (ICP-OES). The main factors affected the preconcentration of Sm, Eu, Gd and Dy were extraction and dispersive solvent type and their volume, extraction time, volume of chelating agent (PAN), centrifuge speed and drying temperature of the samples. Under the best operating condition simultaneous preconcentration factors of 80, 100, 103 and 78 were obtained for Sm, Eu, Gd and Dy, respectively. (author)

Hairy root culture in a liquid-dispersed bioreactor: characterization of spatial heterogeneity.

Science.gov (United States)

Williams, G R; Doran, P M

2000-01-01

A liquid-dispersed reactor equipped with a vertical mesh cylinder for inoculum support was developed for culture of Atropa belladonna hairy roots. The working volume of the culture vessel was 4.4 L with an aspect ratio of 1.7. Medium was dispersed as a spray onto the top of the root bed, and the roots grew radially outward from the central mesh cylinder to the vessel wall. Significant benefits in terms of liquid drainage and reduced interstitial liquid holdup were obtained using a vertical rather than horizontal support structure for the biomass and by operating the reactor with cocurrent air and liquid flow. With root growth, a pattern of spatial heterogeneity developed in the vessel. Higher local biomass densities, lower volumes of interstitial liquid, lower sugar concentrations, and higher root atropine contents were found in the upper sections of the root bed compared with the lower sections, suggesting a greater level of metabolic activity toward the top of the reactor. Although gas-liquid oxygen transfer to the spray droplets was very rapid, there was evidence of significant oxygen limitations in the reactor. Substantial volumes of non-free-draining interstitial liquid accumulated in the root bed. Roots near the bottom of the vessel trapped up to 3-4 times their own weight in liquid, thus eliminating the advantages of improved contact with the gas phase offered by liquid-dispersed culture systems. Local nutrient and product concentrations in the non-free-draining liquid were significantly different from those in the bulk medium, indicating poor liquid mixing within the root bed. Oxygen enrichment of the gas phase improved neither growth nor atropine production, highlighting the greater importance of liquid-solid compared with gas-liquid oxygen transfer resistance. The absence of mechanical or pneumatic agitation and the tendency of the root bed to accumulate liquid and impede drainage were identified as the major limitations to reactor performance. Improved

Dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous separation/preconcentration of nickel, cobalt and copper prior to determination by electrothermal atomic absorption spectrometry

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Mooud Amirkavei

2013-01-01

Full Text Available A dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous extraction of trace amounts of nickel, cobalt and copper followed by their determination with electrothermal atomic absorption spectrometry was developed. 300 µL of acetone and 1-undecanol was injected into an aqueous sample containing diethyldithiocarbamate complexes of metal ions. For a sample volume of 10 mL, enrichment factors of 277, 270 and 300 and detection limits of 1.2, 1.1 and 1 ng L-1 for nickel, cobalt and copper were obtained, respectively. The method was applied to the extraction and determination of these metals in different water samples.

Cavitation dispersion of carbon nanotubes and modification of cement systems

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GUSEV Boris Vladimirovich

2014-12-01

Full Text Available The most common research areas in construction material science deals with the development of new efficient methods to increase strength properties of materials. One of such methods is modification of composite matrices with carbon nanotubes. The characteristics of nanomodified concretes to a great extent depend on selected method of introduction of carbon nanotubes into material. The predispersion of CNT in mixing water with plasticizing additive through ultrasound impact on the environment with colloid and other types of particles including nanoparticles is the most frequently used scientific method which provides even distribution of nanoparticles in cement. In some works the separation of agglomerated CNT in suspension was conducted by means of ultrasound treatment. The further analysis showed that the main drawbacks of ultrasound dispersion are high energy output and low performance. That causes inconvenience for application of them in manufacturing process. The methods of cavitation dispersion which were developed in the late 90ies in the XXI century today are becoming commonly used in practice. The work presents the results of dispersion of multi-layer nanotubes performed on the hydrodynamic cavitation equipment. It was determined that the use of such equipment makes it possible to produce stable and even carbon dispersions and to introduce and distribute them uniformly in concrete in the same way as in the case when ultrasound treatment is performed. The advantages of this technology are considerable decrease of energy consumption and possibility to treat enormous amounts of liquids which are necessary for modification of concrete in real production process.

Dispersive liquid-liquid microextraction with solidification of floating organic droplets for simultaneous extraction of pesticides, pharmaceuticals and personal care products

International Nuclear Information System (INIS)

Marube, Liziane Cardoso; Caldas, Sergiane Souza; Soares, Karina Lotz; Primel, Ednei Gilberto

2015-01-01

Dispersive liquid-liquid microextraction based on solidification of floating organic droplets (DLLME-SFO) has been applied to the extraction of pharmaceutical and personal care products (PPCPs) and pesticides from water samples. The PPCPs included bisphenol A, sodium diclofenac, gemfibrozil, furosemide, glibenclamide, nifedipine, nimesulide, propylparaben and triclocarban. The pesticides included 2,4-D, atrazine, azoxystrobin, cyproconazole, clomazone, dichloran, difenoconazole, diuron, epoxiconazole, fenoxaprop-p-ethyl, fipronil, iprodione, irgarol, propanil, propiconazole, tebuconazole, and trifloxystrobin. The type and volume of extraction solvent, type and volume of disperser solvent, ionic strength and pH were optimized. All species were then quantified by liquid chromatography tandem mass spectrometry (LC-MS/MS). The limits of quantification (LOQs) ranged from 50 to 500 ng L −1 , and the linearity ranged from the LOQ of each compound up to 10,000 ng L −1 . Recoveries ranged from 63 to 120 %, with relative standard deviations lower than 14 %. It is making use of a low-toxicity and affordable extraction solvent (1-dodecanol) and was successfully applied to the analysis of surface water samples. (author)

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

Science.gov (United States)

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

2015-11-01

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

Vortex-assisted magnetic β-cyclodextrin/attapulgite-linked ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the fast determination of four fungicides in water samples.

Science.gov (United States)

Yang, Miyi; Xi, Xuefei; Wu, Xiaoling; Lu, Runhua; Zhou, Wenfeng; Zhang, Sanbing; Gao, Haixiang

2015-02-13

A novel microextraction technique combining magnetic solid-phase microextraction (MSPME) with ionic liquid dispersive liquid-liquid microextraction (IL-DLLME) to determine four fungicides is presented in this work for the first time. The main factors affecting the extraction efficiency were optimized by the one-factor-at-a-time approach and the impacts of these factors were studied by an orthogonal design. Without tedious clean-up procedure, analytes were extracted from the sample to the adsorbent and organic solvent and then desorbed in acetonitrile prior to chromatographic analysis. Under the optimum conditions, good linearity and high enrichment factors were obtained for all analytes, with correlation coefficients ranging from 0.9998 to 1.0000 and enrichment factors ranging 135 and 159 folds. The recoveries for proposed approach were between 98% and 115%, the limits of detection were between 0.02 and 0.04 μg L(-1) and the RSDs changed from 2.96 to 4.16. The method was successfully applied in the analysis of four fungicides (azoxystrobin, chlorothalonil, cyprodinil and trifloxystrobin) in environmental water samples. The recoveries for the real water samples ranged between 81% and 109%. The procedure proved to be a time-saving, environmentally friendly, and efficient analytical technique. Copyright © 2015 Elsevier B.V. All rights reserved.

Ultrasound-Guided Core-Needle Versus Vacuum-Assisted Breast Biopsy: A Cost Analysis Based on the American Society of Breast Surgeons' Mastery of Breast Surgery Registry.

Science.gov (United States)

Grady, Ian; Vasquez, Tony; Tawfik, Sara; Grady, Sean

2017-03-01

To evaluate the cost-efficacy of vacuum-assisted ultrasound-guided breast biopsy instruments compared to ultrasound-guided 14-gauge spring-loaded core-needle biopsy. The American Society of Breast Surgeons' Mastery of Breast Surgery Registry was reviewed. Biopsy findings, any rebiopsy, and the instrument used were abstracted for 31,451 ultrasound-guided biopsy procedures performed between 2001 and July 2014. Rates of cancer diagnosis and rebiopsy were calculated for each instrument. A linear mathematical model was developed to calculate total cost per cancer diagnosis, including procedural costs and the costs of any additional surgical rebiopsy procedures. Mean cost per cancer diagnosis with confidence limits was then determined for 14-gauge spring-loaded core-needle biopsy and 14 different vacuum-assisted instruments. For 14-gauge spring-loaded core-needle biopsy, mean cost per cancer diagnosis was $4346 (4327-$4366). For the vacuum-assisted instruments, mean cost per cancer diagnosis ranged from a low of $3742 ($3732-$3752) to a high of $4779 ($4750-$4809). Vacuum-assisted instruments overall were more cost-effective than core with a mean cost per cancer diagnosis of $4052 ($4038-$4067) (p cancer diagnosis of $3978 ($3964-$3991) (p cancer diagnosis of $4369 ($4350-$4388), a result no better than core (p breast biopsy had a lower mean cost per cancer diagnosis than 14-gauge spring-loaded core-needle biopsy. This advantage was only seen in tethered vacuum-assisted instruments. Within device families, larger instruments tended to outperform smaller instruments.

Synthesis of zirconium dioxide by ultrasound assisted precipitation: effect of calcination temperature.

Science.gov (United States)

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

2011-09-01

Nanostructured zirconium dioxide was synthesized from zirconyl nitrate using both conventional and ultrasound assisted precipitation in alkaline medium. The synthesized samples were calcinated at temperatures ranging from 400°C to 900°C in steps of 100°C. The ZrO(2) specimens were characterized using X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The thermal characteristics of the samples were studied via Differential Scanning Calorimetry-Thermo-Gravimetry Analysis (DSC-TGA). The influence of the calcination temperature on the phase transformation process from monoclinic to tetragonal to cubic zirconia and its consequent effect on the crystallite size and % crystallinity of the synthesized ZrO(2) was studied and interpreted. It was observed that the ultrasound assisted technique helped to hasten to the phase transformation and also at some point resulted in phase stabilization of the synthesized zirconia. Copyright © 2011 Elsevier B.V. All rights reserved.

Rapid screening of oxytetracycline residue in catfish muscle by dispersive liquid-liquid microextraction and europium-sensitized luminescence

Science.gov (United States)

Oxytetracycline (OTC) residue in catfish muscle was screened by dispersive liquid-liquid microextraction (DLLME) and europium-sensitized luminescence (ESL). After extraction in EDTA, HCl, and acetonitrile, cleanup was carried out by DLLME, and ESL was measured at microgram = 385 nm and wavelength = ...

Droplets in annular-dispersed gas-liquid pipe-flows

NARCIS (Netherlands)

Van 't Westende, J.M.C.

2008-01-01

Annular-dispersed gas-liquid pipe-flows are commonly encountered in many industrial applications, and have already been studied for many decades. However, due to the great complexity of this type of flow, there are still many phenomena that are poorly understood. The aim of this thesis is to shed

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

Science.gov (United States)

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

2016-10-01

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

Ultrasound assisted nucleation and growth characteristics of glycine polymorphs--a combined experimental and analytical approach.

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Renuka Devi, K; Raja, A; Srinivasan, K

2015-05-01

For the first time, the effect of ultrasound in the diagnostic frequency range of 1-10 MHz on the nucleation and growth characteristics of glycine has been explored. The investigation employing the ultrasonic interferometer was carried out at a constant insonation time over a wide range of relative supersaturation from σ=-0.09 to 0.76 in the solution. Ultrasound promotes only α nucleation and completely inhibits both the β and γ nucleation in the system. The propagation of ultrasound assisted mass transport facilitates nucleation even at very low supersaturation levels in the solution. The presence of ultrasound exhibits a profound effect on nucleation and growth characteristics in terms of decrease in induction period, increase in nucleation rate and decrease in crystal size than its absence in the solution. With an increase in the frequency of ultrasound, a further decrease in induction period, increase in nucleation rate and decrease in the size of the crystal is noticed even at the same relative supersaturation levels. The increase in the nucleation rate explains the combined dominating effects of both the ultrasound frequency and the supersaturation in the solution. Analytically, the nucleation parameters of the nucleated polymorph have been deduced at different ultrasonic frequencies based on the classical nucleation theory and correlations with the experimental results have been obtained. Structural affirmation of the nucleated polymorph has been ascertained by powder X-ray diffraction. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Directory of Open Access Journals (Sweden)

Ghorbani A.

2014-07-01

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

Preconcentration and determination of ceftazidime in real samples using dispersive liquid-liquid microextraction and high-performance liquid chromatography with the aid of experimental design.

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Razmi, Rasoul; Shahpari, Behrouz; Pourbasheer, Eslam; Boustanifar, Mohammad Hasan; Azari, Zhila; Ebadi, Amin

2016-11-01

A rapid and simple method for the extraction and preconcentration of ceftazidime in aqueous samples has been developed using dispersive liquid-liquid microextraction followed by high-performance liquid chromatography analysis. The extraction parameters, such as the volume of extraction solvent and disperser solvent, salt effect, sample volume, centrifuge rate, centrifuge time, extraction time, and temperature in the dispersive liquid-liquid microextraction process, were studied and optimized with the experimental design methods. Firstly, for the preliminary screening of the parameters the taguchi design was used and then, the fractional factorial design was used for significant factors optimization. At the optimum conditions, the calibration curves for ceftazidime indicated good linearity over the range of 0.001-10 μg/mL with correlation coefficients higher than the 0.98, and the limits of detection were 0.13 and 0.17 ng/mL, for water and urine samples, respectively. The proposed method successfully employed to determine ceftazidime in water and urine samples and good agreement between the experimental data and predictive values has been achieved. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Magnetomotive room temperature dicationic ionic liquid: a new concept toward centrifuge-less dispersive liquid-liquid microextraction.

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Beiraghi, Asadollah; Shokri, Masood; Seidi, Shahram; Godajdar, Bijan Mombani

2015-01-09

A new centrifuge-less dispersive liquid-liquid microextraction technique based on application of magnetomotive room temperature dicationic ionic liquid followed by electrothermal atomic absorption spectrometry (ETAAS) was developed for preconcentration and determination of trace amount of gold and silver in water and ore samples, for the first time. Magnetic ionic liquids not only have the excellent properties of ionic liquids but also exhibit strong response to an external magnetic field. These properties provide more advantages and potential application prospects for magnetic ionic liquids than conventional ones in the fields of extraction processes. In this work, thio-Michler's ketone (TMK) was used as chelating agent to form Ag/Au-TMK complexes. Several important factors affecting extraction efficiency including extraction time, rate of vortex agitator, pH of sample solution, concentration of the chelating agent, volume of ionic liquid as well as effects of interfering species were investigated and optimized. Under the optimal conditions, the limits of detection (LOD) were 3.2 and 7.3ngL(-1) with the preconcentration factors of 245 and 240 for Au and Ag, respectively. The precision values (RSD%, n=7) were 5.3% and 5.8% at the concentration level of 0.05μgL(-1) for Au and Ag, respectively. The relative recoveries for the spiked samples were in the acceptable range of 96-104.5%. The results demonstrated that except Hg(2+), no remarkable interferences are created by other various ions in the determination of Au and Ag, so that the tolerance limits (WIon/WAu or Ag) of major cations and anions were in the range of 250-1000. The validated method was successfully applied for the analysis of Au and Ag in some water and ore samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Air assisted dispersive liquid-liquid microextraction with solidification of the floating organic droplets (AA-DLLME-SFO) and UHPLC-PDA method: Application to antibiotics analysis in human plasma of hospital acquired pneumonia patients.

Science.gov (United States)

Ferrone, Vincenzo; Cotellese, Roberto; Carlucci, Maura; Di Marco, Lorenzo; Carlucci, Giuseppe

2018-03-20

An ultra high-performance liquid chromatographic (UHPLC) method with PDA detection was developed and validated for the simultaneous quantification of metronidazole, meropenem, ciprofloxacin, linezolid and piperacillin in human plasma and applied to patients suffering from hospital acquired pneumonia (HAP). The method uses an air assisted dispersive liquid-liquid microextraction for sample preparation. All parameters in the extraction step, including selection of extractant, amount of extractant, ionic strength, pH, and extraction cycles, were investigated and optimized. Chromatography was carried out using a Poroshell 120 SB C 18 (50 × 2.1 mm I.D. 2.6 μm particle size) column and a gradient mobile phase consisting of ammonium acetate buffer (10 mM, pH 4.0) (eluent A); and a mixture of acetonitrile-methanol in a ratio (80/20)(eluent B). Ulifloxacin was used as internal standard. The method demonstrated good linearity with correlation coefficients, r 2  > 0.9995 for the drugs, as well as high precision (RSD% ≤ 9.87%), accuracy ranged from -8.14% to +8.98. The enrichment factor (EF) obtained ranged within 87 and 121. During the validation, the concentrations of the analytes were found to be stable after 3 freeze-thaw cycles and for at least 24 h after extraction. Subsequently, this method was used to quantify the drugs in patients with HAP in order to establish if the dosage regimen given was sufficient to eradicate the infection at the target site. Copyright © 2017. Published by Elsevier B.V.

Ionic Liquid-Assisted Liquid-Liquid Microextraction based on the Solidification of Floating Organic Droplet in Sample Preparation for Simultaneous Determination of Herbicide Residues in Fruits.

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Vichapong, Jitlada; Santaladchaiyakit, Yanawath; Burakham, Rodjana; Srijaranai, Supalax

2017-09-01

An ionic liquid-assisted liquid-liquid microextraction based on the solidification of floating organic droplet (ILSFODLLME) was investigated for analysis of four herbicide residues (i.e. simazine, atrazine, propazine, and linuron) by high performance liquid chromatography. For ILSFOD-LLME, the optimal extraction conditions were 5% w/v Na2SO4, 30 μL [C4MIM][PF6]RTIL, 100 μL of 1-octanol, ultrasonication time 30 s and centrifugation at 5000 rpm for 5 min. Under the optimal conditions, linearity was obtained within the range of 0.1-1000 μg kg-1, with the correlation coefficients greater than 0.999. The high enrichment factors of the target analytes were in the range of 64.5-139.9 and low limit of detection could be obtained. A modified QuEChERS was applied for fruit sample preparation before analysis. Matrix effects were also investigated using matrix matched standards for construction of the calibration graph. The proposed method has been successfully applied for extraction and preconcentration of herbicide residues in fruit samples, and good recoveries in the range of 87.32% to 99.93% were obtained.

Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography-ultraviolet detection to determination of opium alkaloids in human plasma.

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

2013-11-01

A novel, simple, rapid and sensitive dispersive liquid-liquid microextraction method based on the solidification of floating organic drop (DLLME-SFO) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was used to determine opium alkaloids in human plasma. During the extraction procedure, plasma protein was precipitated by using a mixture of zinc sulfate solution and acetonitrile. Some effective parameters on extraction were studied and optimized. Under the optimum conditions (extraction solvent: 30.0 μl 1-undecanol; disperser solvent: 470 μl acetone; pH: 9; salt addition: 1%(w/v) NaCl and extraction time: 0.5 min), calibration curves are linear in the range of 1.5-1000 μgl(-1) and limit of detections (LODs) are in the range of 0.5-5 μgl(-1). The relative standard deviations (RSDs) for 100 μgl(-1) of morphine and codeine, 10.0 μgl(-1) of papaverine and 20.0 μgl(-1) of noscapine in diluted human plasma are in the range of 4.3-7.4% (n=5). Finally, the method was successfully applied in the determination of opium alkaloids in the actual human plasma samples. The relative recoveries of plasma samples spiked with alkaloids are 88-110.5%. The obtained results show that DLLME-SFO combined with HPLC-UV is a fast and simple method for the determination of opium alkaloids in human plasma. Copyright © 2013 Elsevier B.V. All rights reserved.

Ultrasound assisted synthesis of stable oil in milk emulsion: Study of operating parameters and scale-up aspects.

Science.gov (United States)

Patil, Leena; Gogate, Parag R

2018-01-01

In the present work, application of ultrasound and stirring individually or in combination for improved emulsification of turmeric oil in skimmed milk has been investigated. The effect of different operating parameters/strategies such as addition of surfactant, sodium dodecyl sulfate (SDS), at different concentrations, quantity of oil phase, applied power, sonication time and duty cycle on the droplet size have been investigated. The stability of emulsion was analyzed in terms of the fraction of the emulsion that remains stable for a period of 28days. Optimized set of major emulsification process variables has been used at higher emulsion volumes. The effectiveness of treatment approach was analyzed based on oil droplet size, energy density and the time required for the formation of stable emulsion. It was observed that the stable emulsion at 50mL capacity with mean droplet diameter of about 235.4nm was obtained with the surfactant concentration of 5mg/mL, 11% of rated power (power density: 0.31W/mL) and irradiation time of 5min. The emulsion stability was higher in the case of ultrasound assisted approach as compared to the stirring. For the preparation of stable emulsion at 300mL capacity, it was observed that the sequential approach, i.e., stirring followed by ultrasound, gave lower mean droplet diameter (232.6nm) than the simultaneous approach, i.e., ultrasound and stirring together (257.9nm). However, the study also revealed that the simultaneous approach required very less time (15min) to synthesize stable emulsion as compared to the sequential approach (30min stirring and 60min ultrasound). It was successfully demonstrated that the ultrasound-assisted emulsification in the presence of SDS could be used for the preparation of stable turmeric oil-dairy emulsions, also providing insights into the role of SDS in increasing the stability of emulsions and of ultrasound in giving lower droplet sizes. Copyright © 2017 Elsevier B.V. All rights reserved.

Binary Solvents Dispersive Liquid—Liquid Microextraction (BS-DLLME) Method for Determination of Tramadol in Urine Using High-Performance Liquid Chromatography

Science.gov (United States)

2014-01-01

Background Tramadol is an opioid, synthetic analog of codeine and has been used for the treatment of acute or chronic pain may be abused. In this work, a developed Dispersive liquid liquid microextraction (DLLME) as binary solvents-based dispersive liquid-liquid microextraction (BS-DLLME) combined with high performance liquid chromatography (HPLC) with fluorescence detection (FD) was employed for determination of tramadol in the urine samples. This procedure involves the use of an appropriate mixture of binary extraction solvents (70 μL CHCl3 and 30 μL ethyl acetate) and disperser solvent (600 μL acetone) for the formation of cloudy solution in 5 ml urine sample comprising tramadol and NaCl (7.5%, w/v). After centrifuging, the small droplets of extraction solvents were precipitated. In the final step, the HPLC with fluorescence detection was used for determination of tramadol in the precipitated phase. Results Various factors on the efficiency of the proposed procedure were investigated and optimized. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively. The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6). The relative recoveries of tramadol from urine samples at spiking levels of 10, 30 and 60 μg/L were in the range of 95.6 – 99.6%. Conclusions Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories. PMID:24495475

Enhancement of thermal and mechanical properties of poly(MMA-co-BA)/Cloisite 30B nanocomposites by ultrasound-assisted in-situ emulsion polymerization.

Science.gov (United States)

Sharma, Sachin; Kumar Poddar, Maneesh; Moholkar, Vijayanand S

2017-05-01

This study reports synthesis and characterization of poly(MMA-co-BA)/Cloisite 30B (organo-modified montmorillonite clay) nanocomposites by ultrasound-assisted in-situ emulsion polymerization. Copolymers have been synthesized with MMA:BA monomer ratio of 4:1, and varying clay loading (1-5wt% monomer). The poly(MMA-co-BA)/Cloisite 30B nanocomposites have been characterized for their thermal and mechanical properties. Ultrasonically synthesized nanocomposites have been revealed to possess higher thermal degradation resistance and mechanical strength than the nanocomposites synthesized using conventional techniques. These properties, however, show an optimum (or maxima) with clay loading. The maximum values of thermal and mechanical properties of the nanocomposites with optimum clay loading are as follows. Thermal degradation temperatures: T 10% =320°C (4wt%), T 50 =373°C (4wt%), maximum degradation temperature=384°C (4wt%); glass transition temperature=64.8°C (4wt%); tensile strength=20MPa (2wt%), Young's modulus=1.31GPa (2wt%), Percentage elongation=17.5% (1wt%). Enhanced properties of poly(MMA-co-BA)/Cloisite 30B nanocomposites are attributed to effective exfoliation and dispersion of clay nanoparticles in copolymer matrix due to intense micro-convection induced by ultrasound and cavitation. Clay platelets help in effective heat absorption with maximum surface interaction/adhesion that results in increased thermal resistivity of nanocomposites. Hindered motion of the copolymer chains due to clay platelets results in enhancement of tensile strength and Young's modulus of nanocomposite. Rheological (liquid) study of the nanocomposites reveals that nanocomposites have higher yield stress and infinite shear viscosity than neat copolymer. Nonetheless, nanocomposites still display shear thinning behavior - which is typical of the neat copolymer. Copyright © 2016 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

Xin, Ying; Zhang, Min; Adhikari, Benu

2014-09-01

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

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

Science.gov (United States)

Cui, Feng-Jie; Zhao, Hong-Xia; Sun, Wen-Jing; Wei, Zhuan; Yu, Si-Lian; Zhou, Qiang; Dong, Ying

2013-12-09

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

Decontamination of electronic waste-polluted soil by ultrasound-assisted soil washing.

Science.gov (United States)

Chen, Fu; Yang, Baodan; Ma, Jing; Qu, Junfeng; Liu, Gangjun

2016-10-01

Laboratorial scale experiments were performed to evaluate the efficacy of a washing process using the combination of methyl-β-cyclodextrin (MCD) and tea saponin (TS) for simultaneous desorption of hydrophobic organic contaminants (HOCs) and heavy metals from an electronic waste (e-waste) site. Ultrasonically aided mixing of the field contaminated soil with a combination of MCD and TS solutions simultaneously mobilizes most of polybrominated diphenyl ethers (PBDEs), polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), and the analyte metal (Pb, Cu, and Ni) burdens. It is found that 15 g/L MCD and 10 g/L TS is an efficient reagent combination reconciling extraction performance and reagent costs. Under these conditions, the removal efficiencies of HOCs and heavy metals are 93.5 and 91.2 %, respectively, after 2 cycles of 60-min ultrasound-assisted washing cycles. By contrast, 86.3 % of HOCs and 88.4 % of metals are removed from the soil in the absence of ultrasound after 3 cycles of 120-min washing. The ultrasound-assisted soil washing could generate high removal efficiency and decrease the operating time significantly. Finally, the feasibility of regenerating and reusing the spent washing solution in extracting pollutants from the soil is also demonstrated. By application of this integrated technology, it is possible to recycle the washing solution for a purpose to reduce the consumption of surfactant solutions. Collectively, it has provided an effective and economic treatment of e-waste-polluted soil.

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

Science.gov (United States)

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

2017-08-04

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

Ultrasound assisted synthesis of nanocrystalline zinc oxide: Experiments and modelling

Energy Technology Data Exchange (ETDEWEB)

Hosni, Mongia [Laboratoire des Sciences des Procédés et des Matériaux, LSPM-CNRS, Université Paris 13, 99 av. J.B. Clément, 93430 Villetaneuse (France); Farhat, Samir, E-mail: farhat@lspm.cnrs.fr [Laboratoire des Sciences des Procédés et des Matériaux, LSPM-CNRS, Université Paris 13, 99 av. J.B. Clément, 93430 Villetaneuse (France); Schoenstein, Frederic; Karmous, Farah; Jouini, Noureddine [Laboratoire des Sciences des Procédés et des Matériaux, LSPM-CNRS, Université Paris 13, 99 av. J.B. Clément, 93430 Villetaneuse (France); Viana, Bruno [LCMCP Chimie-Paristech, UPMC, Collège de France, 11 Rue Pierre et Marie Curie, 75231 Paris Cedex 05 (France); Mgaidi, Arbi [Laboratoire de chimie minérale industrielle université Tunis el Manar (Tunisia)

2014-12-05

Highlights: • ZnO nanospheres and nanowires were grown using ultrasound and thermal activation techniques. • The growth uses forced hydrolysis of zinc acetate in diethylene glycol (DEG). • A thermochemical model was developed based on thermodynamic equilibrium calculations. • We estimate species distribution in the bubble in temperature range from 5000 K to ambient. • We propose a new mechanism for ZnO growth assisted by ultrasound irradiation. - Abstract: A fast and green approach is proposed for the preparation of nanocrystalline zinc oxide (ZnO) via ultrasonic (US) irradiation in polyol medium. The process uses forced hydrolysis of zinc acetate in diethylene glycol (DEG). The protocol is compared to thermal activation under the same chemical environment. The activation method is found to be playing a critical role in the selective synthesis of morphologically distinct nanostructures. As compared to thermally activated conventional polyol process, (US) permits to considerably reduce reaction time as well as size of particles. In addition, the shape of these nanoparticles was changed from long nanowires to small nanospheres, indicating different reaction mechanisms. To explain this difference, a thermochemical model was developed based on thermodynamic equilibrium calculations. The model estimate species distribution in the bubble in temperature range from 5000 K to ambient simulating quenching process during bubble formation and collapse. Our results indicate the presence of high density of zinc atoms that could be responsible of a high density of nucleation as compared to thermal activation.

Ultrasound assisted synthesis of nanocrystalline zinc oxide: Experiments and modelling

International Nuclear Information System (INIS)

Hosni, Mongia; Farhat, Samir; Schoenstein, Frederic; Karmous, Farah; Jouini, Noureddine; Viana, Bruno; Mgaidi, Arbi

2014-01-01

Highlights: • ZnO nanospheres and nanowires were grown using ultrasound and thermal activation techniques. • The growth uses forced hydrolysis of zinc acetate in diethylene glycol (DEG). • A thermochemical model was developed based on thermodynamic equilibrium calculations. • We estimate species distribution in the bubble in temperature range from 5000 K to ambient. • We propose a new mechanism for ZnO growth assisted by ultrasound irradiation. - Abstract: A fast and green approach is proposed for the preparation of nanocrystalline zinc oxide (ZnO) via ultrasonic (US) irradiation in polyol medium. The process uses forced hydrolysis of zinc acetate in diethylene glycol (DEG). The protocol is compared to thermal activation under the same chemical environment. The activation method is found to be playing a critical role in the selective synthesis of morphologically distinct nanostructures. As compared to thermally activated conventional polyol process, (US) permits to considerably reduce reaction time as well as size of particles. In addition, the shape of these nanoparticles was changed from long nanowires to small nanospheres, indicating different reaction mechanisms. To explain this difference, a thermochemical model was developed based on thermodynamic equilibrium calculations. The model estimate species distribution in the bubble in temperature range from 5000 K to ambient simulating quenching process during bubble formation and collapse. Our results indicate the presence of high density of zinc atoms that could be responsible of a high density of nucleation as compared to thermal activation

Radiation-curable coatings containing reactive pigment dispersants

International Nuclear Information System (INIS)

Ansel, R.E.

1985-01-01

Liquid coating compositions adapted to be cured by exposure to penetrating radiation are disclosed in which a liquid vehicle of coating viscosity having an ethylenically unsaturated portion comprising one or more polyethylenically unsaturated materials adapted to cure on radiation exposure, pigment dispersed in the vehicle, and an ethylenically unsaturated radiation-curable dispersant containing a carboxyl group for wetting the pigment and assisting in the stable dipsersion of the pigment in the vehicle. This dispersant is a half amide or half ester of an ethylenically unsaturated polycarboxylic acid anhydride, such as maleic anhydride, with an organic compound having a molecular weight of from 100 to 4000 and which contains a single hydroxy group or a single amino group as the sole reactive group thereof

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

International Nuclear Information System (INIS)

Yousefi, Seyed Reza; Shemirani, Farzaneh

2010-01-01

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 μL 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 μg L -1 and 0.03 μg L -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.

Development of Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Drop for the Sensitive Determination of Trace Copper in Water and Beverage Samples by Flame Atomic Absorption Spectrometry

International Nuclear Information System (INIS)

Wu, Chunxia; Zhao, Bin; Li, Yingli; Wu, Qiuhua; Wang, Chun; Wang, Zhi

2011-01-01

A dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) has been developed as a new approach for the extraction of trace copper in water and beverage samples followed by the determination with flame atomic absorption spectrometry. In the DLLME-SFO, 8-hydroxy quinoline, 1-dodecanol, and methanol were used as chelating agent, extraction solvent and dispersive solvent, respectively. The experimental parameters related to the DLLME-SFO such as the type and volume of the extraction and dispersive solvent, extraction time, sample volume, the concentration of chelating agent and salt addition were investigated and optimized. Under the optimum conditions, the enrichment factor for copper was 122. The method was linear in the range from 0.5 to 300 ng mL -1 of copper in the samples with a correlation coefficient (r) of 0.9996 and a limit of detection of 0.1 ng mL -1 . The method was applied to the determination of copper in water and beverage samples. The recoveries for the spiked water and beverage samples at the copper concentration levels of 5.0 and 10.0 ng mL -1 were in the range between 92.0% and 108.0%. The relative standard deviations (RSD) varied from 3.0% to 5.6%

Determination of ten pyrethroids in various fruit juices: comparison of dispersive liquid-liquid microextraction sample preparation and QuEChERS method combined with dispersive liquid-liquid microextraction.

Science.gov (United States)

Zhang, Yaohai; Zhang, Xuelian; Jiao, Bining

2014-09-15

Dispersive liquid-liquid microextraction (DLLME) sample preparation and the quick, easy, cheap, effective, rugged and safe (QuEChERS) method combined with DLLME were developed and compared for the analysis of ten pyrethroids in various fruit juices using gas chromatography-electron capture detection (GC-ECD). QuEChERS-DLLME method has found its widespread applications to all the fruit juices including those samples with more complex matrices (orange, lemon, kiwi and mango) while DLLME was confined to the fruit juices with simpler matrices (apple, pear, grape and peach). The two methods provided acceptable recoveries and repeatability. In addition, the applicabilities of two methods were demonstrated with the real samples and further confirmed by gas chromatography-mass spectrometry (GC-MS). Copyright © 2014. Published by Elsevier Ltd.

Use of Dispersive Liquid-Liquid Microextraction and UV-Vis Spectrophotometry for the Determination of Cadmium in Water Samples

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J. Pérez-Outeiral

2014-01-01

Full Text Available A simple and inexpensive method for cadmium determination in water using dispersive liquid-liquid microextraction and ultraviolet-visible spectrophotometry was developed. In order to obtain the best experimental conditions, experimental design was applied. Calibration was made in the range of 10–100 μg/L, obtaining good linearity (R2 = 0.9947. The obtained limit of detection based on calibration curve was 8.5 μg/L. Intra- and interday repeatability were checked at two levels, obtaining relative standard deviation values from 9.0 to 13.3%. The enrichment factor had a value of 73. Metal interferences were also checked and tolerable limits were evaluated. Finally, the method was applied to cadmium determination in real spiked water samples. Therefore, the method showed potential applicability for cadmium determination in highly contaminated liquid samples.

A simple and sensitive vortex-assisted ionic liquid-dispersive microextraction and spectrophotometric determination of selenium in food samples.

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Bağda, Esra; Tüzen, Mustafa

2017-10-01

In the present study, a novel and eco-friendly vortex-assisted ionic liquid-based microextraction method was developed for the determination of selenium in food. The microextraction method is based on the liberation of iodine in the presence of selenium; the liberated iodine reacts with I - to form I 3 - . Anionic I 3 - reacts with cationic crystal violet dye, and the product is extracted into 1-hexyl-3-methylimidazolium hexafluorophosphate phase in the presence of Triton X-114. The proposed method is linear in the range of 2.0-70µgL -1 and has a detection limit of 9.8×10 -2 µgL -1 . Relative standard deviations were 3.67% and 2.89% for the five replicate measurements of 14 and 35µgL -1 Se(IV), respectively. The proposed method was successfully applied to different food samples (NIST SRM 2976 mussel tissue, pepper, ginger, wheat flour, red lentil, traditional soup, cornflour, cornstarch, and garlic) after microwave digestion. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

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Kulkarni, Vrushali M; Rathod, Virendra K

2014-03-01

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

Combination of flame atomic absorption spectrometry with ligandless-dispersive liquid- liquid microextraction for preconcentration and determination of trace amount of lead in water samples

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Y.M. Baghelani

2013-05-01

Full Text Available A new ligandless-dispersive liquid–liquid microextraction method has been developed for the separation and flame atomic absorption spectrometry determination of trace amount of lead(II ion. In the proposed approach 1,2-dicholorobenzene and ethanol were used as extraction and dispersive solvents. Factors influencing the extraction efficiency of lead, including the extraction and dispersive solvent type and volume, pH of sample solution, concentration of chloride and extraction time were studied. Under the optimal conditions, the calibration curve was linear in the range of 7.0–6000 ng mL−1 of lead with R2 = 0.9992 (n = 10 and detection limit based on three times the standard deviation of the blank (3Sb was 0.5 ng mL−1 in original solution. The relative standard deviation for eight replicate determinations of 1.0 mg mL-1 lead was ±1.6%. The high efficiency of dispersive liquid-liquid microextraction to carry out the determination of trace amounts of lead in complex matrices was demonstrated. The proposed method has been applied for determination of trace amounts of lead in water samples and satisfactory results were obtained. The accuracy was checked by analyzing a certified reference material from the National Institute of Standard and Technology, Trace elements in water (NIST CRM 1643e.

Simple and Rapid Dual-Dispersive Liquid-Liquid Microextraction as an Innovative Extraction Method for Uranium in Real Water Samples Prior to the Determination of Uranium by a Spectrophotometric Technique.

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Khan, Naeemullah; Tuzen, Mustafa; Kazi, Tasneem Gul

2017-11-01

An innovative, rapid, and simple dual-dispersive liquid-liquid microextraction (DDLL-ME) approach was used to extract uranium from real samples for the first time. The main objective of this study was to disperse extraction solvent by using an air-agitated syringe system to overcome matrix effects and avoid dispersion of hazardous dispersive organic solvents by using heat. The DDLL-ME method consisted of two dispersive liquid-liquid extraction steps with chloroform as the extracting solvent. Uranium formed complexes with 4-(2-thiazolylazo) resorcinol in the aqueous phase and was extracted in extracting solvent (chloroform) after the first dispersive liquid-liquid process. Uranium was then back-extracted in the acidic aqueous phase in a second dispersive liquid-liquid process. Finally, uranium was determined by a spectrophotometric detection technique. The variables that played a key role in the proposed method were studied and optimized. The LOD and sensitivity enhancement factor for uranium were found to be 0.60 µg/L and 45, respectively, under optimized conditions. Calibration graphs were found to be linear in the range of 5.0-600 µg/L. The RSD was 2.5%. Reliability of the proposed method was verified by analyzing certified reference material TM-28.3.

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

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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.

Determination of three estrogens and bisphenol A by functional ionic liquid dispersive liquid-phase microextraction coupled with ultra-high performance liquid chromatography and ultraviolet detection.

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Jiang, Yuehuang; Tang, Tingting; Cao, Zhen; Shi, Guoyue; Zhou, Tianshu

2015-06-01

A hydroxyl-functionalized ionic liquid, 1-hydroxyethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide, was employed in an improved dispersive liquid-phase microextraction method coupled with ultra high performance liquid chromatography for the enrichment and determination of three estrogens and bisphenol A in environmental water samples. The introduced hydroxyl group acted as the H-bond acceptor that dispersed the ionic liquid effectively in the aqueous phase without dispersive solvent or external force. Fourier transform infrared spectroscopy indicated that the hydroxyl group of the cation of the ionic liquid enhanced the combination of extractant and analytes through the formation of hydrogen bonds. The improvement of the extraction efficiency compared with that with the use of alkyl ionic liquid was proved by a comparison study. The main parameters including volume of extractant, temperature, pH, and extraction time were investigated. The calibration curves were linear in the range of 5.0-1000 μg/L for estrone, estradiol, and bisphenol A, and 10.0-1000 μg/L for estriol. The detection limits were in the range of 1.7-3.4 μg/L. The extraction efficiency was evaluated by enrichment factor that were between 85 and 129. The proposed method was proved to be simple, low cost, and environmentally friendly for the determination of the four endocrine disruptors in environmental water samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

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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.

Application of ultrasound-assisted emulsification microextraction for simultaneous determination of aminophenol isomers in human urine, hair dye, and water samples using high-performance liquid chromatography.

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Asghari, Alireza; Fazl-Karimi, Hamidreza; Barfi, Behruz; Rajabi, Maryam; Daneshfar, Ali

2014-08-01

Aminophenol isomers (2-, 3-, and 4-aminophenols) are typically classified as industrial pollutants with genotoxic and mutagenic effects due to their easy penetration through the skin and membranes of human, animals, and plants. In the present study, a simple and efficient ultrasound-assisted emulsification microextraction procedure coupled with high-performance liquid chromatography with ultraviolet detector was developed for preconcentration and determination of these compounds in human fluid and environmental water samples. Effective parameters (such as type and volume of extraction solvent, pH and ionic strength of sample, and ultrasonication and centrifuging time) were investigated and optimized. Under optimum conditions (including sample volume: 5 mL; extraction solvent: chloroform, 80 µL; pH: 6.5; without salt addition; ultrasonication: 3.5 min; and centrifuging time: 3 min, 5000 rpm min(-1)), the enrichment factors and limits of detection were ranged from 42 to 51 and 0.028 to 0.112 µg mL(-1), respectively. Once optimized, analytical performance of the method was studied in terms of linearity (0.085-157 µg mL(-1), r (2) > 0.998), accuracy (recovery = 88.6- 101.7%), and precision (repeatability: intraday precision water samples. © The Author(s) 2014.

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction for the determination of sulfonamides in animal tissues using high-performance liquid chromatography.

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Wang, Zhibing; He, Mengyu; Jiang, Chunzhu; Zhang, Fengqing; Du, Shanshan; Feng, Wennan; Zhang, Hanqi

2015-12-01

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction was developed and applied to the extraction of some sulfonamides, including sulfamerazine, sulfamethazine, sulfathiazole, sulfachloropyridazine, sulfadoxine, sulfisoxazole, and sulfaphenazole, in animal tissues. High-performance liquid chromatography was applied to the separation and determination of the target analytes. The solid sample was directly treated by matrix solid-phase dispersion and the eluate obtained was treated by homogeneous ionic liquid microextraction. The ionic liquid was used as the extraction solvent in this method, which may result in the improvement of the recoveries of the target analytes. To avoid using organic solvent and reduce environmental pollution, water was used as the elution solvent of matrix solid-phase dispersion. The effects of the experimental parameters on recoveries, including the type and volume of ionic liquid, type of dispersant, ratio of sample to dispersant, pH value of elution solvent, volume of elution solvent, amount of salt in eluate, amount of ion-pairing agent (NH4 PF6 ), and centrifuging time, were evaluated. When the present method was applied to the analysis of animal tissues, the recoveries of the analytes ranged from 85.4 to 118.0%, and the relative standard deviations were lower than 9.30%. The detection limits for the analytes were 4.3-13.4 μg/kg. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ionic Liquid Dispersive Liquid-Liquid Microextraction Method for the Determination of Irinotecan, an Anticancer Drug, in Water and Urine Samples Using UV-Vis Spectrophotometry.

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Uysal, Deniz; Karadaş, Cennet; Kara, Derya

2017-05-01

A new, simple, efficient, and environmentally friendly ionic liquid dispersive liquid-liquid microextraction method was developed for the determination of irinotecan, an anticancer drug, in water and urine samples using UV-Vis spectrophotometry. The ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate was used as the extraction solvent, and ethanol was used as the disperser solvent. The main parameters affecting the extraction efficiency, including sample pH, volume of the ionic liquid, choice of the dispersive solvent and its volume, concentration of NaCl, and extraction and centrifugation times, were investigated and optimized. The effect of interfering species on the recovery of irinotecan was also examined. Under optimal conditions, the LOD (3σ) was 48.7 μg/L without any preconcentration. Because the urine sample was diluted 10-fold, the LOD for urine would be 487 μg/L. However, this could be improved 16-fold if preconcentration using a 40 mL aliquot of the sample is used. The proposed method was successfully applied to the determination of irinotecan in tap water, river water, and urine samples spiked with 10.20 mg/L for the water samples and 8.32 mg/L for the urine sample. The average recovery values of irinotecan determined were 99.1% for tap water, 109.4% for river water, and 96.1% for urine.

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

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Fazelirad, Hamid; Taher, Mohammad Ali

2013-01-15

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

Application of dispersive liquid-liquid microextraction for the preconcentration of eight parabens in real samples and their determination by high-performance liquid chromatography.

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Shen, Xiong; Liang, Jian; Zheng, Luxia; Lv, Qianzhou; Wang, Hong

2017-11-01

A simple and sensitive method for the simultaneous determination of eight parabens in human plasma and urine samples was developed. The samples were preconcentrated using dispersive liquid-liquid microextraction based on the solidification of floating organic drops and determined by high-performance liquid chromatography with ultraviolet detection. The influence of variables affecting the extraction efficiency was investigated and optimized using Placket-Burman design and Box-Behnken design. The optimized values were: 58 μL of 1-decanol (as extraction solvent), 0.65 mL methanol (as disperser solvent), 1.5% w/v NaCl in 5.0 mL of sample solution, pH 10.6, and 4.0 min centrifugation at 4000 rpm. The extract was injected into the high-performance liquid chromatography system for analysis. Under the optimum conditions, the linear ranges for eight parabens in plasma and urine were 1.0-1000 ng/mL, with correlation coefficients above 0.994. The limit of detection was 0.2-0.4 and 0.1-0.4 ng/mL for plasma and urine samples, respectively. Relative recoveries were between 80.3 and 110.7%, while relative standard deviations were less than 5.4%. Finally, the method was applied to analyze the parabens in 98 patients of primary breast cancer. Results showed that parabens existed widely, at least one paraben detected in 96.9% (95/98) of plasma samples and 98.0% (96/98) of urine samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

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

2015-12-24

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

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

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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.

Surface modification and characterization for dispersion stability of inorganic nanometer-scaled particles in liquid media

International Nuclear Information System (INIS)

Kamiya, Hidehiro; Iijima, Motoyuki

2010-01-01

Inorganic nanoparticles are indispensable for science and technology as materials, pigments and cosmetics products. Improving the dispersion stability of nanoparticles in various liquids is essential for those applications. In this review, we discuss why it is difficult to control the stability of nanoparticles in liquids. We also overview the role of surface interaction between nanoparticles in their dispersion and characterization, e.g. by colloid probe atomic force microscopy (CP-AFM). Two types of surface modification concepts, post-synthesis and in situ modification, were investigated in many previous studies. Here, we focus on post-synthesis modification using adsorption of various kinds of polymer dispersants and surfactants on the particle surface, as well as surface chemical reactions of silane coupling agents. We discuss CP-AFM as a technique to analyze the surface interaction between nanoparticles and the effect of surface modification on the nanoparticle dispersion in liquids. (topical review)

Surface modification and characterization for dispersion stability of inorganic nanometer-scaled particles in liquid media

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Hidehiro Kamiya and Motoyuki Iijima

2010-01-01

Full Text Available Inorganic nanoparticles are indispensable for science and technology as materials, pigments and cosmetics products. Improving the dispersion stability of nanoparticles in various liquids is essential for those applications. In this review, we discuss why it is difficult to control the stability of nanoparticles in liquids. We also overview the role of surface interaction between nanoparticles in their dispersion and characterization, e.g. by colloid probe atomic force microscopy (CP-AFM. Two types of surface modification concepts, post-synthesis and in situ modification, were investigated in many previous studies. Here, we focus on post-synthesis modification using adsorption of various kinds of polymer dispersants and surfactants on the particle surface, as well as surface chemical reactions of silane coupling agents. We discuss CP-AFM as a technique to analyze the surface interaction between nanoparticles and the effect of surface modification on the nanoparticle dispersion in liquids.

Phyocyanin extraction from microalgae Spirulina platensis assisted by ultrasound irradiation: effect of time and temperature

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Hadiyanto

2016-08-01

Full Text Available This research was aimed to extract phycocyanin from microalgae Spirulina platensis using an extraction assisted by ultrasound irradiation. The extraction was conducted by using variable of extraction time, temperature and ultrasound frequency, while ethanol was used as solvent. The results show that the yield of phycocyanin extract was 15.97% at constant frequency of 42 kHz and 11.24% at constant frequency of 28 kHz, while the soxhlet extraction method obtained yield at 11.13%. The ultrasound could reduce the extraction time from 4 hrs (conventional to 20 minutes, while the optimum temperature of extraction was found at 55°C.

A highly selective dispersive liquid-liquid microextraction approach based on the unique fluorous affinity for the extraction and detection of per- and polyfluoroalkyl substances coupled with high performance liquid chromatography tandem-mass spectrometry.

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Wang, Juan; Shi, Yali; Cai, Yaqi

2018-04-06

In the present study, a highly selective fluorous affinity-based dispersive liquid-liquid microextraction (DLLME) technique was developed for the extraction and analysis of per- and polyfluoroalkyl substances (PFASs) followed by high performance liquid chromatography tandem-mass spectrometry. Perfluoro-tert-butanol with multiple C-F bonds was chosen as the extraction solvent, which was injected into the aqueous samples with a dispersive solvent (acetonitrile) in a 120:800 (μL, v/v) mixture for PFASs enrichment. The fluorous affinity-based extraction mechanism was confirmed by the significantly higher extraction recoveries for PFASs containing multiple fluorine atoms than those for compounds with fewer or no fluorine atoms. The extraction recoveries of medium and long-chain PFASs (CF 2  > 5) exceeded 70%, except perfluoroheptanoic acid, while those of short-chain PFASs were lower than 50%, implying that the proposed DLLME may not be suitable for their extraction due to weak fluorous affinity. This highly fluoroselective DLLME technique can greatly decrease the matrix effect that occurs in mass spectrometry detection when applied to the analysis of urine samples. Under the optimum conditions, the relative recoveries of PFASs with CF 2  > 5 ranged from 80.6-121.4% for tap water, river water and urine samples spiked with concentrations of 10, 50 and 100 ng/L. The method limits of quantification for PFASs in water and urine samples were in the range of 0.6-8.7 ng/L. Furthermore, comparable concentrations of PFASs were obtained via DLLME and solid-phase extraction, confirming that the developed DLLME technique is a promising method for the extraction of PFASs in real samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Application of dispersive Liquid-Liquid microextraction based on solidification of floating organic droplet multi-residue method for the simultaneous determination of polychlorinated biphenyls, organochlorine, and pyrethroid pesticides in aqueous sample

International Nuclear Information System (INIS)

Zuo, Mei; Li, Man-Liang; Cheng, Jing; Matsadiq, Guzalnur; Liu, Lu; Zhang, Miao

2012-01-01

Dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) technique was successfully applied for simultaneous assay of eight polychlorinated biphenyls, two organochlorine, and four pyrethroid pesticides multi-residue in aqueous samples by using GC-electron capture detection. The effects of various parameters such as kind of extractant and dispersant and volume of them, extraction time, effect of salt addition, and pH were optimized. As a result, 5.0 μL 1-dodecanol was chosen as extraction solvent, 600 μL methanol were used as dispersive solvent without salt addition, pH was adjusted to 7. Under the optimized conditions, the limits of detection (LOD) were ranged from 1.4 to 8.3 ng L -1 . Satisfactory linear range was observed from 5.0 to 2000 ng L -1 with correlation coefficient better than 0.9909. Good precisions were also acquired with RSD better than 13.6% for all target analytes. The enrichment factors of the method were ranged from 786 to 1427. The method can be successfully applied to simultaneous separation and determination of three class residues in real water samples and good recoveries were obtained ranging from 76 to 130, 73 to 129, and 78 to 130% for tap water, lake water, and industrial waste water, respectively. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Spatial and temporal profile of cisplatin delivery by ultrasound-assisted intravesical chemotherapy in a bladder cancer model.

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Noboru Sasaki

Full Text Available Non-muscle invasive bladder cancer is one of the most common tumors of the urinary tract. Despite the current multimodal therapy, recurrence and progression of disease have been challenging problems. We hereby introduced a new approach, ultrasound-assisted intravesical chemotherapy, intravesical instillation of chemotherapeutic agents and microbubbles followed by ultrasound exposure. We investigated the feasibility of the treatment for non-muscle invasive bladder cancer. In order to evaluate intracellular delivery and cytotoxic effect as a function to the thickness, we performed all experiments using a bladder cancer mimicking 3D culture model. Ultrasound-triggered microbubble cavitation increased both the intracellular platinum concentration and the cytotoxic effect of cisplatin at the thickness of 70 and 122 μm of the culture model. The duration of enhanced cytotoxic effect of cisplatin by ultrasound-triggered microbubble cavitation was approximately 1 hr. Based on the distance and duration of delivery, we further tested the feasibility of repetition of the treatment. Triple treatment increased the effective distance by 1.6-fold. Our results clearly showed spatial and temporal profile of delivery by ultrasound-triggered microbubble cavitation in a tumor-mimicking structure. Furthermore, we demonstrated that the increase in intracellular concentration results in the enhancement of the cytotoxic effect in a structure with the certain thickness. Repetition of ultrasound exposure would be treatment of choice in future clinical application. Our results suggest ultrasound-triggered microbubble cavitation can be repeatable and is promising for the local control of non-muscle invasive bladder cancer.

Ultrasound shock wave generator with one-bit time reversal in a dispersive medium, application to lithotripsy

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Montaldo, Gabriel; Roux, Philippe; Derode, Arnaud; Negreira, Carlos; Fink, Mathias

2002-02-01

The building of high-power ultrasonic sources from piezoelectric ceramics is limited by the maximum voltage that the ceramics can endure. We have conceived a device that uses a small number of piezoelectric transducers fastened to a cylindrical metallic waveguide. A one-bit time- reversal operation transforms the long-lasting low-level dispersed wave forms into a sharp pulse, thus taking advantage of dispersion to generate high-power ultrasound. The pressure amplitude that is generated at the focus is found to be 15 times greater than that achieved with comparable standard techniques. Applications to lithotripsy are discussed and the destructive efficiency of the system is demonstrated on pieces of chalk.

Spectrophotometric determination of mercury in water samples after preconcentration using dispersive liquid-liquid microextraction.

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Lemos, Valfredo Azevedo; dos Santos, Liz Oliveira; Silva, Eldevan dos Santos; Vieira, Emanuel Vitor dos Santos

2012-01-01

A simple method for the determination of mercury in water samples after preconcentration using dispersive liquid-liquid microextraction is described. The procedure is based on the extraction of mercury in the form of a complex and its subsequent determination by spectrophotometry. The complex is formed between Hg(II) and 2-(2-benzothiazolylazo)-p-cresol. The detection at 650 nm is performed directly in the metal-rich phase, which is spread on a triacetylcellulose membrane. The method eliminates the need to use a cuvet or large quantities of samples and reagents. The parameters that influence the preconcentration were studied, and the analytical characteristics were determined. The enrichment factor and the consumptive index for this method were 64 and 0.16 mL, respectively. The LOD (3.3 microg/L) and LOQ (11.1 microg/L) were also determined. The accuracy of the method was tested by the determination of mercury in certified reference materials BCR 397 (Human Hair) and SRM 2781 (Domestic Sludge). The method was applied to the determination of mercury in samples of drinking water, sea water, and river water.

Quantitative Analysis of Piroxicam Using Temperature-Controlled Ionic Liquid Dispersive Liquid Phase Microextraction Followed By Stopped-Flow Injection Spectrofluorimetry

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Mohammad Reza Ganjali

2013-07-01

Full Text Available Background:Piroxicam (PXM belongs to the wide class of non-steroidal anti-inflammatory drugs (NSAIDs. PXM has been widely applied in the treatment of rheumatoid arthritis, gonarthrosis, osteoarthritis, backaches, neuralgia, mialgia. In the presented work, a green and benign sample pretreatment method called temperature-controlled ionic liquid dispersive liquid phase microextraction (TCIL-DLPME was followed with stopped-flow injection spectrofluorimetry (SFIS for quantitation of PXM in pharmaceutical formulations and biological samples.Methods:Temperature-controlled ionic liquid dispersive liquid phase microextraction (TCIL-DLPME was applied as an environmentally friendly sample enrichment method to extract and isolate PXM prior to quantitation. Dispersion of 1-hexyl-3-methylimidazolium hexafluorophosphate ([Hmim][PF6] ionic liquid (IL through the sample aqueous solution was performed by applying a relatively high temperature. PXM was extracted into the extractor, and after phase separation, PXM in the final solution was determined by stopped-flow injection spectrofluorimetry (SFIS.Results and Major Conclusion:Different factors affecting the designed method such as IL amount, diluting agent, pH and temperature were investigated in details and optimized. The method provided a linear dynamic range of 0.2-150 μg l-1, a limit of detection (LOD of 0.046 μg l-1 and a relative standard deviation (RSD of 3.1%. Furthermore, in order to demonstrate the analytical applicability of the recommended method, it was applied for quantitation of PXM in real samples.

Preparation of magnetic Ni@graphene nanocomposites and efficient removal organic dye under assistance of ultrasound

International Nuclear Information System (INIS)

Zhao, Chuang; Guo, Jianhui; Yang, Qing; Tong, Lei; Zhang, Jingwei; Zhang, Jiwei; Gong, Chunhong; Zhou, Jingfang; Zhang, Zhijun

2015-01-01

Graphical abstract: Reduced graphene oxide/Ni microspheres, being prepared under ultrasound conditions, exhibit a better removal efficiency to decolorize RhB with ultrasonic-assisted decolorization process. - Highlights: • One-step synthesis of Ni@graphene microspheres under ultrasound conditions. • During the ultrasonic process, graphene oxide was reduced and Ni nanoparticles were formed and anchored on graphene sheets. • The products exhibit excellent performance for fast and efficient removal of dye contaminants. • The nanocomposites can be easily separated from solution by a magnet. - Abstract: In this article, we report a facile one-step synthesis of Ni@graphene nanocomposite microspheres (NGs) in hydrazine hydrate solution under ultrasound conditions. During the ultrasonic process, graphene oxide (GO) was reduced effectively under mild conditions and Ni nanoparticles were simultaneously formed and anchored on graphene sheets, which act as spacers to keep the neighboring sheets separated. The target products exhibit excellent performance for fast and efficient removal of dye contaminants, rhodamine B (RhB) in aqueous solution, under assistance of ultrasound. Finally, the nanocomposites can be easily separated from solution by a magnet. Furthermore, higher content of graphene can be produced under sonication, which facilitates faster and more efficient removal of organic contaminates in the solution. The nanocomposites were also characterized by scanning electron microscopy, Raman spectroscopy, Fourier transformed infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray powder diffraction and thermogravimetric analysis.

Preparation of magnetic Ni@graphene nanocomposites and efficient removal organic dye under assistance of ultrasound

Energy Technology Data Exchange (ETDEWEB)

Zhao, Chuang; Guo, Jianhui; Yang, Qing; Tong, Lei [Key Laboratory of Ministry of Education for Special Functional Materials, Henan University, Kaifeng 475004 (China); Zhang, Jingwei, E-mail: jwzhang@henu.edu.cn [Key Laboratory of Ministry of Education for Special Functional Materials, Henan University, Kaifeng 475004 (China); Ian Wark Research Institute, University of South Australia, Mawson Lakes, SA 5095 (Australia); Zhang, Jiwei [Key Laboratory of Ministry of Education for Special Functional Materials, Henan University, Kaifeng 475004 (China); Gong, Chunhong [College of Chemistry and Chemical Engineering, Henan University, Kaifeng 475004 (China); Ian Wark Research Institute, University of South Australia, Mawson Lakes, SA 5095 (Australia); Zhou, Jingfang, E-mail: jingfang.zhou@unisa.edu.au [Ian Wark Research Institute, University of South Australia, Mawson Lakes, SA 5095 (Australia); Zhang, Zhijun [Key Laboratory of Ministry of Education for Special Functional Materials, Henan University, Kaifeng 475004 (China)

2015-12-01

Graphical abstract: Reduced graphene oxide/Ni microspheres, being prepared under ultrasound conditions, exhibit a better removal efficiency to decolorize RhB with ultrasonic-assisted decolorization process. - Highlights: • One-step synthesis of Ni@graphene microspheres under ultrasound conditions. • During the ultrasonic process, graphene oxide was reduced and Ni nanoparticles were formed and anchored on graphene sheets. • The products exhibit excellent performance for fast and efficient removal of dye contaminants. • The nanocomposites can be easily separated from solution by a magnet. - Abstract: In this article, we report a facile one-step synthesis of Ni@graphene nanocomposite microspheres (NGs) in hydrazine hydrate solution under ultrasound conditions. During the ultrasonic process, graphene oxide (GO) was reduced effectively under mild conditions and Ni nanoparticles were simultaneously formed and anchored on graphene sheets, which act as spacers to keep the neighboring sheets separated. The target products exhibit excellent performance for fast and efficient removal of dye contaminants, rhodamine B (RhB) in aqueous solution, under assistance of ultrasound. Finally, the nanocomposites can be easily separated from solution by a magnet. Furthermore, higher content of graphene can be produced under sonication, which facilitates faster and more efficient removal of organic contaminates in the solution. The nanocomposites were also characterized by scanning electron microscopy, Raman spectroscopy, Fourier transformed infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray powder diffraction and thermogravimetric analysis.

Stabilization of liquid crystal dispersions with acrylamide copolymers

Energy Technology Data Exchange (ETDEWEB)

Park, S.J.; Kim, M.H.; Lee, J.R. [Korea Research Institute of Chemical Technology, Taejon (Korea, Republic of)

1999-03-01

The effects of hydrophobic moieties(styrene and methyl methacrylate) on the stability of a liquid crystal(LC, E-7)-in-water dispersion stabilized by copolymers of hydrophilic acrylamide with hydrophobic monomers have been studied in terms of nematic curvilinear aligned phase(NCAP) system. It was observed that the preferential adsorption hydrophobic moieties onto LC droplet surface resulted in steric stabilization of the dispersion, due to increasing the interfacial tension of LC and reducing the LC droplet size. According to the interfacial tension, coalescence time, and sedimented layer thickness measurements, it was proposed that the presence of hydrophobic moieties allows to form the apolar microenvironment in the round of LC droplet and finally reduces the anchoring effect between LC and the polymeric wall. 16 refs., 10 figs.

Antiwear performance of ionic liquid+graphene dispersions with anomalous viscosity-temperature behavior

OpenAIRE

Pamies Porras, Ramón Francisco; Arias Pardilla, Joaquín; Espinosa Rodríguez, Tulia; Carrión Vilches, Francisco José; Bermúdez Olivares, María Dolores; Sanes Molina, José; Avilés González, María Dolores

2018-01-01

New dispersions of few-layers graphene (G) in 1-ethyl-3-methylimidazolium ([EMIM]) ionic liquids (ILs) with dicyanamide ([DCA]) or bis(trifluoromethylsulfonyl)imide ([TFSI]) anions have been obtained by mechanical mixing and sonication. IL+0.5 wt% G dispersions show constant viscosity values from 357K (for IL = [EMIM][DCA]) or from 385K (for IL = [EMIM][TFSI]) to 393K. IL + G dispersions with G > 0.5 wt% show linear viscosity increases with increasing temperature, from 306K (for [EMIM][DCA]+1...

Dispersive liquid-liquid microextraction coupled with digital image colorimetric analysis for detection of total iron in water and food samples.

Science.gov (United States)

Peng, Bo; Chen, Guorong; Li, Kai; Zhou, Min; Zhang, Ji; Zhao, Shengguo

2017-09-01

A simple and low cost assay for total iron in various samples based on dispersive liquid-liquid microextraction (DLLME) coupled with digital scanning image analysis was proposed. Orthogonal experiment design was utilized to optimize the amount of extraction solvent and disperser solvent, O-phenanthroline concentration and buffer pH. Under the optimum conditions, the calibration curve was linear over the range of 0.047-1.0μgmL -1 (R 2 >0.99) of iron. The limit of detection (LOD) for iron was 14.1μgL -1 and limit of quantification (LOQ) was 46.5μgL -1 . The relative standard deviations for seven replicate determinations of 0.5μgmL -1 of iron was 3.75%. The method was successfully applied for analysis of total iron in water and food samples without using any spectral instrument and it could have a potential industrial impact in developing fast and portable devices to analyze the iron content in water and certain foods. Copyright © 2017 Elsevier Ltd. All rights reserved.

Rapid determination of some psychotropic drugs in complex matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

Science.gov (United States)

Asghari, Alireza; Fahimi, Ebrahim; Bazregar, Mohammad; Rajabi, Maryam; Boutorabi, Leila

2017-05-01

Simple and rapid determinations of some psychotropic drugs in some pharmaceutical wastewater and human plasma samples were successfully accomplished via the tandem dispersive liquid-liquid microextraction combined with high performance liquid chromatography-ultraviolet detection (TDLLME-HPLC-UV). TDLLME of the three psychotropic drugs clozapine, chlorpromazine, and thioridazine was easily performed through two consecutive dispersive liquid-liquid microextractions. By performing this convenient method, proper sample preconcentrations and clean-ups were achieved in just about 7min. In order to achieve the best extraction efficiency, the effective parameters involved were optimized. The optimal experimental conditions consisted of 100μL of CCl 4 (as the extraction organic solvent), and the pH values of 13 and 2 for the donor and acceptor phases, respectively. Under these optimum experimental conditions, the proposed TDLLME-HPLC-UV technique provided a good linearity in the range of 5-3000ngmL -1 for the three psychotropic drugs with the correlation of determinations (R 2 s) higher than 0.996. The limits of quantification (LOQs) and limits of detection (LODs) obtained were 5.0ngmL -1 and 1.0-1.5ngmL -1 , respectively. Also the proper enrichment factors (EFs) of 96, 99, and 88 for clozapine, chlorpromazine, and thioridazine, respectively, and good extraction repeatabilities (relative standard deviations below 9.3%, n=5) were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

High transmittance optical films based on quantum dot doped nanoscale polymer dispersed liquid crystals

Science.gov (United States)

Gandhi, Sahil Sandesh; Chien, Liang-Chy

2016-04-01

We propose a simple way to fabricate highly transparent nanoscale polymer dispersed liquid crystal (nano-PDLC) films between glass substrates and investigate their incident angle dependent optical transmittance properties with both collimated and Lambertian intensity distribution light sources. We also demonstrate that doping nano-PDLC films with 0.1% InP/ZnS core/shell quantum dots (QD) results in a higher optical transmittance. This work lays the foundation for such nanostructured composites to potentially serve as roll-to-roll coatable light extraction or brightness enhancement films in emissive display applications, superior to complex nanocorrugation techniques proposed in the past.

Ultrasound exfoliation of inorganic analogues of graphene.

Science.gov (United States)

Stengl, Václav; Henych, Jiří; Slušná, Michaela; Ecorchard, Petra

2014-04-05

High-intensity ultrasound exfoliation of a bulk-layered material is an attractive route for large-scale preparation of monolayers. The monolayer slices could potentially be prepared with a high yield (up to 100%) in a few minutes. Exfoliation of natural minerals (such as tungstenite and molybdenite) or bulk synthetic materials (including hexagonal boron nitride (h-BN), hexagonal boron carbon nitride (h-BCN), and graphitic carbon nitride (g-C3N4)) in liquids leads to the breakdown of the 3D graphitic structure into a 2D structure; the efficiency of this process is highly dependent upon the physical effects of the ultrasound. Atomic force microscopy (AFM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED) were employed to verify the quality of the exfoliation. Herein, this new method of exfoliation with ultrasound assistance for application to mono- and bilayered materials in hydrophobic and hydrophilic environments is presented.

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

Science.gov (United States)

Sadeghi, Susan; Ashoori, Vahid

2017-10-01

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

Combination of dispersive liquid-liquid microextraction with flame atomic absorption spectrometry using microsample introduction for determination of lead in water samples.

Science.gov (United States)

Naseri, Mohammad Taghi; Hemmatkhah, Payam; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub

2008-03-03

The dispersive liquid-liquid microextraction (DLLME) was combined with the flame atomic absorption spectrometry (FAAS) for determination of lead in the water samples. Diethyldithiophosphoric acid (DDTP), carbon tetrachloride and methanol were used as chelating agent, extraction solvent and disperser solvent, respectively. A new FAAS sample introduction system was employed for the microvolume nebulization of the non-flammable chlorinated organic extracts. Injection of 20 microL volumes of the organic extract into an air-acetylene flame provided very sensitive spike-like and reproducible signals. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters include extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH and amount of the chelating agent. Under the optimized conditions, the enrichment factor of 450 was obtained from a sample volume of 25.0 mL. The enhancement factor, calculated as the ratio of the slopes of the calibration graphs with and without preconcentration, which was about 1000. The calibration graph was linear in the range of 1-70 microgL(-1) with a detection limit of 0.5 microgL(-1). The relative standard deviation (R.S.D.) for seven replicate measurements of 5.0 and 50 microgL(-1) of lead were 3.8 and 2.0%, respectively. The relative recoveries of lead in tap, well, river and seawater samples at the spiking level of 20 microgL(-1) ranged from 93.8 to 106.2%. The characteristics of the proposed method were compared with those of the liquid-liquid extraction (LLE), cloud point extraction (CPE), on-line and off-line solid-phase extraction (SPE) as well as co-precipitation, based on bibliographic data. Operation simplicity, rapidity, low cost, high enrichment factor, good repeatability, and low consumption of the extraction solvent at a microliter level are the main advantages of the proposed method.

Synergistic effects of non-thermal plasma-assisted catalyst and ultrasound on toluene removal.

Science.gov (United States)

Sun, Yongli; Zhou, Libo; Zhang, Luhong; Sui, Hong

2012-01-01

A wire-mesh catalyst coated by La0.8Sr0.2MnO3 was combined with a dielectric barrier discharge (DBD) reactor for toluene removal at atmospheric pressure. It was found that toluene removal efficiency and carbon dioxide selectivity were enhanced in the catalytic packed-bed reactor. In addition, ozone and nitrogen monoxide from the gas effluent byproducts decreased. This is the first time that ultrasound combined with plasma has been used for toluene removal. A synergistic effect on toluene removal was observed in the plasma-assisted ultrasound system. At the same time, the system increased toluene conversion and reduced ozone emission.

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

Science.gov (United States)

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

2010-02-01

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

Combination of solvent extractants for dispersive liquid-liquid microextraction of fungicides from water and fruit samples by liquid chromatography with tandem mass spectrometry.

Science.gov (United States)

Pastor-Belda, Marta; Garrido, Isabel; Campillo, Natalia; Viñas, Pilar; Hellín, Pilar; Flores, Pilar; Fenoll, José

2017-10-15

A multiresidue method was developed to determine twenty-five fungicides belonging to three different chemical families, oxazoles, strobilurins and triazoles, in water and fruit samples, using dispersive liquid-liquid microextraction (DLLME) and liquid chromatography/tandem mass spectrometry (LC-MS 2 ). Solid-liquid extraction with acetonitrile was used for the analysis in fruits, the extract being used as dispersant solvent in DLLME. Since some of the analytes showed high affinity for chloroform and the others were more efficiently extracted with undecanol, a mixture of both solvents was used as extractant in DLLME. After evaporation of CHCl 3 , the enriched phase was analyzed. Enrichment factors in the 23-119 and 12-60 ranges were obtained for waters and fruits, respectively. The approach was most sensitive for metominostrobin with limits of quantification of 1ngL -1 and 5ngkg -1 in waters and fruits, respectively, while a similar sensitivity was attained for tebuconazole in fruits. Recoveries of the fungicides varied between 86 and 116%. Copyright © 2017 Elsevier Ltd. All rights reserved.

Wire-mesh and ultrasound techniques applied for the characterization of gas-liquid slug flow

Energy Technology Data Exchange (ETDEWEB)

Ofuchi, Cesar Y.; Sieczkowski, Wytila Chagas; Neves Junior, Flavio; Arruda, Lucia V.R.; Morales, Rigoberto E.M.; Amaral, Carlos E.F.; Silva, Marco J. da [Federal University of Technology of Parana, Curitiba, PR (Brazil)], e-mails: ofuchi@utfpr.edu.br, wytila@utfpr.edu.br, neves@utfpr.edu.br, lvrarruda@utfpr.edu.br, rmorales@utfpr.edu.br, camaral@utfpr.edu.br, mdasilva@utfpr.edu.br

2010-07-01

Gas-liquid two-phase flows are found in a broad range of industrial applications, such as chemical, petrochemical and nuclear industries and quite often determine the efficiency and safety of process and plants. Several experimental techniques have been proposed and applied to measure and quantify two-phase flows so far. In this experimental study the wire-mesh sensor and an ultrasound technique are used and comparatively evaluated to study two-phase slug flows in horizontal pipes. The wire-mesh is an imaging technique and thus appropriated for scientific studies while ultrasound-based technique is robust and non-intrusive and hence well suited for industrial applications. Based on the measured raw data it is possible to extract some specific slug flow parameters of interest such as mean void fraction and characteristic frequency. The experiments were performed in the Thermal Sciences Laboratory (LACIT) at UTFPR, Brazil, in which an experimental two-phase flow loop is available. The experimental flow loop comprises a horizontal acrylic pipe of 26 mm diameter and 9 m length. Water and air were used to produce the two phase flow under controlled conditions. The results show good agreement between the techniques. (author)

Guanidinium ionic liquid-based surfactants as low cytotoxic extractants: Analytical performance in an in-situ dispersive liquid-liquid microextraction method for determining personal care products.

Science.gov (United States)

Pacheco-Fernández, Idaira; Pino, Verónica; Ayala, Juan H; Afonso, Ana M

2017-05-01

The IL-based surfactant octylguanidinium chloride (C 8 Gu-Cl) was designed and synthetized with the purpose of obtaining a less harmful surfactant: containing guanidinium as core cation and a relatively short alkyl chain. Its interfacial and aggregation behavior was evaluated through conductivity and fluorescence measurements, presenting a critical micelle concentration value of 42.5 and 44.6mmolL -1 , respectively. Cytotoxicity studies were carried out with C 8 Gu-Cl and other IL-based and conventional surfactants, specifically the analogue 1-octyl-3-methylimidazolium chloride (C 8 MIm-Cl), and other imidazolium- (C 16 MIm-Br) and pyridinium- (C 16 Py-Cl) based surfactants, together with the conventional cationic CTAB and the conventional anionic SDS. From these studies, C 8 Gu-Cl was the only one to achieve the classification of low cytotoxicity. An in situ dispersive liquid-liquid microextraction (DLLME) method based on transforming the water-soluble C 8 Gu-Cl IL-based surfactant into a water-insoluble IL microdroplet via a simple metathesis reaction was then selected as the extraction/preconcentration method for a group of 6 personal care products (PCPs) present in cosmetic samples. The method was carried out in combination with high-performance liquid chromatography (HPLC) and diode array detection (DAD). The method was properly optimized, requiring the use of only 30μL of C 8 Gu-Cl for 10mL of aqueous sample with a NaCl content of 8% (w/v) to adjust the ionic strength and pH value of 5. The metathesis reaction required the addition of the anion exchange reagent (bis[(trifluoromethyl)sulfonyl]imide - 1:1 molar ratio), followed by vortex and centrifugation, and dilution of the final microdroplet up to 60μL with acetonitrile before the injection in the HPLC-DAD system. The optimum in situ DLLME-HPLC-DAD method takes ∼10min for the extraction step and ∼22min for the chromatographic separation, with analytical features of low detection limits: down to 0.4�

Time evolution of the drop size distribution for liquid-liquid dispersion in an agitated tank

Czech Academy of Sciences Publication Activity Database

Šulc, R.; Kysela, Bohuš; Ditl, P.

2018-01-01

Roč. 72, č. 3 (2018), s. 543-553 ISSN 0366-6352 R&D Projects: GA ČR GA16-20175S Institutional support: RVO:67985874 Keywords : liquid–liquid dispersion * drop breakup * drop size distribution * time evolution Subject RIV: BK - Fluid Dynamics Impact factor: 1.258, year: 2016

Ultrasound-assisted surfactant-enhanced emulsification microextraction with solidification of floating organic droplet followed by high performance liquid chromatography for the determination of strobilurin fungicides in fruit juice samples.

Science.gov (United States)

Liang, Pei; Liu, Guojiao; Wang, Fang; Wang, Wanting

2013-05-01

A novel method, ultrasound-assisted surfactant-enhanced emulsification microextraction with solidification of floating organic droplet (UASEME-SFOD), has been developed for the extraction of four strobilurin fungicides (kresoxim-methyl, picoxystrobin, pyraclostrobin and trifloxystrobin) in fruit juices. In the UASEME-SFOD technique, Tween 80 was used as emulsifier, and 1-undecanol was used as extraction solvent without using any organic dispersive solvent. Several parameters that affect the extraction efficiency, such as the kind and volume of extraction solvent, the type and concentration of the surfactant, extraction time, extraction temperature and salt addition were investigated and optimized. Under the optimum extraction condition, the method yields a linear calibration curve in the concentration range from 5 to 10,000 ng mL(-1) for the targeted analytes with the correlation coefficient ranging from 0.9991 to 0.9998. The enrichment factors were in the range between 95 and 135, and the limits of detection of the method were 2-4 ng mL(-1). The fruit juice 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 82.6-97.5%. Copyright © 2013 Elsevier B.V. All rights reserved.

Ultrasound-assisted extraction of three bufadienolides from Chinese medicine ChanSu.

Science.gov (United States)

Sun, Yinshi; Bi, Jianjie; Zhang, Li; Ye, Baoxing

2012-11-01

In this study, the application of ultrasound-assisted extraction (UAE) method was shown to be more efficient in extracting anti-tumor bufadienolides (bufalin, cinobufagin and resibufogenin) from important animal medicine of ChanSu than the maceration extraction (ME) and soxhlet extraction (SE) method. The effects of ultrasonic variables including extraction solvent, solvent concentration, solvent to solid ratio, ultrasound power, temperature, extraction time and particle size on the yields of three bufadienolides were investigated. The optimum extraction conditions found were: 70% (v/v) methanol solution, solvent to solid ratio of 10ml/g, ultrasound power of 125W, temperature of 20°C, extraction time of 20min and particle size of 60-80 mesh. The extraction yields of bufalin, cinobufagin and resibufogenin were 43.17±0.85, 52.58±1.12, 137.70±2.65mg/g, respectively. In order to achieve a similar yield as UAE, soxhlet extraction required 6h and maceration extraction required much longer time of 18h. The results indicated that UAE is an alternative method for extracting bufadienolides from ChanSu. Copyright © 2012 Elsevier B.V. All rights reserved.

Carotid Doppler ultrasound findings in patients with left ventricular assist devices.

Science.gov (United States)

Cervini, Patrick; Park, Soon J; Shah, Dipesh K; Penev, Irina E; Lewis, Bradley D

2010-12-01

Left ventricular assist devices (LVADs) have been used to treat advanced heart failure refractory to medical management, as bridge therapy to myocardial recovery, as bridge therapy to cardiac transplantation, or as destination therapy for patients with unfavorable transplant candidacy. Neurologic complications are some of the most common and devastating complications in these patients. Preoperative carotid ultrasound is, therefore, a standard evaluation in patients at risk for cerebrovascular disease. Postoperative carotid artery Doppler sonography is performed in those patients with neurologic symptoms. It is likely, therefore, that sonographers, radiologists, and other physicians working in a center where LVADs are implanted will likely encounter a carotid artery Doppler study in this patient group. To our knowledge, the carotid Doppler findings in these patients have never been published. We review the Doppler ultrasound findings in 6 patients after LVAD insertion.

Vortex-Assisted Dispersive Micro-Solid Phase Extraction Using CTAB-Modified Zeolite NaY Sorbent Coupled with HPLC for the Determination of Carbamate Insecticides.

Science.gov (United States)

Salisaeng, Pawina; Arnnok, Prapha; Patdhanagul, Nopbhasinthu; Burakham, Rodjana

2016-03-16

A vortex-assisted dispersive micro-solid phase extraction (VA-D-μ-SPE) based on cetyltrimethylammonium bromide (CTAB)-modified zeolite NaY was developed for preconcentration of carbamate pesticides in fruits, vegetables, and natural surface water prior to analysis by high performance liquid chromatography with photodiode array detection. The small amounts of solid sorbent were dispersed in a sample solution, and extraction occurred by adsorption in a short time, which was accelerated by vortex agitation. Finally, the sorbents were filtered from the solution, and the analytes were subsequently desorbed using an appropriate solvent. Parameters affecting the VA-D-μ-SPE performance including sorbent amount, sample volume, desorption solvent ,and vortex time were optimized. Under the optimum condition, linear dynamic ranges were achieved between 0.004-24.000 mg kg(-1) (R(2) > 0.9946). The limits of detection (LODs) ranged from 0.004-4.000 mg kg(-1). The applicability of the developed procedure was successfully evaluated by the determination of the carbamate residues in fruits (dragon fruit, rambutan, and watermelon), vegetables (cabbage, cauliflower, and cucumber), and natural surface water.

Ultrasound-assisted oxidation of dibenzothiophene with phosphotungstic acid supported on activated carbon.

Science.gov (United States)

Liu, Liyan; Zhang, Yu; Tan, Wei

2014-05-01

Phosphotungstic acid (HPW) supported on activated carbon (AC) was applied to catalyze deep oxidation desulfurization of fuel oil with the assist of ultrasound. The sulfur-conversion rate was evaluated by measuring the concentration of dibenzothiophene (DBT) in n-octane before and after the oxidation. Supporting HPW on AC has been verified to play a positive role in UAOD process by a series of contrast tests, where only HPW, AC or a mixture of free HPW and AC was used. The influences of catalyst dose, ultrasound power, reaction temperature, H2O2:oil volume ratio and the reuse of catalyst on the catalytic oxidation desulfurization kinetics were investigated. The DBT conversion rate of the reaction catalyzed by supported HPW under ultrasound irradiation was higher than the summation of the reactions with HPW only and AC only as catalyst. With the increase of loading amount of HPW on AC, ultrasound power, H2O2:oil volume ratio and reaction temperature, the catalytic oxidation reactivity of DBT would be enhanced. The optimum loading amount of HPW was 10%, exceed which DBT conversion would no longer increase obviously. DBT could be completely converted under the optimized conditions (volume ratio of H2O2 to model oil: 1:10, mass ratio of the supported HPW to model oil: 1.25%, temperature: 70°C) after 9 min of ultrasound irradiation. Copyright © 2013 Elsevier B.V. All rights reserved.

Progress on Numerical Modeling of the Dispersion of Ceramic Nanoparticles During Ultrasonic Processing and Solidification of Al-Based Nanocomposites

Science.gov (United States)

Zhang, Daojie; Nastac, Laurentiu

2016-12-01

In present study, 6061- and A356-based nano-composites are fabricated by using the ultrasonic stirring technology (UST) in a coreless induction furnace. SiC nanoparticles are used as the reinforcement. Nanoparticles are added into the molten metal and then dispersed by ultrasonic cavitation and acoustic streaming assisted by electromagnetic stirring. The applied UST parameters in the current experiments are used to validate a recently developed magneto-hydro-dynamics (MHD) model, which is capable of modeling the cavitation and nanoparticle dispersion during UST processing. The MHD model accounts for turbulent fluid flow, heat transfer and solidification, and electromagnetic field, as well as the complex interaction between the nanoparticles and both the molten and solidified alloys by using ANSYS Maxwell and ANSYS Fluent. Molecular dynamics (MD) simulations are conducted to analyze the complex interactions between the nanoparticle and the liquid/solid interface. The current modeling results demonstrate that a strong flow can disperse the nanoparticles relatively well during molten metal and solidification processes. MD simulation results prove that ultrafine particles (10 nm) will be engulfed by the solidification front instead of being pushed, which is beneficial for nano-dispersion.

Atomization of liquids in a Pease-Anthony Venturi scrubber. Part II. Droplet dispersion.

Science.gov (United States)

Gonçalves, J A S; Costa, M A M; Aguiar, M L; Coury, J R

2004-12-10

Droplet distribution is of fundamental importance to the performance of a Venturi scrubber. Ensuring good liquid distribution can increase performance at minimal liquid usage. In this study, droplet dispersion in a rectangular Pease-Anthony Venturi scrubber, operating horizontally, was examined both theoretically and experimentally. The Venturi throat cross-section was 24 mm x 35 mm, and the throat length varied from 63 to 140 mm. Liquid was injected through a single orifice (1.0 mm diameter) on the throat wall. This arrangement allowed the study of the influence of jet penetration on droplet distribution. Gas velocity at the throat was 58.3 and 74.6 m/s, and the liquid flow rate was 286, 559 and 853 ml/min. A probe with a 2.7 mm internal diameter was used to isokinetically remove liquid from several positions inside the equipment. It was possible to study liquid distribution close to the injection point. A new model for droplet dispersion, which incorporates the new description of the jet atomization process developed by the present authors in the first article of this series, is proposed and evaluated. The model predicted well the experimental data.

Liquid-film assisted formation of alumina/niobium interfaces

OpenAIRE

Sugar, Joshua D.; McKeown, Joseph T.; Marks, Robert A.; Glaeser, Andreas M.

2002-01-01

Alumina has been joined at 1400 degrees C using niobium-based interlayers. Two different joining approaches were compared: solid-state diffusion bonding using a niobium foil as an interlayer, and liquid-film assisted bonding using a multilayer copper/niobium/copper interlayer. In both cases, a 127-(mu)m thick niobium foil was used; =1.4-(mu)m or =3-(mu)m thick copper films flanked the niobium. Room-temperature four-point bend tests showed that the introduction of a copper film had a significa...

Effect of oil extraction assisted by ultrasound on the physicochemical properties and fatty acid profile of pumpkin seed oil (Cucurbita pepo).

Science.gov (United States)

Hernández-Santos, Betsabé; Rodríguez-Miranda, Jesús; Herman-Lara, Erasmo; Torruco-Uco, Juan G; Carmona-García, Roselis; Juárez-Barrientos, José M; Chávez-Zamudio, Rubí; Martínez-Sánchez, Cecilia E

2016-07-01

The effects of amplitude and time of ultrasound-assisted extraction on the physicochemical properties and the fatty acid profile of pumpkin seed oil (Cucurbita pepo) were evaluated. Ultrasound time (5-30 min) and the response variables amplitude (25-100%), extraction yield, efficiency, oxidative stability in terms of the free fatty acids (FFA) of the plant design comprising two independent experiments variables, peroxide (PV), p-anisidine (AV), totox value (TV) and the fatty acid profile were evaluated. The results were analyzed by multiple linear regression. The time and amplitude showed significant differences (P<0.05) for all variables. The highest yield of extraction was achieved at 5 min and amplitude of 62.5% (62%). However, the optimal ultrasound-assisted extraction conditions were as follows: ultrasound time of 26.34 min and amplitude of 89.02%. All extracts showed low FFA (2.75-4.93% oleic acid), PV (1.67-4.68 meq/kg), AV (1.94-3.69) and TV (6.25-12.55) values. The main fatty acids in all the extracts were oleic and linoleic acid. Therefore, ultrasound-assisted oil extraction had increased performance and reduced extraction time without affecting the oil quality. Copyright © 2016 Elsevier B.V. All rights reserved.

Derivation of Hamaker Dispersion Energy of Amorphous Carbon Surfaces in Contact with Liquids Using Photoelectron Energy-Loss Spectra

Science.gov (United States)

Godet, Christian; David, Denis

2017-12-01

Hamaker interaction energies and cutoff distances have been calculated for disordered carbon films, in contact with purely dispersive (diiodomethane) or polar (water) liquids, using their experimental dielectric functions ɛ ( q, ω) obtained over a broad energy range. In contrast with previous works, a q-averaged q is derived from photoelectron energy-loss spectroscopy (XPS-PEELS) where the energy loss function (ELF) q is a weighted average over allowed transferred wave vector values, q, given by the physics of bulk plasmon excitation. For microcrystalline diamond and amorphous carbon films with a wide range of (sp3/sp2 + sp3) hybridization, non-retarded Hamaker energies, A 132 ( L < 1 nm), were calculated in several configurations, and distance and wavenumber cutoff values were then calculated based on A 132 and the dispersive work of adhesion obtained from contact angles. A geometric average approximation, H 0 CVL = ( H 0 CVC H 0 LVL )1/2, holds for the cutoff separation distances obtained for carbon-vacuum-liquid (CVL), carbon-vacuum-carbon (CVC) and liquid-vacuum-liquid (LVL) equilibrium configurations. The linear dependence found for A CVL, A CLC and A CLV values as a function of A CVC, for each liquid, allows predictive relationships for Hamaker energies (in any configuration) using experimental determination of the dispersive component of the surface tension, {γ}_{CV}^d , and a guess value of the cutoff distance H 0 CVC of the solid. [Figure not available: see fulltext.

Research on the treatment of phosphoric wastewater by ultrasound-assisted microelectrolysis method.

Science.gov (United States)

Yang, Hui; Xue, Jian-Jun; Wang, Ling; Wang, Zhao-Wei; Ling, Shi-Sheng; Kong, Ling-Guo; Chen, Yu-Lan

2012-01-01

In this research work, ultrasound was introduced to the microelectrolysis (ME) method to improve the treatment efficiency for phosphoric wastewater. The effects of treatment time, Fe/C ratio (v/v) and iron filings dosage on the efficiency of phosphorus removal from wastewater with different initial pH values were investigated. The results showed that the phosphorus removal efficiency by the ME method was significantly enhanced in the presence of ultrasound. The maximum removal rate of phosphorus (RRP) for the wastewater with an initial pH value of 4.0 was 92.4% after 60 min of treatment when the Fe/C and Fe/H2O volume ratio were 2/1 and 1/10, respectively. The reaction kinetics analysis indicated that the phosphorus degradation processes for the ultrasonic and ME methods as well as the ultrasonically assisted ME method (UME) were in accordance with the pseudo-first-order kinetic model. The synergetic effect of the combined ultrasound and ME method for phosphorus removal was also studied by reaction kinetics analysis.

A Numerical Analysis of Phononic-Assisted Control of Ultrasound Waves in Acoustofluidic Device

DEFF Research Database (Denmark)

Moiseyenko, Rayisa; Bruus, Henrik

2015-01-01

and streaming has received much attention, since it relies solely on mechanical properties such as particle size and contrast in density and compressibility. We present a theoretical study of phononic-assisted control of ultrasound waves in acoustofluidic devices. We propose the use of phononic crystal...... diffractors, which can be introduced in acoustofluidic structures. These diffractors can be applied in the design of efficient resonant cavities, directional sound waves for new types of particle sorting methods, or acoustically controlled deterministic lateral displacement. The PnC-diffractor-based devices...... can be made configurable, by embedding the diffractors, all working at the same excitation frequency but with different resulting diffraction patterns, in exchangeable membranes on top of the device....

Power ultrasound effects for in situ compatibilization of polymer-clay nanocomposites

International Nuclear Information System (INIS)

Ryu, Joung Gul; Park, Sang Wan; Kim, Hyungsu; Lee, Jae Wook

2004-01-01

Polymer-clay nanocomposites of various concentrations were prepared by ultrasonically assisted polymerization and melt mixing processes. The sonication process using power ultrasonic wave was employed to enhance nano-scale dispersion during melt mixing of monomer, polymer and organically modified clay. According to the unique mode of power ultrasound wave, we expected enhanced breakup of layered silicate bundle and further reduction in the size of dispersed phase with better homogeneity compared to the in situ polymerization. The optimum conditions to perform stable exfoliated nanocomposites were studied by various compositions and conditions. Dispersion characteristics and morphology of the nanocomposites were verified by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Rheological behaviors were measured under dynamic frequency sweep mode using Rheometric science ARES

Gravity assisted recovery of liquid xenon at large mass flow rates

Science.gov (United States)

Virone, L.; Acounis, S.; Beaupère, N.; Beney, J.-L.; Bert, J.; Bouvier, S.; Briend, P.; Butterworth, J.; Carlier, T.; Chérel, M.; Crespi, P.; Cussonneau, J.-P.; Diglio, S.; Manzano, L. Gallego; Giovagnoli, D.; Gossiaux, P.-B.; Kraeber-Bodéré, F.; Ray, P. Le; Lefèvre, F.; Marty, P.; Masbou, J.; Morteau, E.; Picard, G.; Roy, D.; Staempflin, M.; Stutzmann, J.-S.; Visvikis, D.; Xing, Y.; Zhu, Y.; Thers, D.

2018-06-01

We report on a liquid xenon gravity assisted recovery method for nuclear medical imaging applications. The experimental setup consists of an elevated detector enclosed in a cryostat connected to a storage tank called ReStoX. Both elements are part of XEMIS2 (XEnon Medical Imaging System): an innovative medical imaging facility for pre-clinical research that uses pure liquid xenon as detection medium. Tests based on liquid xenon transfer from the detector to ReStoX have been successfully performed showing that an unprecedented mass flow rate close to 1 ton per hour can be reached. This promising achievement as well as future areas of improvement will be discussed in this paper.

Inhibition of nonlinear acoustic cavitation dynamics in liquid CO2

NARCIS (Netherlands)

Iersel, van M.M.; Cornel, J.; Benes, N.E.; Keurentjes, J.T.F.

2007-01-01

The authors present a model to study ultrasound-induced cavitation dynamics in liquid carbon dioxide (CO2), which includes descriptions for momentum, mass, and energy transport. To assist in the interpretation of these results, numerical simulations are presented for an argon cavity in water. For

Ultrasound: a subexploited tool for sample preparation in metabolomics.

Science.gov (United States)

Luque de Castro, M D; Delgado-Povedano, M M

2014-01-02

Metabolomics, one of the most recently emerged "omics", has taken advantage of ultrasound (US) to improve sample preparation (SP) steps. The metabolomics-US assisted SP step binomial has experienced a dissimilar development that has depended on the area (vegetal or animal) and the SP step. Thus, vegetal metabolomics and US assisted leaching has received the greater attention (encompassing subdisciplines such as metallomics, xenometabolomics and, mainly, lipidomics), but also liquid-liquid extraction and (bio)chemical reactions in metabolomics have taken advantage of US energy. Also clinical and animal samples have benefited from US assisted SP in metabolomics studies but in a lesser extension. The main effects of US have been shortening of the time required for the given step, and/or increase of its efficiency or availability for automation; nevertheless, attention paid to potential degradation caused by US has been scant or nil. Achievements and weak points of the metabolomics-US assisted SP step binomial are discussed and possible solutions to the present shortcomings are exposed. Copyright © 2013 Elsevier B.V. All rights reserved.

Dispersive liquid-liquid microextraction coupled with magnetic nanoparticles for extraction of zearalenone in wheat samples

Directory of Open Access Journals (Sweden)

Mitra Amoli-Diva

2017-01-01

Full Text Available A new, sensitive and fast dispersive liquid-liquid microextraction (DLLME coupled with micro-solid phase extraction (μ-SPE was developed for determination of zearalenone (ZEN in wheat samples. The DLLME was performed using acetonitrile/water (80:20 v/v as the disperser solvent and 1-octanol as the extracting solvent.  The acetonitrile/water (80:20 v/v solvent was also used to extract ZEN from solid wheat matrix, and was directly applied as the disperser solvent for DLLME process. Additionally, hydrophobic oleic-acid-modified magnetic nanoparticles were used in μ-SPE approach to retrieve the analyte from the DLLME step. So, the method uses high surface area and strong magnetism properties of these nanoparticles to avoid time-consuming column-passing processes in traditional SPE. Main parameters affecting the extraction efficiency and signal enhancement were investigated and optimized. Under the optimum conditions, the calibration curve showed a good linearity in the range of 0.1-500 μg kg−1 (R2=0.9996 with low detection limit of 83 ng g−1. The intra-day and inter-day precisions (as RSD % in the range of 2.6-4.3 % and high recoveries ranging from 91.6 to 99.1 % were obtained. The pre-concentration factor was 3. The method is simple, inexpensive, accurate and remarkably free from interference effects.

Annular dispersed flow analysis model by Lagrangian method and liquid film cell method

International Nuclear Information System (INIS)

Matsuura, K.; Kuchinishi, M.; Kataoka, I.; Serizawa, A.

2003-01-01

A new annular dispersed flow analysis model was developed. In this model, both droplet behavior and liquid film behavior were simultaneously analyzed. Droplet behavior in turbulent flow was analyzed by the Lagrangian method with refined stochastic model. On the other hand, liquid film behavior was simulated by the boundary condition of moving rough wall and liquid film cell model, which was used to estimate liquid film flow rate. The height of moving rough wall was estimated by disturbance wave height correlation. In each liquid film cell, liquid film flow rate was calculated by considering droplet deposition and entrainment flow rate. Droplet deposition flow rate was calculated by Lagrangian method and entrainment flow rate was calculated by entrainment correlation. For the verification of moving rough wall model, turbulent flow analysis results under the annular flow condition were compared with the experimental data. Agreement between analysis results and experimental results were fairly good. Furthermore annular dispersed flow experiments were analyzed, in order to verify droplet behavior model and the liquid film cell model. The experimental results of radial distribution of droplet mass flux were compared with analysis results. The agreement was good under low liquid flow rate condition and poor under high liquid flow rate condition. But by modifying entrainment rate correlation, the agreement become good even under high liquid flow rate. This means that basic analysis method of droplet and liquid film behavior was right. In future work, verification calculation should be carried out under different experimental condition and entrainment ratio correlation also should be corrected

Dispersive liquid-liquid microextraction for metals enrichment: a useful strategy for improving sensitivity of laser-induced breakdown spectroscopy in liquid samples analysis.

Science.gov (United States)

Aguirre, M A; Selva, E J; Hidalgo, M; Canals, A

2015-01-01

A rapid and efficient Dispersive Liquid-Liquid Microextraction (DLLME) followed by Laser-Induced Breakdown Spectroscopy detection (LIBS) was evaluated for simultaneous determination of Cr, Cu, Mn, Ni and Zn in water samples. Metals in the samples were extracted with tetrachloromethane as pyrrolidinedithiocarbamate (APDC) complexes, using vortex agitation to achieve dispersion of the extractant solvent. Several DLLME experimental factors affecting extraction efficiency were optimized with a multivariate approach. Under optimum DLLME conditions, DLLME-LIBS method was found to be of about 4.0-5.5 times more sensitive than LIBS, achieving limits of detection of about 3.7-5.6 times lower. To assess accuracy of the proposed DLLME-LIBS procedure, a certified reference material of estuarine water was analyzed. Copyright © 2014 Elsevier B.V. All rights reserved.

Ultrasound propagation in dense aerogels filled with liquid 4He

International Nuclear Information System (INIS)

Matsumoto, K; Ohmori, K; Abe, S; Kanamori, K; Nakanishi, K

2012-01-01

Longitudinal ultrasound propagation was studied in dense aerogels filled with liquid 4 He. Sound velocity and attenuation were measured at the frequency of 6 MHz in both normal and superfluid phases. Pressure dependence of velocity and attenuation were also studied. Studied aerogels had porosities about 85%. They had two different types of structure, tangled strand structure and aggregated particles structure. The pore size distributions were narrow. Reduction of superfluid transition temperature mainly depended on not porosity but mean pore size. The structure of gel played an important role in sound velocity and attenuation.

Segmentation of breast ultrasound images based on active contours using neutrosophic theory.

Science.gov (United States)

Lotfollahi, Mahsa; Gity, Masoumeh; Ye, Jing Yong; Mahlooji Far, A

2018-04-01

Ultrasound imaging is an effective approach for diagnosing breast cancer, but it is highly operator-dependent. Recent advances in computer-aided diagnosis have suggested that it can assist physicians in diagnosis. Definition of the region of interest before computer analysis is still needed. Since manual outlining of the tumor contour is tedious and time-consuming for a physician, developing an automatic segmentation method is important for clinical application. The present paper represents a novel method to segment breast ultrasound images. It utilizes a combination of region-based active contour and neutrosophic theory to overcome the natural properties of ultrasound images including speckle noise and tissue-related textures. First, due to inherent speckle noise and low contrast of these images, we have utilized a non-local means filter and fuzzy logic method for denoising and image enhancement, respectively. This paper presents an improved weighted region-scalable active contour to segment breast ultrasound images using a new feature derived from neutrosophic theory. This method has been applied to 36 breast ultrasound images. It generates true-positive and false-positive results, and similarity of 95%, 6%, and 90%, respectively. The purposed method indicates clear advantages over other conventional methods of active contour segmentation, i.e., region-scalable fitting energy and weighted region-scalable fitting energy.

Terminal velocity of liquids and granular materials dispersed by a high explosive

Science.gov (United States)

Loiseau, J.; Pontalier, Q.; Milne, A. M.; Goroshin, S.; Frost, D. L.

2018-04-01

The explosive dispersal of a layer of solid particles or a layer of liquid surrounding a spherical high-explosive charge generates a turbulent, multiphase flow. Shock compression of the material layer during the initial acceleration may partially consolidate the material, leading to the formation of jet-like structures when the layer fragments and sheds particles upon release. Similarly, release of a shock-compressed liquid shell causes the nucleation of cavitation sites, leading to the radial breakup of the shell and the formation of jets upon expansion. In the current study, a wide variety of granular materials and liquids were explosively dispersed. The maximum terminal jet tip or shell velocity was measured using high-speed videography. Charges were constructed using thin-walled glass bulbs of various diameters and contained a central C-4 charge surrounded by the material to be dispersed. This permitted variation of the ratio of material mass to charge mass (M/C) from 4 to 300. Results indicated that material velocity broadly correlates with predictions of the Gurney model. For liquids, the terminal velocity was accurately predicted by the Gurney model. For granular materials, Gurney over-predicted the terminal velocity by 25-60%, depending on the M/C ratio, with larger M/C values exhibiting larger deficits. These deficits are explained by energy dissipation during the collapse of voids in the granular material bed. Velocity deficits were insensitive to the degree of jetting and granular material properties. Empirical corrections to the Gurney model are presented with improved agreement with the dry powder experimental velocities.

Terminal velocity of liquids and granular materials dispersed by a high explosive

Science.gov (United States)

Loiseau, J.; Pontalier, Q.; Milne, A. M.; Goroshin, S.; Frost, D. L.

2018-05-01

The explosive dispersal of a layer of solid particles or a layer of liquid surrounding a spherical high-explosive charge generates a turbulent, multiphase flow. Shock compression of the material layer during the initial acceleration may partially consolidate the material, leading to the formation of jet-like structures when the layer fragments and sheds particles upon release. Similarly, release of a shock-compressed liquid shell causes the nucleation of cavitation sites, leading to the radial breakup of the shell and the formation of jets upon expansion. In the current study, a wide variety of granular materials and liquids were explosively dispersed. The maximum terminal jet tip or shell velocity was measured using high-speed videography. Charges were constructed using thin-walled glass bulbs of various diameters and contained a central C-4 charge surrounded by the material to be dispersed. This permitted variation of the ratio of material mass to charge mass ( M/ C) from 4 to 300. Results indicated that material velocity broadly correlates with predictions of the Gurney model. For liquids, the terminal velocity was accurately predicted by the Gurney model. For granular materials, Gurney over-predicted the terminal velocity by 25-60%, depending on the M/ C ratio, with larger M/ C values exhibiting larger deficits. These deficits are explained by energy dissipation during the collapse of voids in the granular material bed. Velocity deficits were insensitive to the degree of jetting and granular material properties. Empirical corrections to the Gurney model are presented with improved agreement with the dry powder experimental velocities.

INVESTIGATION OF DENTURE REMOVAL PROCESS BY MEANS OF DESTRUCTION OF FIXING CEMENT BY ULTRASOUND ACTION

Directory of Open Access Journals (Sweden)

M. G. Kiselev

2007-01-01

Full Text Available The paper contains results of experimental investigations in respect of denture removal processes using as models so natural teeth as well and this removal process presupposes destruction of fixing cement by ultrasound action. It has been established that the best conditions for separation of a denture from a tooth body are ensured while ultrasound is acting on non-removable denture structure in liquid phase (water. At the expense of sound-capillary effect water fills in porous structure of fixing cement at high speed and a cavitation that appears in it leads to intensive cement destruction (dispersion.

Investigation of liquid phase axial dispersion in Taylor bubble flow by radiotracer residence time distribution analysis

Directory of Open Access Journals (Sweden)

Jin J.H.

2013-05-01

Full Text Available A gas-liquid Taylor bubble flow occurs in small diameter channels in which gas bubbles are separated by slugs of pure liquid. This type of flow regime is well suited for solid catalyzed gas-liquid reactors in which the reaction efficiency is a strong function of axial dispersion in the regions of pure liquid. This paper presents an experimental study of liquid phase axial dispersion in a Taylor bubble flow developed in a horizontal tube using high speed photography and radiotracer residence time distribution (RTD analysis. A parametric dependence of axial dispersion on average volume fraction of gas phase was also investigated by varying the relative volumetric flow rates of the two phases. 137mBa produced from a 137Cs/137mBa radionuclide generator was used as radiotracer and measurements were made using the NaI(Tl scintillation detectors. Validation of 137mBa in the form of barium chloride as aqueous phase radiotracer was also carried out. Axial Dispersion Model (ADM was used to simulate the hydrodynamics of the system and the results of the experiment are presented. It was observed that the system is characterized by very high values of Peclet Number (Pe∼102 which reveals an approaching plug type flow. The experimental and model estimated values of mean residence times were observed in agreement with each other.

Polarization and switching properties of holographic polymer-dispersed liquid-crystal gratings. I. Theoretical model

Science.gov (United States)

Sutherland, Richard L.

2002-12-01

Polarization properties and electro-optical switching behavior of holographic polymer-dispersed liquid-crystal (HPDLC) reflection and transmission gratings are studied. A theoretical model is developed that combines anisotropic coupled-wave theory with an elongated liquid-crystal-droplet switching model and includes the effects of a statistical orientational distribution of droplet-symmetry axes. Angle- and polarization-dependent switching behaviors of HPDLC gratings are elucidated, and the effects on dynamic range are described. A new type of electro-optical switching not seen in ordinary polymer-dispersed liquid crystals, to the best of the author's knowledge, is presented and given a physical interpretation. The model provides valuable insight to the physics of these gratings and can be applied to the design of HPDLC holographic optical elements.

Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

Science.gov (United States)

Krawczyk-Coda, Magdalena

2017-03-01

In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

The Use of Response Surface Methodology to Optimize the Ultrasound-Assisted Extraction of Five Anthraquinones from Rheum palmatum L.

Directory of Open Access Journals (Sweden)

Xianghua Xia

2011-07-01

Full Text Available In this paper, ultrasound-assisted extraction (UAE was applied to the extraction of anthraquinones (aloe-emodin, rhein, emodin, chrysophanol and physcion from Rheum palmatum L. The five anthraquinones were quantified and analyzed by high performance liquid chromatography coupled with UV detection (HPLC-UV. The extraction solvent, extraction temperature and extraction time parameters, the three main factors for UAE, were optimized with response surface methodology (RSM to obtain the highest extraction efficiency. The optimal conditions were the use of 84% methanol as solvent, an extraction time of 33 min and an extraction temperature of 67 °C. Under these optimal conditions, the experimental values agreed closely with the predicted values. The analysis of variance indicated a high goodness of model fit and the success of RSM method for optimizing anthraquinones extraction in Rheum palmatum L.

Determination of organophosphorus pesticides by dispersive liquid-liquid micro extraction coupled with gas chromatography-electron capture detection

International Nuclear Information System (INIS)

Mohd Marsin Sanagi; Siti Umairah Mokhtar; Mazidatul Akmam Miskam; Wan Aini Wan Ibrahim

2011-01-01

A simple, rapid and sensitive method termed as dispersive liquid-liquid micro extraction (DLLME) combined with gas chromatography-electron capture detector (GC-ECD) was developed for the determination of selected organophosphorus pesticides (OPPs) namely chloropyrifos, dimethoate and diazinon in water sample. In this method, a mixture of carbon disulfide, CS 2 (extraction solvent) and methanol (disperser solvent) was rapidly injected using syringe into the 5.00 mL water sample to form a cloudy solution where the OPPs were extracted into the fine droplets of extraction solvent. Upon centrifugation for 3 min at 3500 rpm, the fine droplets were sedimented at the bottom of the centrifuge tube. Sedimented phase (1 μL) was injected into the GC-ECD for separation and determination of OPPs. Important extraction parameters, such as type of disperser solvent, volume of extraction solvent and volume of disperser solvent were investigated. The optimized conditions for DLLME of the selected OPPs were methanol as disperser solvent, 30 μL of extraction solvent (CS 2 ) and 1.0 mL of disperser solvent (methanol). Under the optimum extraction conditions, the method showed good linearity in the range of 0.1 to 1.0 μg/ mL with correlation coefficient (r 2 ), in the range of 0.9976 to 0.9994 and low limits of detection (LOD) between 0.047 and 0.201 μg/ mL. The proposed method provided acceptable recoveries (72.67- 144 %) with good RSDs ranging from 2.74 % to 7.48 %. This method was successfully applied to the determination of OPPs in water samples obtained from a golf course and chloropyrifos and diazinon were detected at concentration 0.18 μg/ mL and 0.07 μg/ mL, respectively. (author)

Cervical histology after routine ThinPrep or SurePath liquid-based cytology and computer-assisted reading in Denmark

DEFF Research Database (Denmark)

Rebolj, Matejka; Rask, Johanne; van Ballegooijen, Marjolein

2015-01-01

nationwide registers, technological phases were identified by slide preparation, reading technique, and triage of borderline cytology. Trends in the detection of cervical intraepithelial neoplasia (CIN) were an indicator of the technology's relative sensitivity, and trends in false-positive tests......BACKGROUND: We compared the sensitivity and specificity of liquid-based cytology (LBC) and computer-assisted reading for SurePath/FocalPoint and ThinPrep with those of manually read conventional cytology in routine cervical screening in four Danish laboratories. METHODS: Using data from five...

Minimizing complications of ultrasound-assisted lipoplasty: an initial experience with no related complications.

Science.gov (United States)

Tebbetts, J B

1998-10-01

Numerous complications and increased operating times were reported with ultrasonically assisted lipoplasty in the first several months after introduction of the technology in the United States. The purpose of this study was to review early reported complications and management regimens, evaluate possible causes of problems, and apply indications and techniques to attempt to minimize complications during an initial experience with this technique beginning in January of 1997. Seven specific indications and modifications of existing techniques were developed and applied to an initial clinical series of 70 consecutive patients who underwent ultrasound-assisted suction lipoplasty between January 10, 1997, and August 1, 1997. Follow-up ranged from 1 to 7 months. No perioperative or postoperative complication occurred in any patient in this series. In this series of ultrasound-assisted lipoplasty cases, application of the following criteria resulted in a series of 70 patients with 1 to 7-month follow-up without complications: (1) selecting patients with well localized fat deposits who were no more than 20 percent above their ideal body weight; (2) infusing a solution of Ringer's Lactate containing 1 cc of 1:1000 epinephrine per 1000 cc into the area of fat removal, stopping infusion when the tissues first become firm, not infusing to marked tissue turgor or skin induration; (3) restricting the level of energy application to a minimum of 1 cm from the undersurface of the dermis; (4) limiting ultrasonic energy application in each area to approximately 1 minute per estimated 100 cc of total aspirate in a wet to superwet environment; (5) not performing ultrasound-assisted lipoplasty in the same area as another procedure that could potentially compromise tissue vascularity; (6) using a Lysonix 2000 generator and 5-mm golf tee tip probe at a power setting of 8 to apply ultrasonic energy to the area of fat removal, ceasing energy application when tissue resistance to the passage

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

DEFF Research Database (Denmark)

Genina, Natalja; Räikkönen, Heikki; Antikainen, Osmo

2010-01-01

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

Investigation of a polymer-dispersed liquid crystal system by NMR diffusometry and relaxometry

Energy Technology Data Exchange (ETDEWEB)

Tang, Mingxue

2013-02-26

Polymer-dispersed liquid crystals (PDLCs) are polymer composites containing a dispersion of liquid crystal droplets in polymer networks. PDLCs have attracted much attention due to their unique properties and potential usage. The properties of PDLCs depend on the degree of phase separation and the size of liquid crystal droplets. To investigate the structure will help us to better understand and optimize PDLCs.The main aim of this PhD thesis was to investigate PDLCs by NMR techniques. Diffusion constants and spin-lattice relaxation times in the laboratory (T{sub 1}) and rotating frame (T{sub 1{rho}}) were measured for PDLCs as well as precursor mixtures based on the trifunctional monomer trimethylolpropane triacrylate (TMPTA) and the commercial nematic mixture E7. The variation of the main dipolar splitting of {sup 1}H spectra with increasing temperature was analyzed to obtain the nematic-to-isotropic phase transition temperature and the nematic order parameter of E7 and, for comparison, the nematic liquid crystal 5CB.Diffusion constants in TMPTA/E7 mixtures, measured by pulsed-field gradient NMR, increase for both E7 and TMPTA as the mass fraction of E7 increases, due to the lower viscosity of E7. E7 in the PDLC diffuses more slowly than in the bulk because of the hindrance by the polymer matrix. T{sub 1} and T{sub 1{rho}} relaxation times in the liquid or liquid-crystalline phases of TMPTA and bulk E7 are higher than in the PDLC and the pure polymer, due to the lower mobility in the polymer samples. T{sub 1{rho}} in the PDLC is even shorter than in the pure polymer, indicating an anti-softening effect caused by E7 molecules. In bulk E7, the well-ordered rod-like molecules exhibit a unique H-C dipolar coupling, which leads to oscillations in the cross-polarization curve. However, in the PDLC, the anchoring effect at the boundary between the polymer and LC droplets disturbs the molecular order resulting in a smooth cross polarization curve.

Investigation of a polymer-dispersed liquid crystal system by NMR diffusometry and relaxometry

International Nuclear Information System (INIS)

Tang, Mingxue

2013-01-01

Polymer-dispersed liquid crystals (PDLCs) are polymer composites containing a dispersion of liquid crystal droplets in polymer networks. PDLCs have attracted much attention due to their unique properties and potential usage. The properties of PDLCs depend on the degree of phase separation and the size of liquid crystal droplets. To investigate the structure will help us to better understand and optimize PDLCs.The main aim of this PhD thesis was to investigate PDLCs by NMR techniques. Diffusion constants and spin-lattice relaxation times in the laboratory (T 1 ) and rotating frame (T 1ρ ) were measured for PDLCs as well as precursor mixtures based on the trifunctional monomer trimethylolpropane triacrylate (TMPTA) and the commercial nematic mixture E7. The variation of the main dipolar splitting of 1 H spectra with increasing temperature was analyzed to obtain the nematic-to-isotropic phase transition temperature and the nematic order parameter of E7 and, for comparison, the nematic liquid crystal 5CB.Diffusion constants in TMPTA/E7 mixtures, measured by pulsed-field gradient NMR, increase for both E7 and TMPTA as the mass fraction of E7 increases, due to the lower viscosity of E7. E7 in the PDLC diffuses more slowly than in the bulk because of the hindrance by the polymer matrix. T 1 and T 1ρ relaxation times in the liquid or liquid-crystalline phases of TMPTA and bulk E7 are higher than in the PDLC and the pure polymer, due to the lower mobility in the polymer samples. T 1ρ in the PDLC is even shorter than in the pure polymer, indicating an anti-softening effect caused by E7 molecules. In bulk E7, the well-ordered rod-like molecules exhibit a unique H-C dipolar coupling, which leads to oscillations in the cross-polarization curve. However, in the PDLC, the anchoring effect at the boundary between the polymer and LC droplets disturbs the molecular order resulting in a smooth cross polarization curve.

Optimization of biodiesel production from Chlorella protothecoides oil via ultrasound assisted transesterification

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Özçimen Didem

2017-01-01

Full Text Available There is a growing interest in biodiesel as an alternative fuel for diesel engines because of the high oil prices and environmental issues related to massive greenhouse gas emissions. Nowadays, microalgal biomass has become a promising biodiesel feedstock. However, traditional biodiesel production from microalgae consumes a lot of energy and solvents. It is necessary to use an alternative method that can reduce the energy and alcohol consumption and save time. In this study, biodiesel production from Chlorella protothecoides oil by ultrasound assisted transesterification was conducted and effects of reaction parameters such as methanol:oil ratio, catalyst/oil ratio and reaction time on fatty acid methyl ester yields were investigated. The transesterification reactions were carried out by using methanol as alcohol and potassium hydroxide as the catalyst. The highest methyl ester production was obtained under the conditions of 9:1 methanol/oil mole ratio, 1.5% potassium hydroxide catalyst in oil, and for reaction time of 40 min. It was also found that catalyst/oil molar ratio was the most effective parameter on methyl ester yield according to statistical data. The results showed that ultrasound-assisted transesterification may be an alternative and cost effective way to produce biodiesel efficiently.

Salting-out-enhanced ionic liquid microextraction with a dual-role solvent for simultaneous determination of trace pollutants with a wide polarity range in aqueous samples.

Science.gov (United States)

Gao, Man; Qu, Jingang; Chen, Kai; Jin, Lide; Dahlgren, Randy Alan; Wang, Huili; Tan, Chengxia; Wang, Xuedong

2017-11-01

In real aquatic environments, many occupational pollutants with a wide range of polarities coexist at nanogram to milligram per liter levels. Most reported microextraction methods focus on extracting compounds with similar properties (e.g., polarity or specific functional groups). Herein, we developed a salting-out-enhanced ionic liquid microextraction based on a dual-role solvent (SILM-DS) for simultaneous detection of tetracycline, doxycycline, bisphenol A, triclosan, and methyltriclosan, with log K ow ranging from -1.32 to 5.40 in complex milk and environmental water matrices. The disperser in the ionic-liquid-based dispersive liquid-liquid microextraction was converted to the extraction solvent in the subsequent salting-out-assisted microextraction procedures, and thus a single solvent performed a dual role as both extractant and disperser in the SILM-DS process. Acetonitrile was selected as the dual-role solvent because of its strong affinity for both ionic liquids and water, as well as the extractant in the salting-out step. Optimized experimental conditions were 115 μL [C 8 MIM][PF 6 ] as extractor, 1200 μL acetonitrile as dual-role solvent, pH 2.0, 5.0 min ultrasound extraction time, 3.0 g Na 2 SO 4 , and 3.0 min vortex extraction time. Under optimized conditions, the recoveries of the five pollutants ranged from 74.5 to 106.9%, and their LODs were 0.12-0.75 μg kg -1 in milk samples and 0.11-0.79 μg L -1 in environmental waters. Experimental precision based on relative standard deviation was 1.4-6.4% for intraday and 2.3-6.5% for interday analyses. Compared with previous methods, the prominent advantages of the newly developed method are simultaneous determination of pollutants with a wide range of polarities and a substantially reduced workload for ordinary environmental monitoring and food tests. Therefore, the new method has great application potential for simultaneous determination of trace pollutants with strongly contrasting polarities in several

In-syringe dispersive liquid-liquid microextraction with liquid chromatographic determination of synthetic pyrethroids in surface water

Directory of Open Access Journals (Sweden)

Saeed S. Albaseer

2012-03-01

Full Text Available An indigenously fabricated in laboratory glass syringe was used for in-syringe dispersive liquid-liquid microextraction (is-DLLME and preconcentration of synthetic pyrethroids (SPs from surface waters suitable for their determination by high performance liquid chromatography. In contrast to classical DLLME, is-DLLME allows the use of lighter-than-water organic solvents and the analysis of environmental contaminants’ samples without prior filtration, which is of great importance due to the high affinity of pyrethroids to adsorb to solid particulates present in environmental samples. The effects of various parameters on the extraction efficiency were evaluated and optimized systemically using one-factor-at-a-time method (OFAT and statistically using full factorial design (24. Three SPs (viz.; cypermethrin, resmethrin and permethrin were analyzed. The method showed good accuracy with RSD% in the range of of 4.8–6.9%. The method detection limits of the three pesticides ranged from 0.14 to 0.16 ng mL-1. The proposed method was applied for the determination of synthetic pyrethroids in lake water

Ultrasound diagnostics of thyroid diseases

International Nuclear Information System (INIS)

Kharchenko, Vladimir P.; Kotlyarov, Peter M.; Mogutov, Mikhail S.; Sencha, Alexander N.; Patrunov, Yury N.; Belyaev, Denis V.; Alexandrov, Yury K.

2010-01-01

This book is based on the authors' extensive practical experience in the use of modern ultrasound, and other radiological methods, in the diagnosis of thyroid diseases. The authors have analyzed more than 100,000 ultrasound examinations performed between 1995 and 2008 in patients with thyroid and parathyroid disease, as well as many thousands of diagnostic and therapeutic ultrasound-guided minimally invasive procedures. The opening chapters include discussion of current ultrasound techniques, pitfalls, and the specifics of ultrasound examination of the thyroid in children. Detailed attention is then devoted to findings in the normal thyroid and in the presence of diffuse and focal changes. Further chapters focus on such topics as ultrasound examination after thyroid surgery and ultrasound diagnosis of parathyroid disease, recurrent goiter, and neck masses. Ultrasound-guided minimally invasive techniques, such as fine-needle aspiration biopsy, percutaneous laser ablation, and ethanol and glucocorticoid injections, are considered in depth. This up-to-date and richly illustrated book will interest and assist specialists in ultrasound diagnostics, radiologists, endocrinologists, and neck surgeons. (orig.)

Combination of dispersive liquid-liquid microextraction with flame atomic absorption spectrometry using microsample introduction for determination of lead in water samples

International Nuclear Information System (INIS)

Naseri, Mohammad Taghi; Hemmatkhah, Payam; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub

2008-01-01

The dispersive liquid-liquid microextraction (DLLME) was combined with the flame atomic absorption spectrometry (FAAS) for determination of lead in the water samples. Diethyldithiophosphoric acid (DDTP), carbon tetrachloride and methanol were used as chelating agent, extraction solvent and disperser solvent, respectively. A new FAAS sample introduction system was employed for the microvolume nebulization of the non-flammable chlorinated organic extracts. Injection of 20 μL volumes of the organic extract into an air-acetylene flame provided very sensitive spike-like and reproducible signals. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters include extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH and amount of the chelating agent. Under the optimized conditions, the enrichment factor of 450 was obtained from a sample volume of 25.0 mL. The enhancement factor, calculated as the ratio of the slopes of the calibration graphs with and without preconcentration, which was about 1000. The calibration graph was linear in the range of 1-70 μg L -1 with a detection limit of 0.5 μg L -1 . The relative standard deviation (R.S.D.) for seven replicate measurements of 5.0 and 50 μg L -1 of lead were 3.8 and 2.0%, respectively. The relative recoveries of lead in tap, well, river and seawater samples at the spiking level of 20 μg L -1 ranged from 93.8 to 106.2%. The characteristics of the proposed method were compared with those of the liquid-liquid extraction (LLE), cloud point extraction (CPE), on-line and off-line solid-phase extraction (SPE) as well as co-precipitation, based on bibliographic data. Operation simplicity, rapidity, low cost, high enrichment factor, good repeatability, and low consumption of the extraction solvent at a microliter level are the main advantages of the proposed method

A new chiral residue analysis method for triazole fungicides in water using dispersive liquid-liquid microextraction (DLLME).

Science.gov (United States)

Luo, Mai; Liu, Donghui; Zhou, Zhiqiang; Wang, Peng

2013-09-01

A rapid, simple, reliable, and environment-friendly method for the residue analysis of the enantiomers of four chiral fungicides including hexaconazole, triadimefon, tebuconazole, and penconazole in water samples was developed by dispersive liquid-liquid microextraction (DLLME) pretreatment followed by chiral high-performance liquid chromatography (HPLC)-DAD detection. The enantiomers were separated on a Chiralpak IC column by HPLC applying n-hexane or petroleum ether as mobile phase and ethanol or isopropanol as modifier. The influences of mobile phase composition and temperature on the resolution were investigated and most of the enantiomers could be completely separated in 20 min under optimized conditions. The thermodynamic parameters indicated that the separation was enthalpy-driven. The elution orders were detected by both circular dichroism detector (CD) and optical rotatory dispersion detector (ORD). Parameters affecting the DLLME performance for pretreatment of the chiral fungicides residue in water samples, such as the extraction and dispersive solvents and their volume, were studied and optimized. Under the optimum microextraction condition the enrichment factors were over 121 and the linearities were 30-1500 µg L(-1) with the correlation coefficients (R(2)) over 0.9988 and the recoveries were between 88.7% and 103.7% at the spiking levels of 0.5, 0.25, and 0.05 mg L(-1) (for each enantiomer) with relative standard deviations varying from 1.38% to 6.70% (n = 6) The limits of detection (LODs) ranged from 8.5 to 29.0 µg L(-1) (S/N = 3). © 2013 Wiley Periodicals, Inc.

Determination of benzimidazoles in meat samples by capillary zone electrophoresis tandem mass spectrometry following dispersive liquid-liquid microextraction.