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Sample records for ultrasound-assisted extraction coupled

  1. Ultrasound assisted extraction of bioactive compounds

    Directory of Open Access Journals (Sweden)

    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.

  2. Coupling continuous ultrasound-assisted extraction, preconcentration and flame atomic absorption spectrometric detection for the determination of cadmium and lead in mussel samples

    International Nuclear Information System (INIS)

    Yebra-Biurrun, M.C.; Cancela-Perez, S.; Moreno-Cid-Barinaga, A.

    2005-01-01

    Continuous ultrasound-assisted extraction has been coupled with preconcentration and flame atomic absorption spectrometry for the determination of cadmium and lead in mussel samples. Experimental designs were used for the optimisation of the leaching and preconcentration steps. The use of diluted nitric acid as extractant in the continuous mode at a flow rate of 3.5 ml min -1 and room temperature was sufficient for quantitative extraction of these trace metals. A minicolumn containing a chelating resin (Chelite P, with aminomethylphosphoric acid groups) was proved as an excellent material for the quantitative preconcentration of cadmium and lead prior to their flame atomic absorption detection. A flow injection manifold was used as interface for coupling the three analytical steps, which allowed the automation of the whole analytical process. A good precision of the whole procedure (2.0 and 2.3%), high enrichment factors (20.5 and 11.8) and a detection limit of 0.011 and 0.25 μg g -1 for cadmium and lead, respectively, were obtained for 80 mg of sample. The sample throughputs were ca. 16 and 14 samples h -1 for cadmium and lead, respectively. The accuracy of the analytical procedures was verified by using a standard reference material (BCR 278-R, mussel tissue) and the results were in good agreement with the certified values. The method was successfully applied to the determination of trace amounts of cadmium and lead in mussel samples from the coast of Galicia (NW, Spain)

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

    Directory of Open Access Journals (Sweden)

    T. W. Charpe

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

  4. 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.

  5. 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

  6. 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

  7. Ultrasound-Assisted Extraction of Stilbenes from Grape Canes

    Directory of Open Access Journals (Sweden)

    Zulema Piñeiro

    2016-06-01

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

  8. Ultrasound-Assisted Extraction of Stilbenes from Grape Canes.

    Science.gov (United States)

    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.

  9. The choice of ultrasound assisted extraction coupled with spectrophotometric for rapid determination of gallic acid in water samples: Central composite design for optimization of process variables.

    Science.gov (United States)

    Pooralhossini, Jaleh; Ghaedi, Mehrorang; Zanjanchi, Mohammad Ali; Asfaram, Arash

    2017-01-01

    A sensitive procedure namely ultrasound-assisted (UA) coupled dispersive nano solid-phase microextraction spectrophotometry (DNSPME-UV-Vis) was designed for preconcentration and subsequent determination of gallic acid (GA) from water samples, while the detailed of composition and morphology and also purity and structure of this new sorbent was identified by techniques like field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) and Energy-dispersive X-ray spectroscopy (EDX) techniques. Among conventional parameters viz. pH, amount of sorbent, sonication time and volume of elution solvent based on Response Surface Methodology (RSM) and central composite design according to statistics based contour the best operational conditions was set at pH of 2.0; 1.5mg sorbent, 4.0min sonication and 150μL ethanol. Under these pre-qualified conditions the method has linear response over wide concentration range of 15-6000ngmL -1 with a correlation coefficient of 0.9996. The good figure of merits like acceptable LOD (S/N=3) and LOQ (S/N=10) with numerical value of 2.923 and 9.744ngmL -1 , respectively and relative recovery between 95.54 and 100.02% show the applicability and efficiency of this method for real samples analysis with RSDs below 6.0%. Finally the method with good performance were used for monitoring under study analyte in various real samples like tap, river and mineral waters. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. A Simple Method for the Simultaneous Determination of Pharmaceuticals and Personal Care Products in River Sediment by Ultrasound-Assisted Extraction Followed by Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Díaz, Alejandro; Peña-Alvarez, Araceli

    2017-10-01

    A simple method was developed using ultrasound-assisted extraction (UAE) combined with solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of eight different pharmaceuticals and personal care products (PPCPs) (ibuprofen, 2-benzyl-4-chlorophenol, naproxen, triclosan, ketoprofen, diclofenac, bisphenol A and estrone) in river sediment. UAE conditions were optimized involving extraction variables such as extraction solvent, extraction time, sample amount, extraction temperature, pH and salt addition. A 100 mg of sediment was extracted by optimized UAE process using 7 mL deionized water (pH 3) + 1% methanol as solvent, room temperature and 1 min extraction at 70% of amplitude. A 5 mL of supernatant was subsequently extracted by SPME; the extracted analytes were derivatized on fiber in head-space mode with N-methyl-N-(tertbutyldimethylsilyl) trifluoroacetamide and then analyzed by GC-MS. The developed method was evaluated by testing: precision (CV 0.98), recoveries (56-108%), limits of detection (simple and environmentally friendly, and provides straightforward analyses of these trace organic pollutants in sediment samples. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

    Science.gov (United States)

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

    2016-01-01

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

  12. Ultrasound-assisted extraction of amino acids from grapes.

    Science.gov (United States)

    Carrera, Ceferino; Ruiz-Rodríguez, Ana; Palma, Miguel; Barroso, Carmelo G

    2015-01-01

    Recent cultivar techniques on vineyards can have a marked influence on the final nitrogen content of grapes, specifically individual amino acid contents. Furthermore, individual amino acid contents in grapes are related to the final aromatic composition of wines. A new ultrasound-assisted method for the extraction of amino acids from grapes has been developed. Several extraction variables, including solvent (water/ethanol mixtures), solvent pH (2-7), temperature (10-70°C), ultrasonic power (20-70%) and ultrasonic frequency (0.2-1.0s(-)(1)), were optimized to guarantee full recovery of the amino acids from grapes. An experimental design was employed to optimize the extraction parameters. The surface response methodology was used to evaluate the effects of the extraction variables. The analytical properties of the new method were established, including limit of detection (average value 1.4mmolkg(-)(1)), limit of quantification (average value 2.6mmolkg(-)(1)), repeatability (average RSD=12.9%) and reproducibility (average RSD=15.7%). Finally, the new method was applied to three cultivars of white grape throughout the ripening period. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Evaluation of ultrasound-assisted extraction as sample pre-treatment for quantitative determination of rare earth elements in marine biological tissues by inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Costas, M.; Lavilla, I.; Gil, S.; Pena, F.; Calle, I.; Cabaleiro, N. de la; Bendicho, C.

    2010-01-01

    In this work, the determination of rare earth elements (REEs), i.e. Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu in marine biological tissues by inductively coupled-mass spectrometry (ICP-MS) after a sample preparation method based on ultrasound-assisted extraction (UAE) is described. The suitability of the extracts for ICP-MS measurements was evaluated. For that, studies were focused on the following issues: (i) use of clean up of extracts with a C18 cartridge for non-polar solid phase extraction; (ii) use of different internal standards; (iii) signal drift caused by changes in the nebulization efficiency and salt deposition on the cones during the analysis. The signal drift produced by direct introduction of biological extracts in the instrument was evaluated using a calibration verification standard for bracketing (standard-sample bracketing, SSB) and cumulative sum (CUSUM) control charts. Parameters influencing extraction such as extractant composition, mass-to-volume ratio, particle size, sonication time and sonication amplitude were optimized. Diluted single acids (HNO 3 and HCl) and mixtures (HNO 3 + HCl) were evaluated for improving the extraction efficiency. Quantitative recoveries for REEs were achieved using 5 mL of 3% (v/v) HNO 3 + 2% (v/v) HCl, particle size <200 μm, 3 min of sonication time and 50% of sonication amplitude. Precision, expressed as relative standard deviation from three independent extractions, ranged from 0.1 to 8%. In general, LODs were improved by a factor of 5 in comparison with those obtained after microwave-assisted digestion (MAD). The accuracy of the method was evaluated using the CRM BCR-668 (mussel tissue). Different seafood samples of common consumption were analyzed by ICP-MS after UAE and MAD.

  14. 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) ...

  15. 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.

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

    Science.gov (United States)

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

    2011-04-01

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

  17. 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.

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

    OpenAIRE

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

    2016-01-01

    Object. Ultrasound-assisted extraction of total flavonoids from corn silk and their antioxidant activities were studied. Methods. Response surface methodology was adopted to optimize the extraction conditions and antioxidant activities of the extracted total flavonoids were detected through ferric reducing antioxidant power (FRAP) assay. Results. Through a three-level, three-variable Box-Behnken design of response surface methodology (RSM) adopting yield as response, the optimal conditions we...

  19. 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.

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

    Science.gov (United States)

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

    2017-01-01

    This review presents a complete picture of current knowledge on ultrasound-assisted extraction (UAE) in food ingredients and products, nutraceutics, cosmetic, pharmaceutical and bioenergy applications. It provides the necessary theoretical background and some details about extraction by ultrasound, the techniques and their combinations, the mechanisms (fragmentation, erosion, capillarity, detexturation, and sonoporation), applications from laboratory to industry, security, and environmental impacts. In addition, the ultrasound extraction procedures and the important parameters influencing its performance are also included, together with the advantages and the drawbacks of each UAE techniques. Ultrasound-assisted extraction is a research topic, which affects several fields of modern plant-based chemistry. All the reported applications have shown that ultrasound-assisted extraction is a green and economically viable alternative to conventional techniques for food and natural products. The main benefits are decrease of extraction and processing time, the amount of energy and solvents used, unit operations, and CO 2 emissions. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. 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.

  2. 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.

  3. Ultrasound assisted mercury extraction from soil and sediment

    International Nuclear Information System (INIS)

    Collasiol, Andre; Pozebon, Dirce; Maia, Sandra M.

    2004-01-01

    A method for mercury (Hg) determination in soil, river sediment and marine sediment without sample digestion is investigated. Mercury determination is performed by cold vapour atomic absorption spectrometry (CV-AAS) using a flow injection system. Mercury quantitatively leaches out from the investigated marine sediment into 30% (v/v) HNO 3 assisted by ultrasonic irradiation (during 90-120 s) when sample particles size are ≤120 μm. Similar conditions can be applied for Hg determination in river sediment and soil, excepting the time of sonication which needs to be increased to 180 s and KCl is also added to the extraction medium. The presence of 0.15% (m/v) KCl in addition to 30% (v/v) HNO 3 is seen to be effective for quantitative Hg leaching. The certified samples PACS-2 and MESS-3 (both marine sediment from NRCC), Buffalo River (NIST 8704), Montana Soil (NIST 2710) and the non-certified river sediment sample RS-3 were analysed. The attained results were well within the 95% confidence level of the certificate or close to information value. Samples were analysed using aqueous standard calibration. A characteristic mass of 25 pg, a LOD (3s) of 0.2 μg Hg l -1 and a LOQ (10s) of 0.012 μg Hg g -1 are typically attained. These are based on 800 μl of sample solution and 1.000 g of sample mass in 20 ml. The RSD of 10 consecutive runs of the sample is <5%. The proposed method was finally applied for the determination of Hg in real samples of soil, river sediment and marine sediment. The same samples were also analysed using a digestion method giving similar results

  4. 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.

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

    Science.gov (United States)

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

    2017-05-01

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

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

    Science.gov (United States)

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

    2013-10-10

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

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

    Directory of Open Access Journals (Sweden)

    Hasanah Mohd Ghazali

    2013-10-01

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

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

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    Ling-Li Zheng

    2016-01-01

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

  9. 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.

  10. 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.

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2017-04-15

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

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

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    Joël Wajsman

    2013-03-01

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

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

    Science.gov (United States)

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

    2013-03-12

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

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

    Science.gov (United States)

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

    2015-01-01

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

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

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    Javed Ahamad

    2015-01-01

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

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

    Science.gov (United States)

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

    2015-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Jovanović Aleksandra A.

    2016-01-01

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

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

    Science.gov (United States)

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

    2016-02-18

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

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

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    Nelly Medina-Torres

    2017-07-01

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

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

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    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.

  2. 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.

  3. Optimization of ultrasound-assisted extraction (UAE) of phenolic compounds from olive cake.

    Science.gov (United States)

    Mojerlou, Zohreh; Elhamirad, Amirhhossein

    2018-03-01

    The use of ultrasound in ultrasound-assisted extraction (UAE) is one of the main applications of this technology in food industry. This study aimed to optimize UAE conditions for olive cake extract (OCE) through response surface methodology (RSM). The optimal UAE conditions were obtained with extraction temperature of 56 °C, extraction time of 3 min, duty cycle of 0.6 s, and solid to solvent ratio of 3.6%. At the optimum conditions, the total phenolic compounds (TPC) content and antioxidant activity (AA) were measured 4.04 mg/g and 68.9%, respectively. The linear term of temperature had the most effect on TPC content and AA of OCE prepared by UAE. Protocatechuic acid and cinnamic acid were characterized as the highest (19.5%) and lowest (1.6%) phenolic compound measured in OCE extracted by UAE. This research revealed that UAE is an effective method to extract phenolic compounds from olive cake. RSM successfully optimized UAE conditions for OCE.

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

    Directory of Open Access Journals (Sweden)

    L. J. Ong

    2016-09-01

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

  5. 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.

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

    Science.gov (United States)

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

    2017-02-18

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

  7. 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.

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

    Science.gov (United States)

    Kulkarni, Vrushali M; Rathod, Virendra K

    2014-03-01

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

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

    Science.gov (United States)

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

    2015-10-01

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

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

    Directory of Open Access Journals (Sweden)

    Xuejing Jia

    2015-11-01

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

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

    Science.gov (United States)

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

    2015-11-23

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

  12. 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.

  13. 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.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  15. 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.

  16. 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.

  17. 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.

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

    Directory of Open Access Journals (Sweden)

    Mohammad Bagher Gholivand

    2014-12-01

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

  19. Optimization of enzymes-microwave-ultrasound assisted extraction of Lentinus edodes polysaccharides and determination of its antioxidant activity.

    Science.gov (United States)

    Yin, Chaomin; Fan, Xiuzhi; Fan, Zhe; Shi, Defang; Gao, Hong

    2018-05-01

    Enzymes-microwave-ultrasound assisted extraction (EMUE) method had been used to extract Lentinus edodes polysaccharides (LEPs). The enzymatic temperature, enzymatic pH, microwave power and microwave time were optimized by response surface methodology. The yields, properties and antioxidant activities of LEPs from EMUE and other extraction methods including hot-water extraction, enzymes-assisted extraction, microwave-assisted extraction and ultrasound-assisted extraction were evaluated. The results showed that the highest LEPs yield of 9.38% was achieved with enzymatic temperature of 48°C, enzymatic pH of 5.0, microwave power of 440W and microwave time of 10min, which correlated well with the predicted value of 9.79%. Additionally, LEPs from different extraction methods possessed typical absorption peak of polysaccharides, which meant different extraction methods had no significant effects on type of glycosidic bonds and sugar ring of LEPs. However, SEM images of LEPs from different extraction methods were significantly different. Moreover, the different LEPs all showed antioxidant activities, but LEPs from EMUE showed the highest reducing power when compared to other LEPs. The results indicated LEPs from EMUE can be used as natural antioxidant component in the pharmaceutical and functional food industries. Copyright © 2018 Elsevier B.V. All rights reserved.

  20. 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.

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

    Science.gov (United States)

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

    2015-12-24

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

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

    Directory of Open Access Journals (Sweden)

    Dong-Ping Xu

    2015-12-01

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

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

    Science.gov (United States)

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

    2017-02-15

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

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

    Science.gov (United States)

    Li, Yong; Chen, Youliang; Li, Hua

    2017-01-01

    Response surface methodology was used to optimize ultrasound-assisted ethanol extraction (UAE) of cholesterol from cholesterol-β-cyclodextrin (C-β-CD) inclusion complex prepared from duck yolk oil. The best extraction conditions were solvent-solid ratio 10mL/g, ultrasonic power 251W, extraction temperature 56°C and sonication time 36min. Under these conditions, the highest cholesterol extraction yield and cholesterol content obtained 98.12±0.25% and 43.38±0.61mg/g inclusion complex, respectively. As compared with Reflux extraction and Soxhlet extraction, the UAE was more efficient and economical. To increase the purity of crude cholesterol extraction, silica gel column chromatography and crystallization were carried out. Finally, cholesterol was obtained at 95.1% purity, 71.7% recovery and 22.0% yield. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2013-01-01

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

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

    Science.gov (United States)

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

    2017-06-09

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

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

    Science.gov (United States)

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

    2017-09-01

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

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

    Science.gov (United States)

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

    2009-06-10

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

  9. 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.

  10. Double spike isotope dilution GC-ICP-MS for evaluation of mercury species transformation in real fish samples using ultrasound-assisted extraction.

    Science.gov (United States)

    Esteban-Fernández, Diego; Mirat, Manuela; de la Hinojosa, M Ignacia Martín; Alonso, J Ignacio García

    2012-08-29

    Sample preparation continues being a key factor to obtain fast and reliable quantification of Hg species. Assisted procedures enhance the efficiency and reduce the extraction time; however, collateral species transformations have been observed. Moreover, differential interconversions have been observed even between similar matrixes, which introduce an important uncertainty for real sample analysis. Trying to minimize Hg species transformations, we have tested a soft ultrasound-assisted extraction procedure. Species quantification and transformations have been evaluated using double spike isotope dilution analysis (IDA) together with gas chromatography inductively coupled plasma mass spectrometry (GC-ICP-MS) for a CRM material (Tort-2) and shark and swordfish muscle samples. Optimum extraction solution and sonication time led to quantitative extraction and accurate determination of MeHg and IHg in a short time, although different behaviors regarding species preservation were observed depending on the sample. Negligible species transformations were observed in the analysis of the CRM, while a small but significant demethylation factor was observed in the case of real samples. In comparison with other extraction procedures, species transformations became smaller, and fewer differences between fish species were found. Similar results were obtained for fresh and lyophilized samples of both fish samples, which permit one to analyze the fresh sample directly and save time in the sample preparation step. The high grade of species preservation and the affordability of the extraction procedure allow one to obtain accurate determinations even for routine laboratories using quantification techniques, which do not estimate species transformations.

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

    Directory of Open Access Journals (Sweden)

    Chunjian Zhao

    2012-09-01

    Full Text Available Ionic liquid based, ultrasound-assisted extraction was successfully applied to the extraction of phenolcarboxylic acids, carnosic acid and rosmarinic acid, from Rosmarinus officinalis. Eight ionic liquids, with different cations and anions, were investigated in this work and [C8mim]Br was selected as the optimal solvent. Ultrasound extraction parameters, including soaking time, solid–liquid ratio, ultrasound power and time, and the number of extraction cycles, were discussed by single factor experiments and the main influence factors were optimized by response surface methodology. The proposed approach was demonstrated as having higher efficiency, shorter extraction time and as a new alternative for the extraction of carnosic acid and rosmarinic acid from R. officinalis compared with traditional reference extraction methods. Ionic liquids are considered to be green solvents, in the ultrasound-assisted extraction of key chemicals from medicinal plants, and show great potential.

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

    Directory of Open Access Journals (Sweden)

    Ming-Chi Wei

    2015-01-01

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

  13. 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.

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

    Science.gov (United States)

    Hong, Show-Jen

    2015-01-01

    Oleanolic acid (OA) and ursolic acid (UA) were extracted from Hedyotis diffusa using a hyphenated procedure of ultrasound-assisted and supercritical carbon dioxide (HSC–CO2) extraction at different temperatures, pressures, cosolvent percentages, and SC–CO2 flow rates. The results indicated that these parameters significantly affected the extraction yield. The maximal yields of OA (0.917 mg/g of dry plant) and UA (3.540 mg/g of dry plant) were obtained at a dynamic extraction time of 110 min, a static extraction time of 15 min, 28.2 MPa, and 56°C with a 12.5% (v/v) cosolvent (ethanol/water = 82/18, v/v) and SC–CO2 flowing at 2.3 mL/min (STP). The extracted yields were then analyzed by high performance liquid chromatography (HPLC) to quantify the OA and UA. The present findings revealed that H. diffusa is a potential source of OA and UA. In addition, using the hyphenated procedure for extraction is a promising and alternative process for recovering OA and UA from H. diffusa at high concentrations. PMID:26089939

  15. [Determination of Arsenic in Food Package Aluminum by Ultrasound Assisted Solid Phase Extraction/ICP-AES].

    Science.gov (United States)

    Qin, Wen-xia; Gong, Qi; Li, Min; Deng, Li-xin; Mo, Li-shu; Li, Yan-lin

    2015-04-01

    Determination of arsenic in pure aluminum by inductively coupled plasma atomic emission spectrometry was interfered by aluminum matrix. The experiment showed that when the mass concentration of Al was greater than or equal to 5 000 times the As in the test solution, the measurement error was greater than 5%. In order to eliminate the interference, strong acid cation exchange fiber (SACEF) was used as solid phase extraction agent to adsorb Al(3+). The extraction conditions included amount of SACEF, extraction time, temperature and pH were investigated. The optimal extraction conditions were that 0.9000 g SACEF was used to extract the aluminum from the sample solution of pH 2.0 at 55 °C for 5 min with the ultrasonic assist, and in this case, the arsenic in the form of arsenic acid was not extracted and left in the solution for the determination. The results showed that after treating 10. 00 mL test solution containing 1.00 µg arsenic and 20.0 mg aluminum, arsenic did not lose. The mass concentration of residual aluminum in the raffinate was about 2,000 times the As, which had not interfered the determination of arsenic. The detection limit (3 s) was 0.027 µg · mL(-1) and quantification limit (10 s) was 0.0091 µg · mL(-1). The proposed method was successfully applied to the separation and determination of arsenic in the synthetic samples, the aluminum cans and the barbecue aluminum foil. Recovery was in the range of 98.3%-105% and RSD (n = 3) was in the range of 0.1%-4.3%. The results showed that the content of arsenic in the aluminum cans and the aluminum barbecue foil was below the limited value of national standard (GB/T 3190-2008).

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

    Directory of Open Access Journals (Sweden)

    Saeid Khodadoust

    2017-04-01

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

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

    Science.gov (United States)

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

    2016-04-15

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

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

    Directory of Open Access Journals (Sweden)

    Ammar Altemimi

    2015-04-01

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

  19. Direct ultrasound-assisted extraction and characterization of phenolic compounds from fresh houseleek (Sempervivum marmoreum L. leaves

    Directory of Open Access Journals (Sweden)

    Karabegović Ivana T.

    2018-01-01

    Full Text Available The effects of ultrasound power and frequency on the yield of total extractive substances (TES, total phenolic content (TPC, total flavonoid content (TFC and antioxidant activity (AOA of fresh houseleek leaves extracts obtained by direct ultrasound-assisted extraction (DUAE were studied. Preliminary extraction of plant material was performed using methanol, acetone and 2-propanol by Soxhlet extraction. It was found that maximum TES yield could be obtained by methanol extraction (2.91±0.02, followed by acetone and 2-propanol with a TES yield of 2.32±0.01 and 2.01±0.03 g per 100 g of fresh plant material, respectively. In the fresh houseleek leaves extracts obtained by DUAE and methanol as the chosen solvent, TPC, TFC and AOA were in the ranges of: 40.5–85.9 mg gallic acid/g dry extract, 12.7–19.3 mg rutin/g dry extract and 24.6–108.2μg/ml, respectively. The results showed that the increase in the ultrasound power and extraction time have positive and significant (p < 0.05 effects on the TPC, TFC and AOA, while the increase in the ultrasound frequency leads to a decrease in the TPC, TFC and AOA of the extracts. A chromatographic analysis of crude extract identified the following: kaempferol 3-O-(6’’-O-malonylglucoside- 7-O-glucosyde, kaempferol 3-O-glucoside-7-O-rhamnoside, luteolin 5-O-(6’’-O-malonylglucoside, kaempferol 3-O-(6’’-O-acetylglucoside-7-O-rhamnoside, genkwanin 5-O-glucoside, luteolin 5-O-(6’’-O-malonylglucoside, kaempferol 3-O-(6’’-O-malonylglucoside, kaempferol 3-O-rhamnoside, quercetin, genkwanin 4’-O-glucoside and hyperoside. [Project of the Serbian Ministry of Education, Science and Technological Development, Grant no. 172047

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

    Science.gov (United States)

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

    2017-05-01

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

  1. Development and validation of an efficient ultrasound assisted extraction of phenolic compounds from flax (Linum usitatissimum L.) seeds.

    Science.gov (United States)

    Corbin, Cyrielle; Fidel, Thibaud; Leclerc, Emilie A; Barakzoy, Esmatullah; Sagot, Nadine; Falguiéres, Annie; Renouard, Sullivan; Blondeau, Jean-Philippe; Ferroud, Clotilde; Doussot, Joël; Lainé, Eric; Hano, Christophe

    2015-09-01

    Flaxseed accumulates in its seedcoat a macromolecular complex composed of lignan (secoisolariciresinol diglucoside, SDG), flavonol (herbacetin diglucoside, HDG) and hydroxycinnamic acids (p-couramic, caffeic and ferulic acid glucosides). Their antioxidant and/or cancer chemopreventive properties support their interest in human health and therefore, the demand for their extraction. In the present study, ultrasound-assisted extraction (UAE) of flaxseed phenolic compounds was investigated. Scanning Electron Microscopy imaging and histochemical analysis revealed the deep alteration of the seedcoat ultrastructure and the release of the mucilage following ultrasound treatment. Therefore, this method was found to be very efficient for the reduction of mucilage entrapment of flaxseed phenolics. The optimal conditions for UAE phenolic compounds extraction from flaxseeds were found to be: water as solvent supplemented with 0.2N of sodium hydroxide for alkaline hydrolysis of the SDG-HMG complex, an extraction time of 60 min at a temperature of 25°C and an ultrasound frequency of 30 kHz. Under these optimized and validated conditions, highest yields of SDG, HDG and hydroxycinnamic acid glucosides were detected in comparison to other published methods. Therefore, the procedure presented herein is a valuable method for efficient extraction and quantification of the main flaxseed phenolics. Moreover, this UAE is of particular interest within the context of green chemistry in terms of reducing energy consumption and valuation of flaxseed cakes as by-products resulting from the production of flax oil. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    Directory of Open Access Journals (Sweden)

    Hui-Zhen LI

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

  3. Extraction of Natural Antioxidants from the Thelephora ganbajun Mushroom by an Ultrasound-Assisted Extraction Technique and Evaluation of Antiproliferative Activity of the Extract against Human Cancer Cells.

    Science.gov (United States)

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

    2016-10-01

    The Thelephora ganbajun mushroom has been found to be a potential rich source of natural antioxidants. In this study, an ultrasound-assisted extraction (UAE) technique together with GRAS (generally recognized as safe) solvents (ethanol and water) was used to maximize the extraction of antioxidants from Thelephora ganbajun . Five extraction parameters (ethanol concentration, solvent to solid ratio, extraction time, temperature and ultrasound power) were investigated by single-factor experiments, and then a central composite rotatable design was employed to study interaction of three key extraction parameters. The optimum conditions were as follows: 57.38% ethanol, 70.15 mL/g solvent to solid ratio, 10.58 min extraction time, 40 °C extraction temperature and 500 W ultrasound power. Under the optimum conditions, the antioxidant activity obtained was 346.98 ± 12.19 µmol Trolox/g DW, in accordance with the predicted value of 344.67 µmol Trolox/g DW. Comparison of UAE with conventional maceration and Soxhlet extraction, the UAE method showed stronger extract efficiency in a shorter extraction time. These results showed that UAE was an effective technique to extract antioxidants from Thelephora ganbajun . Furthermore, the extracts obtained under the optimized conditions exhibited antiproliferative activities toward human lung (A549), breast (MCF-7), liver (HepG2) and colon (HT-29) cancer cells, especially for liver and lung cancer cells. In addition, rutin, 2-hydrocinnamic acid and epicatechin were identified in the extract, which might contribute to antioxidant and antiproliferative activities.

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

    Science.gov (United States)

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

    2006-09-01

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

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

    Directory of Open Access Journals (Sweden)

    Şule Dinç Zor

    2017-09-01

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

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

    Directory of Open Access Journals (Sweden)

    Gui-Fang Deng

    2015-11-01

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

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

    International Nuclear Information System (INIS)

    Ilander, Aki; Vaeisaenen, Ari

    2007-01-01

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

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

    Science.gov (United States)

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

    2015-11-17

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

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

    Directory of Open Access Journals (Sweden)

    JOELIA M. BARROS

    2013-09-01

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

  10. 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.

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

    OpenAIRE

    Petigny, Lo?c; P?rino-Issartier, Sandrine; Wajsman, Jo?l; Chemat, Farid

    2013-01-01

    Vegetal extracts are widely used as primary ingredients for various products from creams to perfumes in the pharmaceutical, nutraceutic and cosmetic industries. Having concentrated and active extract is essential, as the process must extract as much soluble material as possible in a minimum time, using the least possible volume of solvent. The boldo leaves extract is of great interest for the industry as it holds a great anti-oxidant activity due to high levels of flavonoids and alkaloids suc...

  12. 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.

  13. Comparison of conventional and ultrasound-assisted extraction of carvone and limonene from caraway seeds

    NARCIS (Netherlands)

    Chemat, S.; Lagha, A.; AitAmar, H.; Bartels, P.V.; Chemat, F.

    2004-01-01

    Extraction experiments with hexane were carried out at atmospheric pressure in Soxhlet, conventional and ultrasound extractions of flaked caraway seeds, and detailed results are given for two major plant extract components, carvone and limonene. The results indicate that carvone yield and plant

  14. Evaluation of ultrasound-assisted in situ sorbent formation solid-phase extraction method for determination of arsenic in water, food and biological samples.

    Science.gov (United States)

    Ezoddin, Maryam; Majidi, Behrooz; Abdi, Khosrou

    2015-01-01

    A simple and rapid ultrasound-assisted in situ sorbent formation solid-phase extraction (UAISFSPE) coupled with electrothermal atomic absorption spectrometry detection (ET-AAS) was developed for preconcentration and determination of arsenic (As) in various samples. A small amount of cationic surfactant is dissolved in the aqueous sample containing As ions, which were complexed by ammonium pyrrolidinedithiocarbamate After shaking, a little volume of hexafluorophosphate (NaPF6) as an ion-pairing agent was added into the solution by a microsyringe. Due to the interaction between surfactant and ion-pairing agent, solid particles are formed. The alkyl groups of the surfactant in the solid particles strongly interact with the hydrophobic groups of analytes and become bound. Sonication aids the dispersion of the sorbent into the sample solution and mass transfer of the analyte into the sorbent, thus reducing the extraction time. The solid particles are centrifuged, and the sedimented particles can be dissolved in an appropriate solvent to recover the absorbed analyte. After separation, total arsenic (As(III) and As(V)) was determined by ET-AAS. Several experimental parameters were investigated and optimized. A detection limit of 7 ng L(-1) with preconcentration factor of 100 and relative standard deviation for 10 replicate determinations of 0.1 µg L(-1) As(III) were 4.5% achieved. Consequently, the method was applied to the determination of arsenic in certified reference materials, water, food and biological samples with satisfactory results.

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

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    Chunhui Ma

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

  17. Extraction of Natural Antioxidants from the Thelephora ganbajun Mushroom by an Ultrasound-Assisted Extraction Technique and Evaluation of Antiproliferative Activity of the Extract against Human Cancer Cells

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    Dong-Ping Xu

    2016-10-01

    Full Text Available The Thelephora ganbajun mushroom has been found to be a potential rich source of natural antioxidants. In this study, an ultrasound-assisted extraction (UAE technique together with GRAS (generally recognized as safe solvents (ethanol and water was used to maximize the extraction of antioxidants from Thelephora ganbajun. Five extraction parameters (ethanol concentration, solvent to solid ratio, extraction time, temperature and ultrasound power were investigated by single-factor experiments, and then a central composite rotatable design was employed to study interaction of three key extraction parameters. The optimum conditions were as follows: 57.38% ethanol, 70.15 mL/g solvent to solid ratio, 10.58 min extraction time, 40 °C extraction temperature and 500 W ultrasound power. Under the optimum conditions, the antioxidant activity obtained was 346.98 ± 12.19 µmol Trolox/g DW, in accordance with the predicted value of 344.67 µmol Trolox/g DW. Comparison of UAE with conventional maceration and Soxhlet extraction, the UAE method showed stronger extract efficiency in a shorter extraction time. These results showed that UAE was an effective technique to extract antioxidants from Thelephora ganbajun. Furthermore, the extracts obtained under the optimized conditions exhibited antiproliferative activities toward human lung (A549, breast (MCF-7, liver (HepG2 and colon (HT-29 cancer cells, especially for liver and lung cancer cells. In addition, rutin, 2-hydrocinnamic acid and epicatechin were identified in the extract, which might contribute to antioxidant and antiproliferative activities.

  18. The effects of temperature and frequencies in ultrasound assisted extraction of phycocyanin from microalgae Spirulina sp

    Energy Technology Data Exchange (ETDEWEB)

    Hadiyanto,, E-mail: hadiyanto@live.undip.ac.id; Suttrisnorhadi,; Soetrisnanto, Danny; Azizah, Nur [Department of Chemical Engineering, Diponegoro University, Jl. Prof. Soedarto, SH-Tembalang, Semarang 50239 INDONESIA (Indonesia); Sutanto, Heri [Physic Department, Faculty of Science and Mathematics, Diponegoro University (Indonesia); Suzery, Meiny [Chemistry Department, Faculty of Science and Mathematics, Diponegoro University (Indonesia)

    2015-12-29

    Microalgae Spirulina sp has been identified as source of protein and other high added value compounds. One of the compounds is phycocyanin as also known for antioxidant use. The extraction of this compound by using conventional method (soxhlet extraction) resulted low yield and longer processing time. This research was aimed to extract phycocyanin by using an extraction assisted by ultrasound irradiation. The extraction was performed by using variable of ultrasound frequency and extraction temperature and ethanol was used as a solvent. The result showed that yield of phycocyanin extracted by conventional method was 11.13% while the ultrasound irradiation could increase the yield up to 15.61% at constant frequency of 42 kHz, while the optimum temperature was obtained at 45°C. The analysis of variable interactions showed that both temperature and time has an interaction and temperature was the highest variable in increasing the yield. The conclusion of this research was the ultrasound could improve significantly the efficiency of extraction as well as activity of phycocyanin extracted from microalgae.

  19. The effects of temperature and frequencies in ultrasound assisted extraction of phycocyanin from microalgae Spirulina sp

    Science.gov (United States)

    Hadiyanto, Suttrisnorhadi, Sutanto, Heri; Suzery, Meiny; Soetrisnanto, Danny; Azizah, Nur

    2015-12-01

    Microalgae Spirulina sp has been identified as source of protein and other high added value compounds. One of the compounds is phycocyanin as also known for antioxidant use. The extraction of this compound by using conventional method (soxhlet extraction) resulted low yield and longer processing time. This research was aimed to extract phycocyanin by using an extraction assisted by ultrasound irradiation. The extraction was performed by using variable of ultrasound frequency and extraction temperature and ethanol was used as a solvent. The result showed that yield of phycocyanin extracted by conventional method was 11.13% while the ultrasound irradiation could increase the yield up to 15.61% at constant frequency of 42 kHz, while the optimum temperature was obtained at 45°C. The analysis of variable interactions showed that both temperature and time has an interaction and temperature was the highest variable in increasing the yield. The conclusion of this research was the ultrasound could improve significantly the efficiency of extraction as well as activity of phycocyanin extracted from microalgae.

  20. The effects of temperature and frequencies in ultrasound assisted extraction of phycocyanin from microalgae Spirulina sp

    International Nuclear Information System (INIS)

    Hadiyanto,; Suttrisnorhadi,; Soetrisnanto, Danny; Azizah, Nur; Sutanto, Heri; Suzery, Meiny

    2015-01-01

    Microalgae Spirulina sp has been identified as source of protein and other high added value compounds. One of the compounds is phycocyanin as also known for antioxidant use. The extraction of this compound by using conventional method (soxhlet extraction) resulted low yield and longer processing time. This research was aimed to extract phycocyanin by using an extraction assisted by ultrasound irradiation. The extraction was performed by using variable of ultrasound frequency and extraction temperature and ethanol was used as a solvent. The result showed that yield of phycocyanin extracted by conventional method was 11.13% while the ultrasound irradiation could increase the yield up to 15.61% at constant frequency of 42 kHz, while the optimum temperature was obtained at 45°C. The analysis of variable interactions showed that both temperature and time has an interaction and temperature was the highest variable in increasing the yield. The conclusion of this research was the ultrasound could improve significantly the efficiency of extraction as well as activity of phycocyanin extracted from microalgae

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

    Science.gov (United States)

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

    2009-08-01

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

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

    Science.gov (United States)

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

    2016-01-01

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

  3. Ultrasound assisted extraction of polyphenols and their distribution in whole mung bean, hull and cotyledon.

    Science.gov (United States)

    Singh, Barinderjit; Singh, Narpinder; Thakur, Sheetal; Kaur, Amritpal

    2017-03-01

    In this study, extraction of polyphenols using different solvents (acetone, ethanol, methanol and water) with ultrasound and conventional method from whole mung bean (WMB), hull and cotyledon was conducted. Total phenolic content (TPC), total flavonoids content (TFC), total antioxidant activities (TAA), ferric reducing power (FRP) and DPPH radical scavenging activity were determined. Ultrasound treated extracts exhibited higher TPC, TFC, TAA, FRP and DPPH in different mung bean fractions than CSE. Among the solvents, acetone showed better TPC, TFC, TAA, FRP and DPPH. Hull had significantly higher TPC, TFC, TAA, FRP and DPPH than WMB and cotyledon. Sinapic acid (SA) was the major polyphenol in different fractions. Acetone extract of hull showed high polyphenol content. SA, ferulic acid, catechin, p-coumaric acid, resveratrol, quercetin and luteolin were the major contributors to antioxidant activity of acetone extract. Mung bean hull contained the maximum polyphenols and acetone was observed to be the best extraction medium for polyphenols in combination with ultrasound.

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

    Directory of Open Access Journals (Sweden)

    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.

  5. Ultrasound-Assisted Extraction of Cannabinoids from Cannabis Sativa L. Optimized by Response Surface Methodology.

    Science.gov (United States)

    Agarwal, Charu; Máthé, Katalin; Hofmann, Tamás; Csóka, Levente

    2018-03-01

    Ultrasonication was used to extract bioactive compounds from Cannabis sativa L. such as polyphenols, flavonoids, and cannabinoids. The influence of 3 independent factors (time, input power, and methanol concentration) was evaluated on the extraction of total phenols (TPC), flavonoids (TF), ferric reducing ability of plasma (FRAP) and the overall yield. A face-centered central composite design was used for statistical modelling of the response data, followed by regression and analysis of variance in order to determine the significance of the model and factors. Both the solvent composition and the time significantly affected the extraction while the sonication power had no significant impact on the responses. The response predictions obtained at optimum extraction conditions of 15 min time, 130 W power, and 80% methanol were 314.822 mg GAE/g DW of TPC, 28.173 mg QE/g DW of TF, 18.79 mM AAE/g DW of FRAP, and 10.86% of yield. A good correlation was observed between the predicted and experimental values of the responses, which validated the mathematical model. On comparing the ultrasonic process with the control extraction, noticeably higher values were obtained for each of the responses. Additionally, ultrasound considerably improved the extraction of cannabinoids present in Cannabis. Low frequency ultrasound was employed to extract bioactive compounds from the inflorescence part of Cannabis. The responses evaluated were-total phenols, flavonoids, ferric reducing assay and yield. The solvent composition and time significantly influenced the extraction process. Appreciably higher extraction of cannabinoids was achieved on sonication against control. © 2018 Institute of Food Technologists®.

  6. Improvement of lipid yield from microalgae Spirulina platensis using ultrasound assisted osmotic shock extraction method

    Science.gov (United States)

    Adetya, NP; Hadiyanto, H.

    2018-01-01

    Microalgae Spirulina sp. has been identified as potential source of natural food supplement and food colorant. The high water content of microalgae (70-90%) causes an obstacle in biomass dehydration which requires large amounts of energy, eventually damaging the lipid in the microalgae. Therefore, the lipid must be extracted by using a suitable method which complies to wet biomass conditions. One of the methods is applying osmotic shock. This study was aimed to investigate the influence of osmotic agent (NaCl) concentration (10-30%) and extraction time (20-50 min) on yield of lipid and also to determine the optimal conditions in the extraction process through response surface methodology. The extraction was conducted at a temperature of 40°C under ultrasound frequency of 40 kHz. The result showed that the optimum yield lipid obtained was 6.39% in 16.98% NaCl concentration for 36 minutes 10 seconds.

  7. Pulsed counter-current ultrasound-assisted extraction and characterization of polysaccharides from Boletus edulis.

    Science.gov (United States)

    You, Qinghong; Yin, Xiulian; Ji, Chaowen

    2014-01-30

    Four methods for extracting polysaccharides from Boletus edulis, namely, hot-water extraction, ultrasonic clearer extraction, static probe ultrasonic extraction, and pulsed counter-current probe ultrasonic extraction (CCPUE), were studied. Results showed that CCPUE has the highest extraction efficiency among the methods studied. Under optimal CCPUE conditions, a B. edulis polysaccharide (BEP) yield of 8.21% was obtained. Three purified fractions, BEP-I, BEP-II, and BEP-III, were obtained through sequential purification by DEAE-52 and Sephadex G-75 chromatography. The average molecular weights of BEP-I, BEP-II, and BEP-III were 10,278, 23,761, and 42,736 Da, respectively. The polysaccharides were mainly composed of xylose, mannose, galactose, and glucose; of these, mannose contents were the highest. The antioxidant activities of the BEPs were further investigated by measurement of their ability to scavenge DPPH and hydroxyl radicals as well as their reducing power. The results indicated that the BEPs have good antioxidant activity. Copyright © 2013 Elsevier Ltd. All rights reserved.

  8. Ultrasound assisted methods for enhanced extraction of phycobiliproteins from marine macro-algae, Gelidium pusillum (Rhodophyta).

    Science.gov (United States)

    Mittal, Rochak; Tavanandi, Hrishikesh A; Mantri, Vaibhav A; Raghavarao, K S M S

    2017-09-01

    Extraction of phycobiliproteins (R-phycoerythrin, R-PE and R-phycocyanin, R-PC) from macro-algae is difficult due to the presence of large polysaccharides (agar, cellulose etc.) present in the cell wall which offer major hindrance for cell disruption. The present study is aimed at developing most suitable methodology for the primary extraction of R-PE and R-PC from marine macro-algae, Gelidium pusillum(Stackhouse) Le Jolis. Such extraction of phycobiliproteins by using ultrasonication and other conventional methods such as maceration, maceration in presence of liquid nitrogen, homogenization, and freezing and thawing (alone and in combinations) is reported for the first time. Standardization of ultrasonication for different parameters such as ultrasonication amplitude (60, 90 and 120µm) and ultrasonication time (1, 2, 4, 6, 8 and 10mins) at different temperatures (30, 35 and 40°C) was carried out. Kinetic parameters were estimated for extraction of phycobiliproteins by ultrasonication based on second order mass transfer kinetics. Based on calorimetric measurements, power, ultrasound intensity and acoustic power density were estimated to be 41.97W, 14.81W/cm 2 and 0.419W/cm 3 , respectively. Synergistic effect of ultrasonication was observed when employed in combination with other conventional primary extraction methods. Homogenization in combination with ultrasonication resulted in an enhancement in efficiency by 9.3% over homogenization alone. Similarly, maceration in combination with ultrasonication resulted in an enhancement in efficiency by 31% over maceration alone. Among all the methods employed, maceration in combination with ultrasonication resulted in the highest extraction efficiency of 77 and 93% for R-PE and R-PC, respectively followed by homogenization in combination with ultrasonication (69.6% for R-PE and 74.1% for R-PC). HPLC analysis was carried out in order to ensure that R-PE was present in the extract and remained intact even after processing

  9. EXTRACTION OF PHENOLIC COMPOUNDS FROM PETAI LEAVES (PARKIA SPECIOSA HASSK. USING MICROWAVE AND ULTRASOUND ASSISTED METHODS

    Directory of Open Access Journals (Sweden)

    Buanasari Buanasari

    2017-06-01

    Full Text Available The antioxidant has an activity to neutralize free radical compound that the body needs to avoid damage cells and tissues. Phenolic is one of the compounds that have an antioxidant activity. The influences of ultrasonic-assisted extraction (UAE and microwave-assisted extraction (MAE conditions on phenolic compounds of Parkia speciosa Hassk. leaves were investigated. The effects of temperature (40°C, 50°C, 60°C and 70°C, time (10, 30 and 50 minutes and material-solvent ratio (1:10, 1:13, 1:15 were evaluated based on the yield, total phenolic content (TPC and antioxidant activity. The result showed that the highest yield (15.82% was obtained at 1:15 (w/w of material-solvent ratio, 50°C of temperature and 50 minutes of extraction time for MAE. The highest yield of UAE is 15.53% that sample was obtained at 1:13 (w/w of material-solvent ratio, 60°C of optimal temperature and 30 minutes extraction time. The highest IC50 of UAE method extract was 52.55 ppm, while the extract obtained using MAE method was 50.44 ppm. UAE is more stable at higher temperatures. Time and solvent which was used more efficient than MAE. Extract of petai leaves (Parkia speciosa Hassk. were very potential to be used as a source of natural antioxidants because they have IC50 values from 41.39 to 66.00 ppm. Its antioxidants capacity is ranged from strong to very strong capacity.

  10. Determination of fragrance allergens in indoor air by active sampling followed by ultrasound-assisted solvent extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lamas, J Pablo; Sanchez-Prado, Lucia; Garcia-Jares, Carmen; Llompart, Maria

    2010-03-19

    Fragrances are ubiquitous pollutants in the environment, present in the most of household products, air fresheners, insecticides and cosmetics. Commercial perfumes may contain hundreds of individual fragrance chemicals. In addition to the widespread use and exposure to fragranced products, many of the raw fragrance materials have limited available health and safety data. Because of their nature as artificial fragrances, inhalation should be considered as an important exposure pathway, especially in indoor environments. In this work, a very simple, fast, and sensitive methodology for the analysis of 24 fragrance allergens in indoor air is presented. Considered compounds include those regulated by the EU Directive, excluding limonene; methyl eugenol was also included due to its toxicity. The proposed methodology is based on the use of a very low amount of adsorbent to retain the target compounds, and the rapid ultrasound-assisted solvent extraction (UAE) using a very low volume of solvent which avoids further extract concentration. Quantification was performed by gas chromatography coupled to mass spectrometry (GC-MS). The influence of main factors involved in the UAE step (type of adsorbent and solvent, solvent volume and extraction time) was studied using an experimental design approach to account for possible factor interactions. Using the optimized procedure, 0.2 m(-3) air are sampled, analytes are retained on 25 mg Florisil, from which they are extracted by UAE (5 min) with 2 mL ethyl acetate. Linearity was demonstrated in a wide concentration range. Efficiency of the total sampling-extraction process was studied at several concentration levels (1, 5 and 125 microg m(-3)), obtaining quantitative recoveries, and good precision (RSD<10%). Method detection limits were < or =0.6 microg m(-3). Finally, the proposed method was applied to real samples collected in indoor environments in which several of the target compounds were determined. Copyright 2010 Elsevier B

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

    Directory of Open Access Journals (Sweden)

    Arunachalam Thirunavukkarasu

    2018-03-01

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

  12. Ultrasound-assisted extraction and characterization of hydrolytic and oxidative enzymes produced by solid state fermentation.

    Science.gov (United States)

    Szabo, Orsolya Erzsebet; Csiszar, Emilia; Toth, Karolina; Szakacs, George; Koczka, Bela

    2015-01-01

    Ligninolytic and hydrolytic enzymes were produced with six selected fungi on flax substrate by solid state fermentation (SSF). The extracellular enzyme production of the organisms in two SSF media was evaluated by measuring the soluble protein concentration and the filter paper, endoxylanase, 1,4-β-d-glucosidase, 1,4-β-d-endoglucanase, polygalacturonase, lignin peroxidase, manganese peroxidase and laccase activities of the clear culture solutions produced by conventional extraction from the SSF materials. The SSF material of the best enzyme producer (Trichoderma virens TUB F-498) was further investigated to enhance the enzyme recovery by low frequency ultrasound treatment. Performance of both the original and ultrasound macerated crude enzyme mixtures was evaluated in degradation of the colored lignin-containing and waxy materials of raw linen fabric. Results proved that sonication (at 40%, 60% and 80% amplitudes, for 60min) did not result in reduction in the filter paper, lignin peroxidase and laccase activities of the crude enzyme solution, but has a significant positive effect on the efficiency of enzyme extraction from the SSF material. Depending on the parameters of sonication, the enzyme activities in the extracts obtained can be increased up to 129-413% of the original activities measured in the control extracts recovered by a common magnetic stirrer. Sonication also has an effect on both the enzymatic removal of the lignin-containing color materials and hydrophobic surface layer from the raw linen. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Optimization of ultrasound-assisted extraction of polyphenolic compounds from coriander seeds using response surface methodology

    Directory of Open Access Journals (Sweden)

    Zeković Zoran P.

    2016-01-01

    Full Text Available Coriandrum sativum L. (coriander seeds (CS were used for preparation of extracts with high content of biologically active compounds. In order to optimize ultrasoundassisted extraction process, three levels and three variables of Box-Behnken experimental design (BBD in combination with response surface methodology (RSM were applied, yielding maximized total phenolics (TP and flavonoids (TF content and antioxidant activity (IC50 and EC50 values. Independent variables were temperature (40-80oC, extraction time (40-80 min and ultrasonic power (96-216 W. Experimental results were fitted to a second-order polynomial model with multiple regression, while the analysis of variance (ANOVA was employed to assess the model fitness and determine optimal conditions for TP (79.60oC, 49.20 min, 96.69 W, TF (79.40oC, 43.60 min, 216.00 W, IC50 (80.00oC, 60.40 min, 216.00 W and EC50 (78.40oC, 68.60 min, 214.80 W. On the basis of the obtained mathematical models, three-dimensional surface plots were generated. The predicted values for TP, TF, IC50 and EC50 were: 382.68 mg GAE/100 g CS, 216 mg CE/100 g CS, 0.03764 mg/mL and 0.1425 mg/mL, respectively. [Projekat Ministarstva nauke Republike Srbije, br. TR31013

  14. 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.

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

    Science.gov (United States)

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

    2012-10-08

    In the present study, ultrasound-assisted extraction of crude oil from winter melon seeds was investigated through response surface methodology (RSM). Process variables were power level (25-75%), temperature (45-55 °C) and sonication time (20-40 min). It was found that all process variables have significant (p yield (108.62 mg-extract/g-dried matter). The antioxidant activity, total phenolic content and fatty acid composition of extract obtained under optimized conditions were determined and compared with those of oil obtained by the Soxhlet method. It was found that crude extract yield (CEY) of ultrasound-assisted extraction was lower than that of the Soxhlet method, whereas antioxidant activity and total phenolic content of the extract obtained by ultrasound-assisted extraction were clearly higher than those of the Soxhlet extract. Furthermore, both extracts were rich in unsaturated fatty acids. The major fatty acids of the both extracts were linoleic acid and oleic acid.

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

    Science.gov (United States)

    Cabrera-Peralta, Jerónimo; Peña-Alvarez, Araceli

    2018-05-01

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

  17. Ultrasound-assisted extraction and solid-phase extraction for the simultaneous determination of five amide herbicides in fish samples by gas chromatography with electron capture detection.

    Science.gov (United States)

    Qu, Zhipeng; Bai, Xiuzhi; Zhang, Ting; Yang, Zhaoguang

    2017-03-01

    An efficient sample extraction and clean-up method was developed for simultaneous determination of five amide herbicides (alachlor, acetochlor, propisochlor, metazachlor, and butachlor) in fish samples. The protocol consisted of ultrasound-assisted solvent extraction and solid-phase extraction clean-up. In detail, aliquots of homogenized fish flesh were thoroughly mixed with 20 mL of n-hexane and then extracted with ultrasonication for 40 min. Each sample was centrifuged and the supernatant was collected for the subsequent clean-up. For the sample preparation, the above supernatant was processed with a C 18 column with 3 mL of dichloromethane/n-hexane (1:1, v/v) as the eluant. Then the samples were analyzed by gas chromatography with electron capture detection. The correlation coefficients of the five calibration curves were 0.9976-0.9998 (n = 3). The limits of detection (S/N = 3, n = 11) and limits of quantification (S/N = 10, n = 11) were 0.19-0.42 and 0.63-1.39 μg/kg, respectively. The recoveries of this method were 71.2-92.6% with good precision (<4.7% relative standard deviations, n = 6). The developed method was successfully applied to monitor the five amide herbicides in fish samples collected from different cities. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Determination of total arsenic and arsenic(III) in phosphate fertilizers by hydride generation atomic absorption spectrometry after ultrasound-assisted extraction based on a control acid media.

    Science.gov (United States)

    Rezende, Helen Cristine; Coelho, Nivia Maria Melo

    2014-01-01

    An ultrasound-assisted extraction procedure was developed for determination of inorganic arsenic (As) in phosphate fertilizer by hydride generation atomic absorption spectrometry. The variables that affect the hydride generation step were optimized, including the reducer, acid, sample flow rate, and concentrations of the acid and reducer. The determination of As(lll) was performed through the simple control of solution pH with a 0.5 M citric acid-sodium citrate buffer solution at pH 4.5, and total As was determined after a pre-reduction reaction with 1.0% (w/v) thiourea. Ultrasound-assisted acid extraction was performed, and the parameters sonication time and acid and Triton X-114 concentrations were optimized using a 23 factorial design and central composite design. LODs for As(lll) and total As were 0.029 and 0.022 microg/L, respectively. The accuracy of the method was confirmed with certified reference materials. The method was successfully applied in the determination of inorganic As in phosphate fertilizer samples.

  19. Determination of gardenia yellow colorants in soft drink, pastry, instant noodles with ultrasound-assisted extraction by high performance liquid chromatography-electrospray ionization tandem mass spectrum.

    Science.gov (United States)

    Zhou, Wei-E; Zhang, Yuan; Li, Yang; Ling, Yun; Li, Hong-Na; Li, Shao-Hui; Jiang, Shou-Jun; Ren, Zhi-Qin; Huang, Zhi-Qiang; Zhang, Feng

    2016-05-13

    A novel, rapid and simple analytical method was developed for the quantitative determination of crocin, crocetin and geniposide in soft drink, pastry and instant noodles. The solid samples were relatively homogenized into powders and fragments. The gardenia yellow colorants were successively extracted with methanol using ultrasound-assisted extraction. The analytes were quantitatively measured in the extracts by liquid chromatography coupled with electrospray ionization tandem mass spectrometry. High correlation coefficients (r(2)>0.995) of crocin, crocetin and geniposide were obtained within their linear ranges respectively (50-1000ng/mL, 50-1000ng/mL, 15-240ng/mL) by external standard method. The limits of detection (LODs) were 0.02μg/g for crocin, 0.01μg/g for crocetin and 0.002μg/g for geniposide. And the limits of quantitation (LOQs) were in the ranges of 0.05-0.45μg/g for crocin, and in the ranges of 0.042-0.32μg/g for crocetin, and in the ranges of 0.02-0.15μg/g for geniposide in soft drink, pastry and instant noodles samples. The average recoveries of crocin, crocetin and geniposide ranged from 81.3% to 117.6% in soft drink, pastry and instant noodles. The intra- and inter-day precisions were respectively in the range of 1.3-4.8% and 1.7-11.8% in soft drink, pastry and instant noodle. The developed methods were successfully validated and applied to the soft drink, pastry, and instant noodles collected from the located market in Beijing from China. Crocin, crocetin and geniposide were detected in the collected samples. The average concentrations ranged from 0.84 to 4.20mg/g for crocin, and from 0.62 to 3.11mg/g for crocetin, and from 0.18 to 0.79mg/g for gardenia in various food samples. The method can provide evidences for government to determine gardenia yellow pigments and geniposide in food. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Comparison, artificial neural network modeling and genetic algorithm optimization of the resinoid and potassium yields from white lady’s bedstraw (Galium mollugo L. by conventional, reflux and ultrasound-assisted aqueous-ethanolic extraction

    Directory of Open Access Journals (Sweden)

    Milić Petar S.

    2013-01-01

    Full Text Available In this work, the yields of resinoid and potassium obtained from aerial parts of white lady’s bedstraw (Galium mollugo L. by maceration, reflux extraction and ultrasound-assisted extraction using aqueous ethanol solutions as solvents. The main goal was to define the influence of the extraction technique and the ethanol concentration on the resinoid and potassium yields. The resinoid and potassium yields were determined by the solvent evaporation from the liquid extracts to constant weight and the AAS emission method, respectively. The dependence of resinoid and potassium yields on the ethanol concentration was described by linear and quadratic polynomial models, respectively. The best potassium extraction selectivity of 0.077 g K/g of dry extract was achieved by maceration at the ethanol concentrations of 10 g/100 g. The artificial neural network (ANN was successfully applied to estimate the resinoid and potassium yields based on the ethanol concentration in the extracting solvent and the time duration for all three extraction techniques employed. The response surface methodology was also used to present the dependence of ANN results on the operating factors. The extraction process was optimized using the ANN model coupled with genetic algorithm. The maximum predicted resinoid and potassium yields of 30.4 and 1.67 g/100 g of dry plant were obtained by the ultrasonic extraction (80 min using the 10 g/100 g aqueous ethanol solution.

  1. A possible general mechanism for ultrasound-assisted extraction (UAE) suggested from the results of UAE of chlorogenic acid from Cynara scolymus L. (artichoke) leaves.

    Science.gov (United States)

    Saleh, I A; Vinatoru, M; Mason, T J; Abdel-Azim, N S; Aboutabl, E A; Hammouda, F M

    2016-07-01

    The use of ultrasound-assisted extraction (UAE) for the extraction of chlorogenic acid (CA) from Cynara scolymus L., (artichoke) leaves using 80% methanol at room temperature over 15 min gave a significant increase in yield (up to a 50%) compared with maceration at room temperature and close to that obtained by boiling over the same time period. A note of caution is introduced when comparing UAE with Soxhlet extraction because, in the latter case, the liquid entering the Soxhlet extractor is more concentrated in methanol (nearly 100%) that the solvent in the reservoir (80% methanol) due to fractionation during distillation. The mechanism of UAE is discussed in terms of the effects of cavitation on the swelling index, solvent diffusion and the removal of a stagnant layer of solvent surrounding the plant material. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Maceration of Extra Virgin Olive Oil with Common Aromatic Plants Using Ultrasound-Assisted Extraction: An UV-Vis Spectroscopic Investigation

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    Ozren Jović

    2018-01-01

    Full Text Available Rosemary (Rosmarinus officinalis, garden sage (Salvia officinalis, summer savory (Satureja hortensis, laurel (Laurus nobilis, and other aromatic plants were put in olive oil and exposed to ultrasounds for different duration. Filtrated oils were dissolved in cyclohexane, and UV-Vis measurements were carried out. Absorbance values corresponding to chlorophylls, carotenoids, flavonoids (370 nm, and polyphenols (around 300 nm were measured. In addition, for some samples, total phenols were determined using Folin-Denis reagent and compared with the similar maceration procedure in water solvent (instead of olive oil. Maceration without ultrasound in olive oil for each plant was also compared with ultrasound-assisted extraction. The results show that significant amount of aromatic content can be extracted in olive oil by applying ultrasounds for only few minutes, especially for Salvia officinalis powder. The use of UV-Vis measurements is simple but enough to examine the extent of phenol content extraction through such maceration procedure.

  3. Optimization of ultrasound-assisted aqueous two-phase system extraction of polyphenolic compounds from Aronia melanocarpa pomace by response surface methodology.

    Science.gov (United States)

    Xu, Yan-Yang; Qiu, Yang; Ren, Hui; Ju, Dong-Hu; Jia, Hong-Lei

    2017-03-16

    Aronia melanocarpa berries are abundant in polyphenolic compounds. After juice production, the pomace of pressed berries still contains a substantial amount of polyphenolic compounds. For efficient utilization of A. melanocarpa berries and the enhancement of polyphenolic compound yields in Aronia melanocarpa pomace (AMP), total phenolics (TP) and total flavonoids (TF) from AMP were extracted, using ultrasound-assisted aqueous two-phase system (UAE-ATPS) extraction method. First, the influences of ammonium sulfate concentration, ethanol-water ratio, ultrasonic time, and ultrasonic power on TP and TF yields were investigated. On this basis, process variables such as ammonium sulfate concentration (0.30-0.35 g mL -1 ), ethanol-water ratio (0.6-0.8), ultrasonic time (40-60 min), and ultrasonic power (175-225 W) were further optimized by implementing Box-Benhnken design with response surface methodology. The experimental results showed that optimal extraction conditions of TP from AMP were as follows: ammonium sulfate concentration of 0.324 g mL -1 , ethanol-water ratio of 0.69, ultrasonic time of 52 min, and ultrasonic power of 200 W. Meanwhile, ammonium sulfate concentration of 0.320 g mL -1 , ethanol-water ratio of 0.71, ultrasonic time of 50 min, and ultrasonic power of 200 W were determined as optimum extraction conditions of TF in AMP. Experimental validation was performed, where TP and TF yields reached 68.15 ± 1.04 and 11.67 ± 0.63 mg g -1 , respectively. Close agreement was found between experimental and predicted values. Overall, the present results demonstrated that ultrasound-assisted aqueous two-phase system extraction method was successfully used to extract total phenolics and flavonoids in A. melanocarpa pomace.

  4. Optimization of Ultrasound-Assisted Extraction, HPLC and UHPLC-ESI-Q-TOF-MS/MS Analysis of Main Macamides and Macaenes from Maca (Cultivars of Lepidium meyenii Walp

    Directory of Open Access Journals (Sweden)

    Shu-Xiao Chen

    2017-12-01

    Full Text Available Ultrasound-assisted extraction (UAE, using petroleum ether as the solvent, was systematically applied to extract main macamides and macaenes from Maca hypocotyls. Extraction yield was related with four variables, including ratio of solution to solid, extraction temperature, extraction time, and extraction power. On the basis of response surface methodology (RSM, the optimal conditions were determined to be the ratio of solution to solid as 10:1 (mL/g, the extraction temperature of 40 °C, the extraction time of 30 min, and the extraction power of 200 W. Based on the optimal extraction method of UAE, the total contents of ten main macamides and two main macaenes of Maca cultivated in twenty different areas of Tibet were analyzed by HPLC and UHPLC-ESI-Q-TOF-MS/MS. This study indicated that UAE was able to effectively extract macamides alkaloids from Maca hypocotyls. Quantitative analysis showed that geographical origins, not ecotypes, played a more important role on the accumulation of active macamides in Maca.

  5. Optimization of Ultrasound-Assisted Extraction, HPLC and UHPLC-ESI-Q-TOF-MS/MS Analysis of Main Macamides and Macaenes from Maca (Cultivars of Lepidium meyenii Walp).

    Science.gov (United States)

    Chen, Shu-Xiao; Li, Ke-Ke; Pubu, Duoji; Jiang, Si-Ping; Chen, Bin; Chen, Li-Rong; Yang, Zhen; Ma, Chao; Gong, Xiao-Jie

    2017-12-10

    Ultrasound-assisted extraction (UAE), using petroleum ether as the solvent, was systematically applied to extract main macamides and macaenes from Maca hypocotyls. Extraction yield was related with four variables, including ratio of solution to solid, extraction temperature, extraction time, and extraction power. On the basis of response surface methodology (RSM), the optimal conditions were determined to be the ratio of solution to solid as 10:1 (mL/g), the extraction temperature of 40 °C, the extraction time of 30 min, and the extraction power of 200 W. Based on the optimal extraction method of UAE, the total contents of ten main macamides and two main macaenes of Maca cultivated in twenty different areas of Tibet were analyzed by HPLC and UHPLC-ESI-Q-TOF-MS/MS. This study indicated that UAE was able to effectively extract macamides alkaloids from Maca hypocotyls. Quantitative analysis showed that geographical origins, not ecotypes, played a more important role on the accumulation of active macamides in Maca.

  6. Comparisons between conventional, ultrasound-assisted and microwave-assisted methods for extraction of anthraquinones from Heterophyllaea pustulata Hook f. (Rubiaceae).

    Science.gov (United States)

    Barrera Vázquez, M F; Comini, L R; Martini, R E; Núñez Montoya, S C; Bottini, S; Cabrera, J L

    2014-03-01

    This work reports a comparative study about extraction methods used to obtain anthraquinones (AQs) from stems and leaves of Heterophyllae pustulata Hook (Rubiáceae). One of the conventional procedures used to extract these metabolites from a vegetable matrix is by successive Soxhlet extractions with solvents of increasing polarity: starting with hexane to eliminate chlorophylls and fatty components, following by benzene and finally ethyl acetate. However, this technique shows a low extraction yield of total AQs, and consumes large quantities of solvent and time. Ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) have been investigated as alternative methods to extract these compounds, using the same sequence of solvents. It was found that UAE increases the extraction yield of total AQs and reduces the time and amount of solvent used. Nevertheless, the combination UAE with benzene, plus MAE with ethyl acetate at a constant power of 900 W showed the best results. A higher yield of total AQs was obtained in less time and using the same amount of solvent that UAE. The optimal conditions for this latter procedure were UAE with benzene at 50 °C during 60 min, followed by MAE at 900 W during 15 min using ethyl acetate as extraction solvent. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Effects of Ultrasound Assisted Extraction in Conjugation with Aid of Actinidin on the Molecular and Physicochemical Properties of Bovine Hide Gelatin

    Directory of Open Access Journals (Sweden)

    Tanbir Ahmad

    2018-03-01

    Full Text Available Actinidin was used to pretreat the bovine hide and ultrasonic wave (53 kHz and 500 W was used for the time durations of 2, 4 and 6 h at 60 °C to extract gelatin samples (UA2, UA4 and UA6, respectively. Control (UAC gelatin was extracted using ultrasound for 6 h at 60 °C without enzyme pretreatment. There was significant (p < 0.05 increase in gelatin yield as the time duration of ultrasound treatment increased with UA6 giving the highest yield of 19.65%. Gel strength and viscosity of UAC and UA6 extracted gelatin samples were 627.53 and 502.16 g and 16.33 and 15.60 mPa.s, respectively. Longer duration of ultrasound treatment increased amino acids content of the extracted gelatin and UAC exhibited the highest content of amino acids. Progressive degradation of polypeptide chains was observed in the protein pattern of the extracted gelatin as the time duration of ultrasound extraction increased. Fourier transform infrared (FTIR spectroscopy depicted loss of molecular order and degradation in UA6. Scanning electron microscopy (SEM revealed protein aggregation and network formation in the gelatin samples with increasing time of ultrasound treatment. The study indicated that ultrasound assisted gelatin extraction using actinidin exhibited high yield with good quality gelatin.

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

    Directory of Open Access Journals (Sweden)

    Miguel Ángel SÁNCHEZ-MADRIGAL

    Full Text Available Abstract The effects of ultrasound-assisted extraction (UAE at different ultrasound power densities (UPDs; 40, 80, and 120 mW/mL and solid:liquid (S:L ratio (1:2, 1:3, and 1:6 on the extraction of carbohydrates from Agave tequilana plant of different ages were evaluated. Extracts obtained (6- and 7-year-old plant were analyzed in the yield of carbohydrates (YC, fructan (FRU content, simple sugars, fructan profile and the average degree of polymerization (DPn. UPD, S:L ratio, and plant age all affected YC, FRU, and DPn. Maximum YC and FRU were obtained from the older agave with UPD and S:L ratio of 120 mW/mL and 1:6, respectively; while glucose, fructose, and sucrose were highly released from the younger plant. Agave of 7-year-old presented the highest DPn. Fructan degradation occurred at high UPD, increasing the simple sugars and decreasing the DPn. Thermal-traditional extraction without sonication caused more fructan degradation; and overall, ultrasound enhanced fructan extraction and minimized fructan damage, representing a technological alternative for fructan extraction from agave.

  9. Simultaneous optimization of the ultrasound-assisted extraction for phenolic compounds content and antioxidant activity of Lycium ruthenicum Murr. fruit using response surface methodology.

    Science.gov (United States)

    Chen, Shasha; Zeng, Zhi; Hu, Na; Bai, Bo; Wang, Honglun; Suo, Yourui

    2018-03-01

    Lycium ruthenicum Murr. (LR) is a functional food that plays an important role in anti-oxidation due to its high level of phenolic compounds. This study aims to optimize ultrasound-assisted extraction (UAE) of phenolic compounds and antioxidant activities of obtained extracts from LR using response surface methodology (RSM). A four-factor-three-level Box-Behnken design (BBD) was employed to discuss the following extracting parameters: extraction time (X 1 ), ultrasonic power (X 2 ), solvent to sample ratio (X 3 ) and solvent concentration (X 4 ). The analysis of variance (ANOVA) results revealed that the solvent to sample ratio had a significant influence on all responses, while the extraction time had no statistically significant effect on phenolic compounds. The optimum values of the combination of phenolic compounds and antioxidant activities were obtained for X 1 =30min, X 2 =100W, X 3 =40mL/g, and X 4 =33% (v/v). Five phenolic acids, including chlorogenic acid, caffeic acid, syringic acid, p-coumaric acid and ferulic acid, were analyzed by HPLC. Our results indicated that optimization extraction is vital for the quantification of phenolic compounds and antioxidant activity in LR, which may be contributed to large-scale industrial applications and future pharmacological activities research. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. Simultaneous ultrasound-assisted water extraction and β-cyclodextrin encapsulation of polyphenols from Mangifera indica stem bark in counteracting TNFα-induced endothelial dysfunction.

    Science.gov (United States)

    Mura, Marzia; Palmieri, Daniela; Garella, Davide; Di Stilo, Antonella; Perego, Patrizia; Cravotto, Giancarlo; Palombo, Domenico

    2015-01-01

    This study proposes an alternative technique to prevent heat degradation induced by classic procedures of bioactive compound extraction, comparing classical maceration/decoction in hot water of polyphenols from Mango (Mangifera indica L.) (MI) with ultrasound-assisted extraction (UAE) in a water solution of β-cyclodextrin (β-CD) at room temperature and testing their biological activity on TNFα-induced endothelial dysfunction. Both extracts counteracted TNFα effects on EAhy926 cells, down-modulating interleukin-6, interleukin-8, cyclooxygenase-2 and intracellular adhesion molecule-1, while increasing endothelial nitric oxide synthase levels. β-CD extract showed higher efficacy in improving endothelial function. These effects were abolished after pre-treatment with the oestrogen receptor inhibitor ICI1182,780. Moreover, the β-CD extract induced Akt activation and completely abolished the TNFα-induced p38MAPK phosphorylation. UAE and β-CD encapsulation provide an efficient extraction protocol that increases polyphenol bioavailability. Polyphenols from MI play a protective role on endothelial cells and may be further considered as oestrogen-like molecules with vascular protective properties.

  11. 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.

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

    Science.gov (United States)

    Bashi, Davoud Salar; Dowom, Samaneh Attaran; Bazzaz, Bibi Sedigheh Fazly; Khanzadeh, Farhad; Soheili, Vahid; Mohammadpour, Ali

    2016-05-01

    To optimize the extraction method using response surface methodology, extract the phenolic compounds, and identify the antioxidant and biological properties of Stachys parviflora L. extracts. Maceration and ultrasound-assisted extraction (UAE) (4, 7, 10 min treatment time, 40, 70, 100 % high-intensity and 60, 80, 100 % (v v-1) methanol purity) were applied to obtain the extracts. SEM was conducted to provide the microstructure of the extracted plant. MICs (colorimetric assay), MFCs (colony diameter), total phenolic content, total flavonoid content, radical scavenging capacity and extraction efficiency were determined. HPLC analysis was applied to measure the existent phenolic compounds. A quadratic model (4 min treatment time, 74.5 % high-intensity and 74.2 % solvent purity) was suggested as the best (TPC: 20.89 mg GAE g-1 d.m., TFC: 6.22 mg QEs g-1 d.m., DPPH IC50: 21.86 µg ml-1 and EE: 113.65 mg g-1 d.m.) UAE extraction model. The optimized UAE extract was generally more effective against Gram-positive microorganisms (MIC: 10-20; MBC: 10-40 (mg ml-1)) than Gram-negative ones (MIC: 40; MBC: >40 (mg ml-1)). Moreover, it (MGI: 2.32-100 %) revealed more anti-mold activity than maceration (MGI: <28.77 %). Explosive disruption of the cell walls, therefore, enhanced extraction yield by acoustic cavitation, was elucidated using SEM. Caffeic acid, tannic acid, quercetin, trans ferulic acid and rosmarinic acid were determined as the phenolic compounds in the optimized extract. RSM optimization was successfully applied for UAE from S. parviflora. The considerable antioxidant and biological properties were attributed to the phenolic compounds.

  13. Optimization of Ultrasound-Assisted Extraction of Crude Oil from Winter Melon (Benincasa hispida Seed Using Response Surface Methodology and Evaluation of Its Antioxidant Activity, Total Phenolic Content and Fatty Acid Composition

    Directory of Open Access Journals (Sweden)

    Md. Zaidul Islam Sarker

    2012-10-01

    Full Text Available In the present study, ultrasound-assisted extraction of crude oil from winter melon seeds was investigated through response surface methodology (RSM. Process variables were power level (25–75%, temperature (45–55 °C and sonication time (20–40 min. It was found that all process variables have significant (p < 0.05 effects on the response variable. A central composite design (CCD was used to determine the optimum process conditions. Optimal conditions were identified as 65% power level, 52 °C temperature and 36 min sonication time for maximum crude yield (108.62 mg-extract/g-dried matter. The antioxidant activity, total phenolic content and fatty acid composition of extract obtained under optimized conditions were determined and compared with those of oil obtained by the Soxhlet method. It was found that crude extract yield (CEY of ultrasound-assisted extraction was lower than that of the Soxhlet method, whereas antioxidant activity and total phenolic content of the extract obtained by ultrasound-assisted extraction were clearly higher than those of the Soxhlet extract. Furthermore, both extracts were rich in unsaturated fatty acids. The major fatty acids of the both extracts were linoleic acid and oleic acid.

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

    Directory of Open Access Journals (Sweden)

    Davoud Salarbashi

    2016-05-01

    Full Text Available Objective(s:To optimize the extraction method using response surface methodology, extract the phenolic compounds, and identify the antioxidant and biological properties of Stachys parviflora L.  extracts. Materials and Methods: Maceration and ultrasound-assisted extraction (UAE (4, 7, 10 min treatment time, 40, 70, 100 % high-intensity and 60, 80, 100 % (v v-1 methanol purity were applied to obtain the extracts. SEM was conducted to provide the microstructure of the extracted plant. MICs (colorimetric assay, MFCs (colony diameter, total phenolic content, total flavonoid content, radical scavenging capacity and extraction efficiency were determined. HPLC analysis was applied to measure the existent phenolic compounds. Results: A quadratic model (4 min treatment time, 74.5 % high-intensity and 74.2 % solvent purity was suggested as the best (TPC: 20.89 mg GAE g-1 d.m., TFC: 6.22 mg QEs g-1 d.m., DPPH IC50: 21.86 µg ml-1 and EE: 113.65 mg g-1 d.m. UAE extraction model. The optimized UAE extract was generally more effective against Gram-positive microorganisms (MIC: 10-20; MBC: 10-40 (mg ml-1 than Gram-negative ones (MIC: 40; MBC: >40 (mg ml-1. Moreover, it (MGI: 2.32-100 % revealed more anti-mold activity than maceration (MGI: Conclusion: RSM optimization was successfully applied for UAE from S. parviflora. The considerable antioxidant and biological properties were attributed to the phenolic compounds.

  15. Ultrasound-assisted extraction technique for establishing selenium contents in breast cancer biopsies by Zeeman-electrothermal atomic absorption spectrometry using multi-injection

    International Nuclear Information System (INIS)

    Lavilla, I.; Mosquera, A.; Millos, J.; Cameselle, J.; Bendicho, C.

    2006-01-01

    A solid-liquid extraction method is developed to establish the contents of selenium in breast cancer biopsies. The method is based on the ultrasound-assisted extraction of selenium from pretreated biopsies prior to Se determination by atomic absorption spectrometry with longitudinal-Zeeman background correction. Fifty-one breast biopsies were collected from the Cies Hospital (Vigo, Spain), 32 of which correspond to tumor tissue and 19 to normal tissue (parenchyma). Difficulties arising from the samples analyzed, i.e. small samples mass (50-100 mg), extremely low Se contents and sample texture modification including tissue hardening due to formaldehyde preservation are addressed and overcome. High intensity sonication using a probe together with addition of hydrogen peroxide succeeded in completely extracting Se from biopsies. The multiple injection technique was useful to tackle the low Se contents present in some biopsies. The detection limit was 25 ng g -1 of Se and the precision, expressed as relative standard deviation, was less than 10%. Se contents ranged from 0.08 to 0.4 μg g -1 for parenchyma samples and from 0.09 to 0.8 μg g -1 for tumor samples. In general, Se levels in tumor biopsies were higher as compared with the adjacent normal tissue in 19 patients by a factor of up to 6. Analytical data confirmed Se accumulation in the breast tumors

  16. 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)

  17. Ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME)-a fast new approach to measure phthalate metabolites in nails.

    Science.gov (United States)

    Alves, Andreia; Vanermen, Guido; Covaci, Adrian; Voorspoels, Stefan

    2016-09-01

    A new, fast, and environmentally friendly method based on ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME) was developed and optimized for assessing the levels of seven phthalate metabolites (including the mono(ethyl hexyl) phthalate (MEHP), mono(2-ethyl-5-hydroxyhexyl) phthalate (5-OH-MEHP), mono(2-ethyl-5-oxohexyl) phthalate (5-oxo-MEHP), mono-n-butyl phthalate (MnBP), mono-isobutyl phthalate (MiBP), monoethyl phthalate (MEP), and mono-benzyl phthalate (MBzP)) in human nails by UPLC-MS/MS. The optimization of the US-DLLME method was performed using a Taguchi combinatorial design (L9 array). Several parameters such as extraction solvent, solvent volume, extraction time, acid, acid concentration, and vortex time were studied. The optimal extraction conditions achieved were 180 μL of trichloroethylene (extraction solvent), 2 mL trifluoroacetic acid in methanol (2 M), 2 h extraction and 3 min vortex time. The optimized method had a good precision (6-17 %). The accuracy ranged from 79 to 108 % and the limit of method quantification (LOQm) was below 14 ng/g for all compounds. The developed US-DLLME method was applied to determine the target metabolites in 10 Belgian individuals. Levels of the analytes measured in nails ranged between <12 and 7982 ng/g. The MEHP, MBP isomers, and MEP were the major metabolites and detected in every sample. Miniaturization (low volumes of organic solvents used), low costs, speed, and simplicity are the main advantages of this US-DLLME based method. Graphical Abstract Extraction and phase separation of the US-DLLME procedure.

  18. Determination of Pb in river water samples by inductively coupled plasma optical emission spectrometry after ultrasound-assisted co-precipitation with manganese dioxide

    International Nuclear Information System (INIS)

    Sousa Bispo, Marcia; Santos da Boa Morte, Elane; Korn das Gracas Andrade, Maria; Sena Gomes Teixeira, Leonardo; Korn, Mauro; Costa, Antonio Celso Spinola

    2005-01-01

    A simple and efficient procedure for separation and pre-concentration using ultrasound-assisted co-precipitation with manganese dioxide was developed for Pb determination by inductively coupled plasma optical emission spectrometry (ICP OES). The optimization process was carried out using a two-level factorial design and a Doehlert matrix. Three variables (i.e. concentration of oxidizing solution-KMnO 4 , concentration of MnSO 4 solution and time of ultrasonic irradiation) were used as factors in the optimization. The recoveries, based on the analysis of spiked samples, were between 90% and 105%, and the precision was ≤ 5%. The detection limit and quantification limit for Pb determination were 3.2 and 10.7 μg L -1 , respectively. The proposed method was applied for the determination of Pb in water samples from a river heavily polluted by industrial effluents. The recovery measured by analyte addition technique showed that the proposed pre-concentration method had good accuracy

  19. Development and Validation of a HPLC-UV Method for the Evaluation of Ellagic Acid in Liquid Extracts of Eugenia uniflora L. (Myrtaceae Leaves and Its Ultrasound-Assisted Extraction Optimization

    Directory of Open Access Journals (Sweden)

    Paulo Isaac Dias Assunção

    2017-01-01

    Full Text Available A simple HPLC-UV method has been developed and validated for the quantification of ellagic acid (EA in ethanol extracts of Eugenia uniflora L. (Myrtaceae leaves. The ultrasound-assisted extraction (UAE optimization was performed using a Box Behnken design (33 combined with response surface methodology to study the effects of the ethanol concentration (%, w/w, extraction time (minutes, and temperature (°C on the EA concentration. The optimized results showed that the highest extraction yield of EA by UAE was 26.0 μg mL−1 when using 44% (w/w ethanol as the solvent, 22 minutes as the extraction time, and 59°C as the extraction temperature. The concentration of EA in relation to the predicted value was 93.7%  ±  0.4. UAE showed a strong potential for EA extraction.

  20. Development and Validation of a HPLC-UV Method for the Evaluation of Ellagic Acid in Liquid Extracts of Eugenia uniflora L. (Myrtaceae) Leaves and Its Ultrasound-Assisted Extraction Optimization.

    Science.gov (United States)

    Assunção, Paulo Isaac Dias; da Conceição, Edemilson Cardoso; Borges, Leonardo Luiz; de Paula, Joelma Abadia Marciano

    2017-01-01

    A simple HPLC-UV method has been developed and validated for the quantification of ellagic acid (EA) in ethanol extracts of Eugenia uniflora L. (Myrtaceae) leaves. The ultrasound-assisted extraction (UAE) optimization was performed using a Box Behnken design (3 3 ) combined with response surface methodology to study the effects of the ethanol concentration (%, w/w), extraction time (minutes), and temperature (°C) on the EA concentration. The optimized results showed that the highest extraction yield of EA by UAE was 26.0  μ g mL -1 when using 44% (w/w) ethanol as the solvent, 22 minutes as the extraction time, and 59°C as the extraction temperature. The concentration of EA in relation to the predicted value was 93.7%  ±  0.4. UAE showed a strong potential for EA extraction.

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

    Science.gov (United States)

    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.

  2. Ultrasound-assisted extraction of azadirachtin from dried entire fruits of Azadirachta indica A. Juss. (Meliaceae) and its determination by a validated HPLC-PDA method.

    Science.gov (United States)

    de Paula, Joelma Abadia Marciano; Brito, Lucas Ferreira; Caetano, Karen Lorena Ferreira Neves; de Morais Rodrigues, Mariana Cristina; Borges, Leonardo Luiz; da Conceição, Edemilson Cardoso

    2016-01-01

    Azadirachta indica A. Juss., also known as neem, is a Meliaceae family tree from India. It is globally known for the insecticidal properties of its limonoid tetranortriterpenoid derivatives, such as azadirachtin. This work aimed to optimize the azadirachtin ultrasound-assisted extraction (UAE) and validate the HPLC-PDA analytical method for the measurement of this marker in neem dried fruit extracts. Box-Behnken design and response surface methodology (RSM) were used to investigate the effect of process variables on the UAE. Three independent variables, including ethanol concentration (%, w/w), temperature (°C), and material-to-solvent ratio (gmL(-1)), were studied. The azadirachtin content (µgmL(-1)), i.e., dependent variable, was quantified by the HPLC-PDA analytical method. Isocratic reversed-phase chromatography was performed using acetonitrile/water (40:60), a flow of 1.0mLmin(-1), detection at 214nm, and C18 column (250×4.6mm(2), 5µm). The primary validation parameters were determined according to ICH guidelines and Brazilian legislation. The results demonstrated that the optimal UAE condition was obtained with ethanol concentration range of 75-80% (w/w), temperature of 30°C, and material-to-solvent ratio of 0.55gmL(-1). The HPLC-PDA analytical method proved to be simple, selective, linear, precise, accurate and robust. The experimental values of azadirachtin content under optimal UAE conditions were in good agreement with the RSM predicted values and were superior to the azadirachtin content of percolated extract. Such findings suggest that UAE is a more efficient extractive process in addition to being simple, fast, and inexpensive. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Ultrasound assisted extraction of polysaccharides from Lentinus edodes and its anti-hepatitis B activity in vitro.

    Science.gov (United States)

    Zhao, Yong-Ming; Yang, Jian-Ming; Liu, Ying-Hui; Zhao, Ming; Wang, Jin

    2018-02-01

    The aim of this study was to optimize the extraction process of polysaccharides from the fruiting bodies of Lentinus edodes and investigate its anti-hepatitis B virus activity. The extracting parameters including ultrasonic power (240-320W), extraction temperature (40-60°C) and extraction time (15-25min) was optimized by using three-variable-three-level Box-Behnken design based on the single-factor experiments. Data analysis results showed that the optimal conditions for extracting LEPs were an extraction temperature of 45°C, extraction time of 21min and ultrasonic power of 290W. Under these optimal conditions, the experimental yield of LEPs was 9.75%, a 1.62-fold increase compared with conventional heat water extraction (HWE). In addition, crude polysaccharides were purified to obtain two fractions (LEP-1 and LEP-2). Chemical analysis showed that these components were rich in glucose, arabinose and mannose. Furthermore, HepG2.2.15 cells were used as in vitro models to evaluate their anti-hepatitis B virus (HBV) activity. The results suggest that LEPs possesses potent anti-HBV activity in vitro. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Fast determination of trace elements in organic fertilizers using a cup-horn reactor for ultrasound-assisted extraction and fast sequential flame atomic absorption spectrometry.

    Science.gov (United States)

    Teixeira, Leonel Silva; Vieira, Heulla Pereira; Windmöller, Cláudia Carvalhinho; Nascentes, Clésia Cristina

    2014-02-01

    A fast and accurate method based on ultrasound-assisted extraction in a cup-horn sonoreactor was developed to determine the total content of Cd, Co, Cr, Cu, Mn, Ni, Pb and Zn in organic fertilizers by fast sequential flame atomic absorption spectrometry (FS FAAS). Multivariate optimization was used to establish the optimal conditions for the extraction procedure. An aliquot containing approximately 120 mg of the sample was added to a 500 µL volume of an acid mixture (HNO3/HCl/HF, 5:3:3, v/v/v). After a few minutes, 500 µL of deionized water was added and eight samples were simultaneously sonicated for 10 min at 50% amplitude, allowing a sample throughput of 32 extractions per hour. The performance of the method was evaluated with a certified reference material of sewage sludge (CRM 029). The precision, expressed as the relative standard deviation, ranged from 0.58% to 5.6%. The recoveries of analytes were found to 100%, 109%, 96%, 92%, 101%, 104% and 102% for Cd, Cr, Cu, Mn, Ni, Pb and Zn, respectively. The linearity, limit of detection and limit of quantification were calculated and the values obtained were adequate for the quality control of organic fertilizers. The method was applied to the analysis of several commercial organic fertilizers and organic wastes used as fertilizers, and the results were compared with those obtained using the microwave digestion procedure. A good agreement was found between the results obtained by microwave and ultrasound procedures with recoveries ranging from 80.4% to 117%. Two organic waste samples were not in accordance with the Brazilian legislation regarding the acceptable levels of contaminants. © 2013 Published by Elsevier B.V.

  5. Extraction of bioactives from Orthosiphon stamineus using microwave and ultrasound-assisted techniques: Process optimization and scale up.

    Science.gov (United States)

    Chan, Chung-Hung; See, Tiam-You; Yusoff, Rozita; Ngoh, Gek-Cheng; Kow, Kien-Woh

    2017-04-15

    This work demonstrated the optimization and scale up of microwave-assisted extraction (MAE) and ultrasonic-assisted extraction (UAE) of bioactive compounds from Orthosiphon stamineus using energy-based parameters such as absorbed power density and absorbed energy density (APD-AED) and response surface methodology (RSM). The intensive optimum conditions of MAE obtained at 80% EtOH, 50mL/g, APD of 0.35W/mL, AED of 250J/mL can be used to determine the optimum conditions of the scale-dependent parameters i.e. microwave power and treatment time at various extraction scales (100-300mL solvent loading). The yields of the up scaled conditions were consistent with less than 8% discrepancy and they were about 91-98% of the Soxhlet extraction yield. By adapting APD-AED method in the case of UAE, the intensive optimum conditions of the extraction, i.e. 70% EtOH, 30mL/g, APD of 0.22W/mL, AED of 450J/mL are able to achieve similar scale up results. Copyright © 2016 Elsevier Ltd. All rights reserved.

  6. Ultrasound assisted combined molecularly imprinted polymer for selective extraction of nicotinamide in human urine and milk samples: Spectrophotometric determination and optimization study.

    Science.gov (United States)

    Asfaram, Arash; Ghaedi, Mehrorang; Dashtian, Kheibar

    2017-01-01

    Ultrasound-assisted dispersive solid phase microextraction followed by UV-vis spectrophotometer (UA-DSPME-UV-vis) was designed for extraction and preconcentration of nicotinamide (vitamin B 3 ) by HKUST-1 metal organic framework (MOF) based molecularly imprinted polymer (MIP). This new material was characterized by FTIR and FE-SEM techniques. The preliminary Plackett-Burman design was used for screening and subsequently the central composite design justifies significant terms and possible construction of mathematical equation which give the individual and cooperative contribution of variables like HKUST-1-MOF-NA-MIP mass, sonication time, temperature, eluent volume, pH and vortex time. Accordingly the optimum condition was set as: 2.0mg HKUST-1-MOF-NA-MIP, 200μL eluent and 5.0min sonication time in center points other variables were determined as the best conditions to reach the maximum recovery of the analyte. The UA-DSPME-UV-vis method performances like excellent linearity (LR), limits of detection (LOD), limits of quantification of 10-5000μgL -1 with R 2 of 0.99, LOD (1.96ngmL -1 ), LOQ (6.53μgL -1 ), respectively show successful and accurate applicability of the present method for monitoring analytes with within- and between-day precision of 0.96-3.38%. The average absolute recoveries of the nicotinamide extracted from the urine, milk and water samples were 95.85-101.27%. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Ultrasound assisted extraction of bioactive compounds from Nephelium lappaceum L. fruit peel using central composite face centered response surface design

    Directory of Open Access Journals (Sweden)

    J. Prakash Maran

    2017-02-01

    Full Text Available In this study, four factors at three level central composite face centered design was employed to study and optimize the process variables on extraction of bioactive compounds (total anthocyanin, phenolic and flavonoid content from Nephelium lappaceum L. fruit peel. The effect of process variables such as extraction temperature (30–50 °C, power of ultrasound (20–40 W, extraction time (10–30 min and solid–liquid ratio (1:10–1:20 g/ml is studied. Multiple regression analysis was done on the experimental data to develop second-order polynomial models with high coefficient of determination value (R2 > 0.99. The optimal conditions based on both individual and combinations of all process variables (extraction temperature of 50 °C, ultrasound power of 20 W, extraction time of 20 min and solid–liquid ratio of 1:18.6 g/ml were determined by Derringer’s desired function methodology. Under these conditions, total anthocyanin (10.26 ± 0.39 (mg/100 g, phenolics (552.64 ± 1.57 (mg GAE/100 g and flavonoid (104 ± 1.13 (mg RE/100 g content values were determined and it is closely related with the predicted values (10.17 mg/100 g of total anthocyanin, 546.98 mg GAE/100 g of total phenolics and 100.93 mg RE/100 g of total flavonoid content and indicted the suitability of the developed models.

  8. Optimisation of Ultrasound-Assisted Extraction Conditions for Phenolic Content and Antioxidant Capacity from Euphorbia tirucalli Using Response Surface Methodology

    Science.gov (United States)

    Vuong, Quan V.; Goldsmith, Chloe D.; Dang, Trung Thanh; Nguyen, Van Tang; Bhuyan, Deep Jyoti; Sadeqzadeh, Elham; Scarlett, Christopher J.; Bowyer, Michael C.

    2014-01-01

    Euphorbia tirucalli (E. tirucalli) is now widely distributed around the world and is well known as a source of traditional medicine in many countries. This study aimed to utilise response surface methodology (RSM) to optimise ultrasonic-assisted extraction (UAE) conditions for total phenolic compounds (TPC) and antioxidant capacity from E. tirucalli leaf. The results showed that ultrasonic temperature, time and power effected TPC and antioxidant capacity; however, the effects varied. Ultrasonic power had the strongest influence on TPC; whereas ultrasonic temperature had the greatest impact on antioxidant capacity. Ultrasonic time had the least impact on both TPC and antioxidant capacity. The optimum UAE conditions were determined to be 50 °C, 90 min. and 200 W. Under these conditions, the E. tirucalli leaf extract yielded 2.93 mg GAE/g FW of TPC and exhibited potent antioxidant capacity. These conditions can be utilised for further isolation and purification of phenolic compounds from E. tirucalli leaf. PMID:26785074

  9. Selective determination of caffeine in foods with 3D-graphene based ultrasound-assisted magnetic solid phase extraction.

    Science.gov (United States)

    Rahimi, Afshin; Zanjanchi, Mohammad Ali; Bakhtiari, Sadjad; Dehsaraei, Mohammad

    2018-10-01

    An efficient method was applied for extraction of caffeine in food samples. Three-dimensional graphene-Fe 3 O 4 (3D-G-Fe 3 O 4 ) nanoparticles was successfully synthesized and used as adsorbent in magnetic solid phase extraction (MSPE) step. The properties of synthesized adsorbent were characterized by fourier-transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), vibrating sample magnetometer (VSM), X-ray diffraction (XRD), Raman spectroscopy, Brunauer-Emmett-Teller (BET) and Barrett-Joyner-Halenda (BJH) methods. The influence of main parameters of extraction procedure such as ultrasound parameter, amount of nanoparticles, pH, salt concentration and desorption condition were investigated and optimized. Under the optimized experimental conditions, the figure of merit results showed excellent linear dynamic range (LDR) of 0.5-500 µg mL -1 , with determination coefficient (R 2 ) higher than 0.996 and limit of detection (LOD) of 0.1 µg mL -1 . Intra- and inter-day relative standard deviations (RSDs) were less than 5.9 and 7.1%, respectively. The method was successfully applied for determination of caffeine in different food samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

  10. Utility of ultrasound assisted-cloud point extraction and spectophotometry as a preconcentration and determination tool for the sensitive quantification of mercury species in fish samples

    Science.gov (United States)

    Altunay, Nail

    2018-01-01

    The current study reports, for the first time, the development of a new analytical method employing ultrasound assisted-cloud point extraction (UA-CPE) for the extraction of CH3Hg+ and Hg2 + species from fish samples. Detection and quantification of mercury species were performed at 550 nm by spectrophotometry. The analytical variables affecting complex formation and extraction efficiency were extensively evaluated and optimized by univariate method. Due to behave 14-fold more sensitive and selective of thiophene 2,5-dicarboxylic acid (H2TDC) to Hg2 + ions than CH3Hg+ in presence of mixed surfactant, Tween 20 and SDS at pH 5.0, the amounts of free Hg2 + and total Hg were spectrophotometrically established at 550 nm by monitoring Hg2 + in the pretreated- and extracted-fish samples in ultrasonic bath to speed up extraction using diluted acid mixture (1:1:1, v/v, 4 mol L- 1 HNO3, 4 mol L- 1 HCl, and 0.5 mol L- 1 H2O2), before and after pre-oxidation with permanganate in acidic media. The amount of CH3Hg+ was calculated from difference between total Hg and Hg2 + amounts. The UA-CPE method showed to be suitable for the extraction and determination of mercury species in certified reference materials. The results were in a good agreement (with Student's t-test at 95% confidence limit) with the certified values, and the relative standard deviation was lower than 3.2%. The limits of detection have been 0.27 and 1.20 μg L- 1, for Hg2 + from aqueous calibration solutions and matrix-matched calibration solutions spiked before digestion, respectively, while it is 2.43 μg L- 1 for CH3Hg+ from matrix-matched calibration solutions. A significant matrix effect was not observed from comparison of slopes of both calibration curves, so as to represent the sample matrix. The method was applied to fish samples for speciation analysis of Hg2 + and CH3Hg+. In terms of speciation, while total Hg is detected in range of 2.42-32.08 μg kg- 1, the distribution of mercury in fish were in

  11. Development of "ultrasound-assisted dynamic extraction" and its combination with CCC and CPC for simultaneous extraction and isolation of phytochemicals.

    Science.gov (United States)

    Zhang, Yuchi; Liu, Chunming; Li, Jing; Qi, Yanjuan; Li, Yuchun; Li, Sainan

    2015-09-01

    A new method for the extraction of medicinal herbs termed ultrasonic-assisted dynamic extraction (UADE) was designed and evaluated. This technique was coupled with counter-current chromatography (CCC) and centrifugal partition chromatography (CPC) and then applied to the continuous extraction and online isolation of chemical constituents from Paeonia lactiflora Pall (white peony) roots. The mechanical parameters, including the pitch and diameter of the shaft, were optimized by means of mathematical modeling. Furthermore, the configuration and mechanism of online UADE coupled with CCC and CPC were elaborated. The stationary phases of the two-phase solvent systems from CCC and CPC were utilized as the UADE solution. The extraction solution was pumped into the sample loop and then introduced into the CCC column; the target compounds were eluted with the lower aqueous phase of the two-phase solvent system. During the CCC separation, the extraction solution was continuously fed in the sample loop by turning the ten-port valve; the extraction solution was then pumped into the CPC column and eluted by the mobile phase of the two-phase solvent system mentioned above. When the first cycle of the UADE/CCC/CPC was completed, the second cycle experiment could be carried out, and so on. Four target compounds (albiflorin, benzoylpaeoniflorin, paeoniflorin, and galloylpaeoniflorin) with purities above 94.96% were successfully extracted and isolated online using the two-phase solvent system comprising ethyl acetate-n-butanol-ethanol-water (1:3.5:2:4.5, v/v/v/v). Compared with conventional extraction methods, the instrumental setup of the present method offers the advantages of automation and systematic extraction and isolation of natural products. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2016-11-01

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

  13. Ultrasound-assisted extraction of phenolic compounds from Cratoxylum formosum ssp. formosum leaves using central composite design and evaluation of its protective ability against H2O2-induced cell death.

    Science.gov (United States)

    Yingngam, Bancha; Monschein, Marlene; Brantner, Adelheid

    2014-09-01

    To optimize the processing parameters for phenolic compounds extracted from Cratoxylum formosum ssp. formosum leaves using an ultrasound-assisted extraction and to evaluate its protective ability against H2O2-induced cell death. The influence of three independent variables including ethanol concentration (%), extraction temperature (°C) and extraction time (min) on the extraction yield of phenolic compounds were optimized using a central composite design-based response surface methodology. The obtained extract was assessed for its antioxidant activity by DPPH(•) and ABTS(•)(+) methods. Cellular protective ability against H2O2-induced cell death was evaluated on HEK293 cells using the MTT assay. The optimal conditions to achieve maximal yields of phenolic compounds were ethanol concentration of 50.33% (v/v), temperature of 65 °C, and extractiontion time of 15 min. The yield of phenolic compounds was (40.00±1.00) mg gallic acid equivalent/g dry powder which matched well with the values predicted from the proposed model. These conditions resulted in a higher efficiency concerning the extraction of phenolics compared to a conventional heat reflux extraction by providing shorter extraction time and reduced energy consumption. 5-O-caffeoylquinic acid identified by high performance liquid chromatography-diode array detector-electron spin ionization-mass spectrometry was the major compound in the obtained extract [(41.66±0.07) mg/g plant extract]. The obtained extract showed a strong ability to scavenge both DPPH(•) and ABTS(•)(+) free radicals and exhibited additionally good ability to protect HEK293 cells death against oxidative stress. These results indicate the suitability of ultrasound-assisted extraction for the extraction of phenolic compounds from Cratoxylum formosum ssp. formosum leaves. This phenolic-enriched extract can be used as valuable antioxidant source for health benefits. Copyright © 2014 Hainan Medical College. Published by Elsevier B.V. All

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

    Science.gov (United States)

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

    2016-01-29

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

  15. 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.

  16. 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.

  17. Effect of ultrasound on olive oil extraction and optimization of ultrasound-assisted extraction of extra virgin olive oil by response surface methodology (RSM)

    International Nuclear Information System (INIS)

    Aydar, A.Y.; Bağdatlıoğlu, N.; Köseoğlu, O.

    2017-01-01

    In this study, the effects of different extraction parameters including ultrasound time, temperature and malaxation time on olive oil quality were investigated. The extraction variables ultrasound initial temperature (20–50 °C), ultrasound time (2–10 min) and malaxation time (30–50 min) were studied to obtain ideal conditions of ultrasonic treatment on the olive paste for obtaining of a greater yield in the extraction of oil, while maintaining a maximum level of commercial quality. To evaluate the level of commercial quality, absorbance in the UV region, peroxide (PV) and free acidity values (AV), the total chlorophyll, carotenoid, phenol contents, total antioxidant activity and sensory analysis of EVOOs extracted from Edremit cultivar were determined. The optimum conditions were found to be 50 °C, 2 min and 43.23 min for ultrasound initial temperature, sonication time and malaxation time, respectively. This optimal condition gave an extraction yield of 8.25 % and the acidity value of 0.24 mg oleic acid/100 g olive oil. The experimental values obtained under optimal conditions were in agreement with the theoretical values [es

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

    Science.gov (United States)

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

    2017-12-15

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

  19. Trace determination of five triazole fungicide residues in traditional Chinese medicine samples by dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction and UHPLC-MS/MS.

    Science.gov (United States)

    Ma, Shuping; Yuan, Xucan; Zhao, Pengfei; Sun, Hong; Ye, Xiu; Liang, Ning; Zhao, Longshan

    2017-08-01

    A novel and reliable method for determination of five triazole fungicide residues (triadimenol, tebuconazole, diniconazole, flutriafol, and hexaconazol) in traditional Chinese medicine samples was developed using dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction before ultra-high performance liquid chromatography with tandem mass spectrometry. The clean up of the extract was conducted using dispersive solid-phase extraction by directly adding sorbents into the extraction solution, followed by shaking and centrifugation. After that, a mixture of 400 μL trichloromethane (extraction solvent) and 0.5 mL of the above supernatant was injected rapidly into water for the dispersive liquid-liquid microextraction procedure. The factors affecting the extraction efficiency were optimized. Under the optimum conditions, the calibration curves showed good linearity in the range of 2.0-400 (tebuconazole, diniconazole, and hexaconazole) and 4.0-800 ng/g (triadimenol and flutriafol) with the regression coefficients higher than 0.9958. The limit of detection and limit of quantification for the present method were 0.5-1.1 and 1.8-4.0 ng/g, respectively. The recoveries of the target analytes ranged from 80.2 to 103.2%. The proposed method has been successfully applied to the analysis of five triazole fungicides in traditional Chinese medicine samples, and satisfactory results were obtained. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. 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.

  1. 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.

  2. Ultrasound assisted extraction of Maxilon Red GRL dye from water samples using cobalt ferrite nanoparticles loaded on activated carbon as sorbent: Optimization and modeling.

    Science.gov (United States)

    Mehrabi, Fatemeh; Vafaei, Azam; Ghaedi, Mehrorang; Ghaedi, Abdol Mohammad; Alipanahpour Dil, Ebrahim; Asfaram, Arash

    2017-09-01

    In this research, a selective, simple and rapid ultrasound assisted dispersive solid-phase micro-microextraction (UA-DSPME) was developed using cobalt ferrite nanoparticles loaded on activated carbon (CoFe 2 O 4 -NPs-AC) as an efficient sorbent for the preconcentration and determination of Maxilon Red GRL (MR-GRL) dye. The properties of sorbent are characterized by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Vibrating sample magnetometers (VSM), Fourier transform infrared spectroscopy (FTIR), Particle size distribution (PSD) and Scanning Electron Microscope (SEM) techniques. The factors affecting on the determination of MR-GRL dye were investigated and optimized by central composite design (CCD) and artificial neural networks based on genetic algorithm (ANN-GA). CCD and ANN-GA were used for optimization. Using ANN-GA, optimum conditions were set at 6.70, 1.2mg, 5.5min and 174μL for pH, sorbent amount, sonication time and volume of eluent, respectively. Under the optimized conditions obtained from ANN-GA, the method exhibited a linear dynamic range of 30-3000ngmL -1 with a detection limit of 5.70ngmL -1 . The preconcentration factor and enrichment factor were 57.47 and 93.54, respectively with relative standard deviations (RSDs) less than 4.0% (N=6). The interference effect of some ions and dyes was also investigated and the results show a good selectivity for this method. Finally, the method was successfully applied to the preconcentration and determination of Maxilon Red GRL in water and wastewater samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. 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.

  4. 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).

  5. Ultrasound-assisted dyeing of cellulose acetate.

    Science.gov (United States)

    Udrescu, C; Ferrero, F; Periolatto, M

    2014-07-01

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

  6. 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.

    Science.gov (United States)

    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.

  7. 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.

  8. 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)

  9. Deep eutectic solvent-based ultrasound-assisted dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the determination of ultraviolet filters in water samples.

    Science.gov (United States)

    Wang, Huazi; Hu, Lu; Liu, Xinya; Yin, Shujun; Lu, Runhua; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang

    2017-09-22

    In the present study, a simple and rapid sample preparation method designated ultrasound-assisted dispersive liquid-liquid microextraction based on a deep eutectic solvent (DES) followed by high-performance liquid chromatography with ultraviolet (UV) detection (HPLC-UVD) was developed for the extraction and determination of UV filters from water samples. The model analytes were 2,4-dihydroxybenzophenone (BP-1), benzophenone (BP) and 2-hydroxy-4-methoxybenzophenone (BP-3). The hydrophobic DES was prepared by mixing trioctylmethylammonium chloride (TAC) and decanoic acid (DecA). Various influencing factors (selection of the extractant, amount of DES, ultrasound duration, salt addition, sample volume, sample pH, centrifuge rate and duration) on UV filter recovery were systematically investigated. Under optimal conditions, the proposed method provided good recoveries in the range of 90.2-103.5% and relative standard deviations (inter-day and intra-day precision, n=5) below 5.9%. The enrichment factors for the analytes ranged from 67 to 76. The limits of detection varied from 0.15 to 0.30ngmL -1 , depending on the analytes. The linearities were between 0.5 and 500ngmL -1 for BP-1 and BP and between 1 and 500ngmL -1 for BP-3, with coefficients of determination greater than 0.99. Finally, the proposed method was applied to the determination of UV filters in swimming pool and river water samples, and acceptable relative recoveries ranging from 82.1 to 106.5% were obtained. Copyright © 2017. Published by Elsevier B.V.

  10. Determination of fluorine in herbs and water samples by molecular absorption spectrometry after preconcentration on nano-TiO2 using ultrasound-assisted dispersive micro solid phase extraction.

    Science.gov (United States)

    Krawczyk-Coda, Magdalena; Stanisz, Ewa

    2017-11-01

    This work presents ultrasound-assisted dispersive micro solid phase extraction (USA DMSPE) for preconcentration of fluorine (F) in water and herb samples. TiO 2 nanoparticles (NPs) were used as an adsorbent. The determination with slurry sampling was performed via molecular absorption of calcium monofluoride (CaF) at 606.440 nm using a high-resolution continuum source electrothermal absorption spectrometry (HR-CS ET MAS). Several factors influencing the efficiency of the preconcentration technique, such as the amount of TiO 2 , pH of sample solution, ultrasonication and centrifugation time and TiO 2 slurry solution preparation before injection to HR-CS ET MAS, were investigated in detail. The conditions of detection step (wavelength, calcium amount, pyrolysis and molecule-forming temperatures) were also studied. After extraction, adsorbent with the analyte was mixed with 200 μL of H 2 O to prepare a slurry solution. The concentration limit of detection was 0.13 ng mL -1 . The achieved preconcentration factor was 7. The relative standard deviations (RSDs, %) for F in real samples were 3-15%. The accuracy of this method was evaluated by analyses of certified reference materials after spiking: INCT-MPH-2 (Mixed Polish Herbs), INCT-SBF-4 (Soya Bean Flour), ERM-CAO11b (Hard Drinking Water) and TMDA-54.5 (Lake Ontario Water). The measured F contents in reference materials were in satisfactory agreement with the added amounts, and the recoveries were found to be 97-109%. Under the developed extraction conditions, the proposed method has been successfully applied for the determination of F in real water samples (lake, sea, tap water) and herbs.

  11. Determination of organophosphate flame retardants in soil and fish using ultrasound-assisted extraction, solid-phase clean-up, and liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Lorenzo, María; Campo, Julián; Picó, Yolanda

    2018-03-22

    A solid-liquid extraction method in combination with high-performance liquid chromatography and tandem mass spectrometry was developed and optimized for extraction and analysis of organophosphorus flame retardants in soil and fish. Methanol was chosen as the optimum extraction solvent, not only in terms of extraction efficiency, but also for its broader analyte coverage. The subsequent clean-up by solid-phase extraction is required to eliminate matrix coextractives and reduce matrix effects. Recoveries of the optimized method were 50-121% for soil and 47-123% for biota, both with high precision (RSDs solid-phase extraction cartridge clogging that increase variability and analysis time. The method was successfully applied for the determination of organophosphorus flame retardants in soil and fish from L'Albufera Natural Park (Valencia, Spain). Target compounds were detected in all soil and fish samples with values varying from 13.8 to 89.7 ng/g dry weight and from 3.3 to 53.0 ng/g wet weight, respectively. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Ultrasound-Assisted Oxidative Desulfurization of Diesel

    Directory of Open Access Journals (Sweden)

    Niran K. Ibrahim

    2016-11-01

    Full Text Available 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 compounds into their corresponding highly polar oxides, which can be eliminated easily by extraction with a certain highly polar solvent. The oxidizing system utilized was H2O2 as an oxidant, CH3COOH as a promoter, with FeSO4 as a catalyst; whereas acetonitrile was used as extractant. The major influential parameters related to UAODS process have been investigated, namely: ratio of oxidant/fuel, ratio of the promoter/oxidant, dose of catalyst, reaction temperature, and intensity of ultrasonic waves. Kinetics of the reaction has been also studied; it was observed that the UAODS of diesel fuels fitted pseudo-first-order kinetics under the best experimental conditions, whereas values of the apparent rate constant and activation energy were 0.373 min-1 and 24 KJ/mol, respectively. The oxidation treatment, in combination with ultrasonic irradiation, revealed a synergistic effect for diesel desulfurization. The experimental results showed that sulfur removal efficiency could amount to 98% at mild operating conditions (70 ○C and 1 bar. This indicates that the process is efficient and promising for the production of ultra-low-sulfur diesel fuels.

  13. Ultrasound-assisted extraction, characterization, and antioxidant activity in vitro and in vivo of polysaccharides from Chestnut rose (Rosa roxburghii tratt) fruit.

    Science.gov (United States)

    Chen, Guangjing; Kan, Jianquan

    2018-03-01

    In this study, the response surface methodology was utilized to determine optimum conditions for extracting the polysaccharides from Rosa roxburghii Tratt fruit (RRTPs) using ultrasonic-assisted extraction, and the characterization and antioxidant activities of the RRTPs were discussed. RRTPs yield was 6.59 ± 1.34%, which was well consistent with the predicted value of 6.716%, under the following optimum conditions: ratio of water to raw material 40.18 mL/g, extraction temperature 78.8 °C, ultrasonic power 148 W, and extraction time 32.8 min. The monosaccharide composition analysis indicated that RRTPs were composed of mannose (Man), rhamnose (Rha), glucuronic acid (GlcA), galacturonic acid (GalA), glucose (Glc), galactose (Gal), arabinose (Ara) and xylose (Xyl). The molecular weight distribution analysis showed that RRTPs had four main components with molecular weights of 332.56, 183.96, 11.92 and 5.95 kDa, respectively. In vitro antioxidant studies revealed RRTPs exhibited significant antioxidant potential on hydroxyl, superoxide and DPPH radicals. In addition, antioxidant assays in vivo demonstrated that RRTPs can significantly increase the superoxide dismutase (SOD), glutathione peroxidase (GSH-Px) and catalase (CAT) activities, and total antioxidant capacity (TAOC) to some extent, as well as decrease the level of malondialdehyde (MDA) in both serum and liver of d-Gal aging-induced mice. These data suggested that RRTPs could be a potential candidate of natural antioxidants for applications in functional food, pharmaceuticals or cosmetic industries. In summary, this work provided an effective method for the exploitation and utilization of value-added R. roxburghii Tratt fruit which would be useful to fully utilize this resource.

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

    Science.gov (United States)

    Altunay, Nail; Elik, Adil; Gürkan, Ramazan

    2018-02-01

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

  15. 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.

  16. Combined alkaline hydrolysis and ultrasound-assisted extraction for the release of nonextractable phenolics from cauliflower (Brassica oleracea var. botrytis) waste.

    Science.gov (United States)

    Gonzales, Gerard Bryan; Smagghe, Guy; Raes, Katleen; Van Camp, John

    2014-04-16

    Cauliflower waste contains high amounts phenolic compounds, but conventional solvent extraction misses high amounts of nonextractable phenolics (NEP), which may contribute more to the valorization of these waste streams. In this study, the NEP content and composition of cauliflower waste were investigated. The ability of alkaline hydrolysis, sonication, and their combination to release NEP was assessed. Alkaline hydrolysis with sonication was found to extract the highest NEP content (7.3 ± 0.17 mg gallic acid equivalents (GAE)/g dry waste), which was higher than the extractable fraction. The highest yield was obtained after treatment of 2 M NaOH at 60 °C for 30 min of sonication. Quantification and identification were done using U(H)PLC-DAD and U(H)PLC-ESI-MS(E). Kaempferol and quercetin glucosides along with several phenolic acids were found. The results of the study show that there are higher amounts of valuable health-promoting compounds from cauliflower waste than what is currently described in the literature.

  17. Microbial production, ultrasound-assisted extraction and characterization of biopolymer polyhydroxybutyrate (PHB) from terrestrial (P. hysterophorus) and aquatic (E. crassipes) invasive weeds.

    Science.gov (United States)

    Pradhan, Sushobhan; Borah, Arup Jyoti; Poddar, Maneesh Kumar; Dikshit, Pritam Kumar; Rohidas, Lilendar; Moholkar, Vijayanand S

    2017-10-01

    This study reports synthesis of biodegradable poly(3-hydroxybutyrate) (PHB) polymer from two invasive weeds, viz. P. hysterophorus and E. crassipes. The pentose and hexose-rich hydrolyzates obtained from acid pretreatment and enzymatic hydrolysis of two biomasses were separately fermented using Ralstonia eutropha MTCC 8320 sp. PHB was extracted using sonication and was characterized using FTIR, 1 H and 13 C NMR and XRD. PHB content of dry cell mass was 8.1-21.6% w/w, and the PHB yield was 6.85×10 -3 -36.41×10 -3 % w/w raw biomass. Thermal properties of PHB were determined by TGA, DTG and DSC analysis. PHB obtained from pentose-hydrolyzate had glass transition temperatures of 6°-9°C, while PHB from hexose-rich hydrolyzate had maximum thermal degradation temperatures of 370°-389°C. These thermal properties were comparable to the properties of commercial PHB. Probable causes leading to differences in thermal properties of pentose and hexose-derived PHB are: extent of crystallinity and presence of impurity in the polymer matrix. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. 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...

  19. Ultrasound-assisted oxidative desulfurization of bitumen

    Science.gov (United States)

    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.

  20. 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.

  1. Optimisation of ultrasound-assisted reverse micelles dispersive liquid-liquid micro-extraction by Box-Behnken design for determination of acetoin in butter followed by high performance liquid chromatography.

    Science.gov (United States)

    Roosta, Mostafa; Ghaedi, Mehrorang; Daneshfar, Ali

    2014-10-15

    A novel approach, ultrasound-assisted reverse micelles dispersive liquid-liquid microextraction (USA-RM-DLLME) followed by high performance liquid chromatography (HPLC) was developed for selective determination of acetoin in butter. The melted butter sample was diluted and homogenised by n-hexane and Triton X-100, respectively. Subsequently, 400μL of distilled water was added and the microextraction was accelerated by 4min sonication. After 8.5min of centrifugation, sedimented phase (surfactant-rich phase) was withdrawn by microsyringe and injected into the HPLC system for analysis. The influence of effective variables was optimised using Box-Behnken design (BBD) combined with desirability function (DF). Under optimised experimental conditions, the calibration graph was linear over the range of 0.6-200mgL(-1). The detection limit of method was 0.2mgL(-1) and coefficient of determination was 0.9992. The relative standard deviations (RSDs) were less than 5% (n=5) while the recoveries were in the range of 93.9-107.8%. Copyright © 2014. Published by Elsevier Ltd.

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

    African Journals Online (AJOL)

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

  3. 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.

  4. 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.

  5. Ultrasound assisted dispersive micro solid-phase extraction of four tyrosine kinase inhibitors from serum and cerebrospinal fluid by using magnetic nanoparticles coated with nickel-doped silica as an adsorbent

    International Nuclear Information System (INIS)

    Ghazaghi, Mehri; Mousavi, Hassan Zavvar; Shirkhanloo, Hamid; Rashidi, Alimorad

    2016-01-01

    Nanoparticles (NPs) consisting of a magnetic Fe 3 O 4 core and a nickel(II)-doped silica shell were prepared and are shown to be viable materials for selective magnetic extraction of trace quantities of the tyrosine kinase inhibitors (TKIs) imatinib, nilotinib, erlotinib and sunitinib. The NPs were characterized by scanning electron microscopy, transmission electron microscopy, DLS and XRD analysis, and the results revealed a uniform in size (with a typical diameter of 40 nm) and a core-shell structure. The magnetic nanoadsorbent displays good affinity of the TKIs, probably because of the affinity between the Ni(II) ions of the NPs with the nitrogen atoms in the TKIs. The magnetism of the NPs enables them to be quickly separated from serum and cerebrospinal fluid samples. Imidazole, with its higher affinity for Ni(II) than that of the TKIs, was used for desorption of the TKIs from the NPs prior to their quantification by HPLC with UV detection. The detection limits are as low as 200, 480, 130, and 250 ng·L -1 for imatinib, sunitinib, erlotinib, and nilotinib, respectively. The intra-day precisions (RSDs) were lower than 4.0 %. The method displays a wide linear range. It was applied to the determination of TKIs in (spiked) human serum and cerebrospinal fluid and gave recoveries in the range from 94.6 to 98.6 %. (author)

  6. Microbial Inactivation by Ultrasound Assisted Supercritical Fluids

    Science.gov (United States)

    Benedito, Jose; Ortuño, Carmen; Castillo-Zamudio, Rosa Isela; Mulet, Antonio

    A method combining supercritical carbon dioxide (SC-CO2) and high power ultrasound (HPU) has been developed and tested for microbial/enzyme inactivation purposes, at different process conditions for both liquid and solid matrices. In culture media, using only SC-CO2, the inactivation rate of E. coli and S. cerevisiae increased with pressure and temperature; and the total inactivation (7-8 log-cycles) was attained after 25 and 140 min of SC-CO2 (350 bar, 36 °C) treatment, respectively. Using SC-CO2+HPU, the time for the total inactivation of both microorganisms was reduced to only 1-2 min, at any condition selected. The SC-CO2+HPU inactivation of both microorganisms was slower in juices (avg. 4.9 min) than in culture media (avg. 1.5 min). In solid samples (chicken, turkey ham and dry-cured pork cured ham) treated with SC-CO2 and SC-CO2+HPU, the inactivation rate of E. coli increased with temperature. The application of HPU to the SC-CO2 treatments accelerated the inactivation rate of E. coli and that effect was more pronounced in treatments with isotonic solution surrounding the solid food samples. The application of HPU enhanced the SC-CO2 inactivation mechanisms of microorganisms, generating a vigorous agitation that facilitated the CO2 solubilization and the mass transfer process. The cavitation generated by HPU could damage the cell walls accelerating the extraction of vital constituents and the microbial death. Thus, using the combined technique, reasonable industrial processing times and mild process conditions could be used which could result into a cost reduction and lead to the minimization in the food nutritional and organoleptic changes.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2001-08-01

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

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

    Directory of Open Access Journals (Sweden)

    Namasivayam Manickam

    2014-03-01

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

  10. 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.

  11. 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.

  12. Ultrasound assisted enzymatic hydrolysis for isolating titanium dioxide nanoparticles from bivalve mollusk before sp-ICP-MS.

    Science.gov (United States)

    Taboada-López, María Vanesa; Iglesias-López, Sara; Herbello-Hermelo, Paloma; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

    2018-08-14

    Applicability of single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS) using dwell times equal to or shorter than 100 μs has been tested for assessing titanium dioxide nanoparticles (TiO 2 NPs) in bivalve mollusks. TiO 2 NPs isolation from fresh mollusk tissues was achieved by ultrasound assisted enzymatic hydrolysis procedure using a pancreatin/lipase mixture. Optimum extraction conditions imply ultrasonication (60% amplitude) for 10 min, and 7.5 mL of a solution containing 3.0 g L -1 of pancreatin and lipase (pH 7.4). The developed method was found to be repeatable (repeatability of 17% for the over-all procedure, TiO 2 NPs concentration of 5.33 × 10 7  ± 8.89 × 10 6 , n = 11), showing a limit of detection of 5.28 × 10 6 NPs g -1 , and a limit of detection in size of 24.4-30.4 nm, based on the 3σ criteria, and on the 3σ/5 σ criteria, respectively. The analytical recovery within the 90-99% range (use of TiO 2 NPs standards of 50 nm at 7 and 14 μg L -1 as Ti). Several bivalve mollusks (clams, cockles, mussels, razor clams, oysters and variegated scallops) were analyzed for total titanium (ICP-MS after microwave assisted acid digestion), and for TiO 2 NPs by the proposed method. TiO 2 NPs concentrations were within the 2.36 × 10 7 -1.25 × 10 8 NPs g -1 range, and the most frequent sizes were from 50 to 70 nm. Copyright © 2018 Elsevier B.V. All rights reserved.

  13. 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.

    Science.gov (United States)

    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.

  14. 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.

  15. 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)

  16. 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.

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

    Science.gov (United States)

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

    2014-10-01

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

  18. Approaches for on-line coupling of extraction and chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Hyoetylaeinen, Tuulia; Riekkola, Marja-Liisa [Laboratory of Analytical Chemistry, Department of Chemistry, University of Helsinki, P.O. Box 55, 00014, Helsinki (Finland)

    2004-04-01

    This review provides an overview of the approaches available in order to perform on-line coupling of various extraction techniques with liquid and gas chromatography, for the analysis of semivolatile and nonvolatile analytes in liquid and solid samples. The main focus is on the instrumental set-up of these techniques. Selected real applications are described by way of illustration. The extraction methods suitable for on-line coupling covered in this review are: liquid-liquid extraction, solid-phase extraction, membrane-based techniques, pressurised liquid extraction, supercritical fluid extraction, and microwave- and sonication-assisted extractions. The following systems are not covered in this review: on-line coupled solid-phase extraction-liquid chromatography, purge-and-trap-GC, and membrane extraction with a sorbent interface-GC. (orig.)

  19. 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.

  20. 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.

  1. Wave energy extraction by coupled resonant absorbers.

    Science.gov (United States)

    Evans, D V; Porter, R

    2012-01-28

    In this article, a range of problems and theories will be introduced that will build towards a new wave energy converter (WEC) concept, with the acronym 'ROTA' standing for resonant over-topping absorber. First, classical results for wave power absorption for WECs constrained to operate in a single degree of freedom will be reviewed and the role of resonance in their operation highlighted. Emphasis will then be placed on how the introduction of further resonances can improve power take-off characteristics by extending the range of frequencies over which the efficiency is close to a theoretical maximum. Methods for doing this in different types of WECs will be demonstrated. Coupled resonant absorbers achieve this by connecting a WEC device equipped with its own resonance (determined from a hydrodynamic analysis) to a new system having separate mass/spring/damper characteristics. It is shown that a coupled resonant effect can be realized by inserting a water tank into a WEC, and this idea forms the basis of the ROTA device. In essence, the idea is to exploit the coupling between the natural sloshing frequencies of the water in the internal tank and the natural resonance of a submerged buoyant circular cylinder device that is tethered to the sea floor, allowing a rotary motion about its axis of attachment.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. Ultrasound Assisted Esterification of Rubber Seed Oil for Biodiesel Production

    Directory of Open Access Journals (Sweden)

    W Widayat

    2012-04-01

    Full Text Available Production of biodiesel is currently shifting from the first to the second generation inwhich the raw materials are mostly from non-edible type oils and fats. Biodiesel production iscommonly conducted under batch operation using mechanical agitation to accelerate masstransfers. The main drawback of oil esterification is the high content of free fatty acids (FFA whichmay reduce the yield of biodiesel and prolong the production time (2-5 hours. Ultrasonificationhas been used in many applications such as component extraction due to its ability to producecavitation under certain frequency. This research is aimed to facilitate ultrasound system forimproving biodiesel production process particularly rubber seed oil. An ultrasound unit was usedunder constant temperature (40oC and frequency of 40 Hz. The result showed that ultrasound canreduces the processing time and increases the biodiesel yield significantly. A model to describecorrelation of yield and its independent variables is yield (Y = 43,4894 – 0,6926 X1 + 1,1807 X2 –7,1042 X3 + 2,6451 X1X2 – 1,6557 X1X3 + 5,7586 X2X3 - 10,5145 X1X2X3, where X1 is mesh sizes, X2ratio oil: methanol and X3 type of catalyst.

  8. Ultrasound Assisted Esterification of Rubber Seed Oil for Biodiesel Production

    Directory of Open Access Journals (Sweden)

    Berkah Fajar Tamtomo Kiono

    2012-02-01

    Full Text Available roduction of biodiesel is currently shifting from the first to the second generation in which the raw materials are mostly from non-edible type oils and fats. Biodiesel production is commonly conducted under batch operation using mechanical agitation to accelerate mass transfers. The main drawback of oil esterification is the high content of free fatty acids (FFA which may reduce the yield of biodiesel and prolong the production time (2-5 hours. Ultrasonification has been used in many applications such as component extraction due to its ability to produce cavitation under certain frequency. This research is aimed to facilitate ultrasound system for improving biodiesel production process particularly rubber seed oil. An ultrasound unit was used under constant temperature (40oC and frequency of 40 Hz. The result showed that ultrasound can reduces the processing time and increases the biodiesel yield significantly. A model to describe correlation of yield and its independent variables is yield (Y = 43,4894 – 0,6926 X1 + 1,1807 X2 – 7,1042 X3 + 2,6451 X1X2 – 1,6557 X1X3 + 5,7586 X2X3 - 10,5145 X1X2X3, where X1 is mesh sizes, X2 ratio oil: methanol and X3 type of catalyst.

  9. Glossary of terms used in extraction (IUPAC Provisional Recommendations 2016)

    DEFF Research Database (Denmark)

    Poole, Colin; Mester, Zoltan; Miro, Manuel

    2016-01-01

    in analytical extraction are presented. Exhaustive, microextraction, elevated temperature, microwave- and ultrasound-assisted, parallel batch, flow through systems, and membrane extraction approaches are discussed. An associated tutorial titled “Extraction” provides a detailed introduction to the topic....

  10. 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.

  11. Determination of As, Cr, Mo, Sb, Se and V in agricultural soil samples by inductively coupled plasma optical emission spectrometry after simple and rapid solvent extraction using choline chloride-oxalic acid deep eutectic solvent.

    Science.gov (United States)

    Matong, Joseph M; Nyaba, Luthando; Nomngongo, Philiswa N

    2017-01-01

    A rapid, simple and green ultrasound-assisted extraction method using deep eutectic solvents (DES) for extraction of As, Cr, Mo, Sb, Se and V in soil samples, has been developed. Choline chloride-oxalic acid based DES was used as a solvent. The target analytes were subsequently quantified using inductively coupled plasma optical emission spectrometer (ICP OES). The parameters that affect the extraction of the target analytes was optimized using standard reference material of San Joaquin soil (SRM 2709a). In the optimization step, a two-level full factorial experimental design was used. The factors under investigation include extraction time, sample mass and acid concentration. Under optimized conditions, limits of detection (LOD) and limits of quantification (LOQ) ranged from 0.009 to 0.1 and 0.03-0.3µgg -1 , respectively. The repeatability (n=20) estimated in terms of relative standard deviation (%RSD) ranged from 0.9% to 3.7%. The accuracy of the proposed method was carried out using SRM 2709a. The obtained and certified/ indicative values were statistically in good agreement at 95% confidence level. The proposed method applied for quantification of As, Cr, Mo, Sb, Se and V in real soil samples. For comparison, the analytes of interest were also determined using a conventional acid digestion method. According to the paired t-test, the analytical results were not significant differences at 95% confidence level. The method was found to be accurate, precise and environmentally friendly. Copyright © 2016 Elsevier Inc. All rights reserved.

  12. Determination of 21 antibiotics in sea cucumber using accelerated solvent extraction with in-cell clean-up coupled to ultra-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Zhu, Minghua; Zhao, Hongxia; Xia, Deming; Du, Juan; Xie, Huaijun; Chen, Jingwen

    2018-08-30

    An accelerated solvent extraction (ASE) with in-cell clean-up method coupled to ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed to determine 21 antibiotics in sea cucumber. The analytes include 10 sulfonamides, 4 fluoroquinolones, 3 amphenicols, 2 beta-lactams, 1 lincosamide and trimethoprim. Optimal parameters of ASE method were obtained at 80 °C, 1 static cycle of 5 min with methanol/acetonitrile (1/1, v/v) using 2 g of C18 as adsorbent. Recoveries at 50.1-129.2% were achieved with RSD under 20%. Method detection limits ranged from 0.03 to 2.9 μg kg -1 . Compared to the reported ultrasound-assisted extraction method, the proposed method offered comparable extraction efficiency for sulfonamides from sea cucumber, but higher for other categories of antibiotics. This validated method was then successfully applied to sea cucumber samples and 9 antibiotics were detected with the highest concentration up to 57.7 μg kg -1 for norfloxacin. Copyright © 2018 Elsevier Ltd. All rights reserved.

  13. 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.

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

    Directory of Open Access Journals (Sweden)

    Ratnawati Ratnawati

    2016-03-01

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

  15. 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.

  16. Optimization of biodiesel production from Chlorella protothecoides oil via ultrasound assisted transesterification

    Directory of Open Access Journals (Sweden)

    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.

  17. 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.

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

    Science.gov (United States)

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

    2017-02-20

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

  19. 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

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

    Directory of Open Access Journals (Sweden)

    Peniel Jean Gildo

    2018-01-01

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

  1. Ultrasound-Assisted Esterification of Valeric Acid to Alkyl Valerates Promoted by Biosilicified Lipases

    Directory of Open Access Journals (Sweden)

    Soledad Cebrián-García

    2018-06-01

    Full Text Available A novel, environmentally friendly, and sustainable ultrasound-assisted methodology in the valorization of valeric acid to alkyl valerate using a biosilicified lipase from Candida antarctica is reported. This one-pot room temperature methodology of enzyme biosilicification leads to biosilicified lipases with improved activity and reaction efficiency as compared to free enzymes. Yields in the ultrasound-promoted esterification of valeric acid was ca. 90% in 2 h with 15% m/v of biosilicified lipase (Bio-lipase; 616 U/g biocatalyst enzymatic activity and a molar ratio 1:2 (valeric acid:ethanol, slightly superior to that observed by the free enzyme (75% conversion, 583U/g biocatalyst enzymatic activity. The reuse of enzymes in these conditions was tested and the results show a relatively good reusability of these biosilicified enzymes under the investigated conditions, particularly preserving fairly stable specific activities (616 vs. 430 U/g biocatalyst after four reuses.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-01-30

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

  3. 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...

  4. 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

  5. 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.

  6. Ultrasound assisted synthesis of Mn3O4 nanoparticles anchored graphene nanosheets for supercapacitor applications

    International Nuclear Information System (INIS)

    Raj, Balasubramaniam Gnana Sundara; Ramprasad, Rajasekharan Nair Radhika; Asiri, Abdullah M.; Wu, Jerry J; Anandan, Sambandam

    2015-01-01

    Highlights: • Room temperature synthesis of Mn 3 O 4 –graphene (MG) composite via ultra sound assisted method. • TEM images shows Mn 3 O 4 nanoparticles are uniformly distributed on the surface of graphene nanosheets. • MG composite exhibited high specific capacitance of 312 F g −1 in 1 M Na 2 SO 4 which was three times greater than pristine Mn 3 O 4 . • 76% of the initial capacitance was retained even after 1000 cycles. • The higher specific capacitance of the MG nanocomposite due to the synergistic effect between the Mn 3 O 4 nanoparticles and graphene nanosheets. - Abstract: Mn 3 O 4 nanoparticles anchored graphene nanosheets (MG) have been successfully synthesized by a simple ultrasound assisted synthesis at room temperature without the use of any templates or surfactants for supercapacitor applications. Upon ultrasound assisted synthesis, the formation of Mn 3 O 4 nanoparticles and the graphene oxide reduction occurs simultaneously. The crystalline structure of thus prepared MG nanocomposite have been characterized by the powder X-ray diffraction (XRD) analysis. Thermo Gravimetric Analysis (TGA) is used to determine the mass content of graphene (17 wt%) in the MG nanocomposite. Transmission electron microscopy (TEM) and Atomic force microscopy (AFM) studies shows that the Mn 3 O 4 nanoparticles (4–8 nm) were uniformly anchored on the surface of graphene nanosheets. The electrochemical properties of the MG nanocomposite were investigated by employing cyclic voltammetry (CV), galvanostatic charge-discharge and electrochemical impedance spectroscopy (EIS). The capacitive properties of MG nanocomposite studied in the presence of 1 M Na 2 SO 4 exhibited high specific capacitance of 312 F g −1 which was approximately three times greater than that of pristine Mn 3 O 4 (113 F g −1 ) at the same current density of 0.5 mA cm −2 in the potential range from -0.1 to +0.9 V. About 76% of the initial capacitance was retained even after 1000 cycles

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

    Directory of Open Access Journals (Sweden)

    Abbas Afkhami

    2017-06-01

    Full Text Available A method based on the ultrasound-assisted solidification of floating drop microextraction technique was developed for the spectrophotometric and spectrofluorimetric determination of curcumin in turmeric powder. In this work a small volume of an organic solvent was floated on the surface of an aqueous solution. After sonication the organic solvent is solidified and separated. The effect of extraction parameters such as type and the volume of organic solvent, temperature, salt addition and exposure time, on the extraction recovery was investigated and optimized. Finally, the method droplet was used for the determination of analyte. Under the optimum extraction conditions, a linear range of 0.006–30 μg mL-1 and a relative standard deviation (RSD of 2.72% for curcumin wasachieved. Limits of detection of 7 and 2 ng mL-1 curcumin was obtained for the spectrophotometric and spectrofluometric methods, respectively. The obtained results show that the application of this method can be successful for the analysis of curcumin in turmeric powder samples.

  8. Effect of ultrasound on olive oil extraction and optimization of ultrasound-assisted extraction of extra virgin olive oil by response surface methodology (RSM); Efecto del ultrasonido en la extracción de aceite de oliva y optimización de la extracción asistida por ultrasonido del aceite de oliva virgen extra mediante metodología de superficie de respuesta (RSM)

    Energy Technology Data Exchange (ETDEWEB)

    Aydar, A.Y.; Bağdatlıoğlu, N.; Köseoğlu, O.

    2017-07-01

    In this study, the effects of different extraction parameters including ultrasound time, temperature and malaxation time on olive oil quality were investigated. The extraction variables ultrasound initial temperature (20–50 °C), ultrasound time (2–10 min) and malaxation time (30–50 min) were studied to obtain ideal conditions of ultrasonic treatment on the olive paste for obtaining of a greater yield in the extraction of oil, while maintaining a maximum level of commercial quality. To evaluate the level of commercial quality, absorbance in the UV region, peroxide (PV) and free acidity values (AV), the total chlorophyll, carotenoid, phenol contents, total antioxidant activity and sensory analysis of EVOOs extracted from Edremit cultivar were determined. The optimum conditions were found to be 50 °C, 2 min and 43.23 min for ultrasound initial temperature, sonication time and malaxation time, respectively. This optimal condition gave an extraction yield of 8.25 % and the acidity value of 0.24 mg oleic acid/100 g olive oil. The experimental values obtained under optimal conditions were in agreement with the theoretical values [Spanish] En este estudio se investigó el efecto de diferentes parámetros de extracción, incluyendo tiempo de ultrasonido, temperatura y tiempo de malaxación en la calidad del aceite de oliva. Se estudiaron las variables de la extracción como temperatura inicial de ultrasonido (20–50 °C), tiempo de ultrasonido (2–10 min) y tiempo de malaxación (30–50 min) para obtener las condiciones ideales del tratamiento ultrasónico en la pasta de oliva para obtener un mayor rendimiento en la extracción de aceite y manteniendo un máximo de calidad comercial. Para determinar el nivel de calidad comercial, se determinaron la absorbancia en la región UV, índice de peróxido (PV) y los valores de acidez libre (AV), contenido total de clorofila, carotenoides, fenoles, actividad antioxidante total y análisis sensorial de aceites de oliva

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

    García-Medina, J.

    2013-01-01

    Purpose: To evaluate the value of duplex ultrasound assistance during thromboaspiration of thrombosed arteriovenous fistulae for haemodialysis. Materials and Methods: We prospectively studied 54 thrombosed native fistulae (23 with total thrombosis and 31 with partial thrombosis), in which we performed manual thromboaspiration guided by ultrasonography associated with fluoroscopy. Results: The fistulae were located in the forearm (n = 39) or in the upper arm (n = 15) of 46 patients. Mean patient age was 65 years, and hypertension was the most common risk factor (74 %). Mean access age was 928 days (range 69–2,290), and most fistulae were on the left side (41 cases, 75.92 %). The success rate was 83 % in the total thrombosis group and 100 % in the partial thrombosis group. Including initial failures, the respective primary patency rates in the total thrombosis group and the partial thrombosis group were, respectively, 83 ± 8 % (n = 20) and 87 ± 6 % (n = 28) at 1 month, 39 ± 10 % (n = 10) and 61 ± 8 % (n = 20) at 6 months, and 17 ± 8 % (n = 5) and 26 ± 8 % (n = 9) at 1 year. The mean decrease of fluoroscopy time with ultrasound was 3 min (range 1–5). The mean decrease of radiation dose was 2.6 Gy cm² (range 0.9–4.3]. Conclusion: Ultrasound is a feasible and useful tool in the management of thrombosed native fistulae, thus decreasing radiation exposure, and has no detrimental effect on success rates

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

    Science.gov (United States)

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

    2017-12-01

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

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

    Science.gov (United States)

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

    2015-11-01

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

  13. Ultrasound-Assisted 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.

  14. Process optimization of ultrasound-assisted alcoholic-alkaline treatment for granular cold water swelling starches.

    Science.gov (United States)

    Zhu, Bo; Liu, Jianli; Gao, Weidong

    2017-09-01

    This paper reports on the process optimization of ultrasonic assisted alcoholic-alkaline treatment to prepare granular cold water swelling (GCWS) starches. In this work, three statistical approaches such as Plackett-Burman, steepest ascent path analysis and Box-Behnken design were successfully combined to investigate the effects of major treatment process variables including starch concentration, ethanol volume fraction, sodium hydroxide dosage, ultrasonic power and treatment time, and drying operation, that is, vacuum degree and drying time on cold-water solubility. Results revealed that ethanol volume fraction, sodium hydroxide dosage, applied power and ultrasonic treatment time were significant factors that affected the cold-water solubility of GCWS starches. The maximum cold-water solubility was obtained when treated at 400W of applied power for 27.38min. Optimum volume fraction of ethanol and sodium hydroxide dosage were 66.85% and 53.76mL, respectively. The theoretical values (93.87%) and the observed values (93.87%) were in reasonably good agreement and the deviation was less than 1%. Verification and repeated trial results indicated that the ultrasound-assisted alcoholic-alkaline treatment could be successfully used for the preparation of granular cold water swelling starches at room temperatures and had excellent improvement on the cold-water solubility of GCWS starches. Copyright © 2016. Published by Elsevier B.V.

  15. Optimisation of ultrasound-assisted osmotic dehydration of sweet potato (Ipomea batatas) using response surface methodology.

    Science.gov (United States)

    Oladejo, Ayobami Olayemi; Ma, Haile

    2016-08-01

    Sweet potato is a highly nutritious tuber crop that is rich in β-carotene. Osmotic dehydration is a pretreatment method for drying of fruit and vegetables. Recently, ultrasound technology has been applied in food processing because of its numerous advantages which include time saving, little damage to the quality of the food. Thus, there is need to investigate and optimise the process parameters [frequency (20-50 kHz), time (10-30 min) and sucrose concentration (20-60% w/v)] for ultrasound-assisted osmotic dehydration of sweet potato using response surface methodology. The optimised values obtained were frequency of 33.93 kHz, time of 30 min and sucrose concentration of 35.69% (w/v) to give predicted values of 21.62, 4.40 and 17.23% for water loss, solid gain and weight reduction, respectively. The water loss and weight reduction increased when the ultrasound frequency increased from 20 to 35 kHz and then decreased as the frequency increased from 35 to 50 kHz. The results from this work show that low ultrasound frequency favours the osmotic dehydration of sweet potato and also reduces the use of raw material (sucrose) needed for the osmotic dehydration of sweet potato. © 2015 Society of Chemical Industry. © 2015 Society of Chemical Industry.

  16. 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.

  17. 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

  18. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Almeida, Jorge S.; Anunciação, Taiana A.; Brandão, Geovani C.; Dantas, Alailson F.; Lemos, Valfredo A.

    2015-01-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO 3 gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box–Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L −1 HNO 3 as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg −1 . Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method. - Highlights: • The determination of cadmium in vegetable oils was developed using UA-SDME. • HR-CS ET-AAS was employed as a detection technique with direct drop sampling. • The procedure allowed for a reduction in the consumption of reagents and samples

  19. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Almeida, Jorge S.; Anunciação, Taiana A.; Brandão, Geovani C.; Dantas, Alailson F.; Lemos, Valfredo A.; Teixeira, Leonardo S. G.

    2015-05-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO3 gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box-Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L- 1 HNO3 as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg- 1. Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method.

  20. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Jorge S.; Anunciação, Taiana A. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Brandão, Geovani C. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); INCT de Energia e Ambiente, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Dantas, Alailson F. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Lemos, Valfredo A. [Laboratório de Química Analítica (LQA), Universidade Estadual do Sudoeste da Bahia, Campus de Jequié, Jequié, Bahia 45506-191 (Brazil); and others

    2015-05-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO{sub 3} gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box–Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L{sup −1} HNO{sub 3} as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg{sup −1}. Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method. - Highlights: • The determination of cadmium in vegetable oils was developed using UA-SDME. • HR-CS ET-AAS was employed as a detection technique with direct drop sampling. • The procedure allowed for a reduction in the consumption of reagents and

  1. 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.

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

    Science.gov (United States)

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

    2016-06-01

    An efficient analytical method called ionic-liquid-based ultrasound-assisted in situ solvent formation microextraction followed by high-performance liquid chromatography was developed for the determination of atenolol in human plasma. A hydrophobic ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate) was formed by the addition of a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate) to a sample solution containing an ion-pairing agent during microextraction. The analyte was extracted into the ionic liquid phase while the microextraction solvent was dispersed throughout the sample by utilizing ultrasound. The sample was then centrifuged, and the extracting phase retracted into the microsyringe and injected to liquid chromatography. After optimization, the calibration curve showed linearity in the range of 2-750 ng/mL with the regression coefficient corresponding to 0.998. The limits of detection (S/N = 3) and quantification (S/N = 10) were 0.5 and 2 ng/mL, respectively. A reasonable relative recovery range of 90-96.7% and satisfactory intra-assay (4.8-5.1%, n = 6) and interassay (5.0-5.6%, n = 9) precision along with a substantial sample clean-up demonstrated good performance of the procedure. It was applied for the determination of atenolol in human plasma after oral administration and some pharmacokinetic data were obtained. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Strong coupling constant extraction from high-multiplicity Z +jets observables

    Science.gov (United States)

    Johnson, Mark; Maître, Daniel

    2018-03-01

    We present a strong coupling constant extraction at next-to-leading order QCD accuracy using ATLAS Z +2 ,3,4 jets data. This is the first extraction using processes with a dependency on high powers of the coupling constant. We obtain values of the strong coupling constant at the Z mass compatible with the world average and with uncertainties commensurate with other next-to-leading order extractions at hadron colliders. Our most conservative result for the strong coupling constant is αS(MZ)=0.117 8-0.0043+0.0051 .

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    Science.gov (United States)

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

    2017-08-01

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

  6. 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.

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

    Science.gov (United States)

    Tuzen, Mustafa; Pekiner, Ozlem Zeynep

    2015-12-01

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

  8. 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.

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

    DEFF Research Database (Denmark)

    Genina, Natalja; Räikkönen, Heikki; Heinämäki, Jyrki

    2010-01-01

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

  10. 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.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-02-03

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

  13. FI/SI on-line solvent extraction/back extraction preconcentration coupled to direct injection nebulization inductively coupled plasma mass spectrometry for determination of copper and lead

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

    An automated sequential injection on-line preconcentration procedure for determination of trace levels of copper and lead via solvent extraction/back extraction coupled to ICP-MS is described. In citrate buffer of pH 3, neutral complexes between the analytes and the chelating reagent, ammonium...... loop, the content of which is subsequently introduced into the ICP-MS, via a direct injection high efficiency nebulizer (DIHEN), for quantification. Enrichment factors of 29.6 (Cu) and 23.3 (Pb), detection limits of 17 ng/l (Cu) and 11 ng/l (Pb), along with a sampling frequency of 13 s/h were obtained...

  14. 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.

  15. A comparative study of Averrhoabilimbi extraction method

    Science.gov (United States)

    Zulhaimi, H. I.; Rosli, I. R.; Kasim, K. F.; Akmal, H. Muhammad; Nuradibah, M. A.; Sam, S. T.

    2017-09-01

    In recent year, bioactive compound in plant has become a limelight in the food and pharmaceutical market, leading to research interest to implement effective technologies for extracting bioactive substance. Therefore, this study is focusing on extraction of Averrhoabilimbi by different extraction technique namely, maceration and ultrasound-assisted extraction. Fewplant partsof Averrhoabilimbiweretaken as extraction samples which are fruits, leaves and twig. Different solvents such as methanol, ethanol and distilled water were utilized in the process. Fruit extractsresult in highest extraction yield compared to other plant parts. Ethanol and distilled water have significant role compared to methanol in all parts and both extraction technique. The result also shows that ultrasound-assisted extraction gave comparable result with maceration. Besides, the shorter period on extraction process gives useful in term of implementation to industries.

  16. A convenient ultrasound-assisted saponification for the simultaneous determination of vitamin E isomers in vegetable oil by HPLC with fluorescence detection.

    Science.gov (United States)

    Yang, Yi; Lu, Dan; Yin, Shuo; Yang, Danni; Chen, Yaling; Li, Yongxin; Sun, Chengjun

    2018-04-01

    An efficient ultrasound-assisted saponification was developed for simultaneous determination of vitamin E isomers in vegetable oil by high-performance liquid chromatography with fluorescence detection. The samples were saponified ultrasonically with potassium hydroxide solution for only 7 min, then the analytes were extracted with ether. Vitamin E isomers were separated on a C 18 column at 25°C with a mobile phase of methanol/acetonitrile (81:19, v/v) at a flow rate of 0.8 mL/min. Fluorescence detection was operated at 290 nm of excitation wavelength and 327 nm of emission wavelength. Under the optimized conditions, good linearities over the range of 0.001-8.00 μg/mL (r > 0.999) were obtained. Mean recoveries of the method were 88.0-106%, with intra- and interday RSDs less than 11.8 and 12.8%, respectively. The detection limits and quantification limits of the method were 0.30-1.8 and 1.0-6.1 μg/kg, respectively. The recoveries of this method were much higher than that of the quick, easy, cheap, effective, rugged, and safe method and direct dilution method, but were similar to those of hot saponification. This proposed method provides reliable, simple, and rapid quantification of vitamin E isomers in vegetable oils. Five kinds of vegetable oils were analyzed, the quantification results were within the ranges reported by other authors. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Comparison of extraction methods for quantifying vitamin E from animal tissues.

    Science.gov (United States)

    Xu, Zhimin

    2008-12-01

    Four extraction methods: (1) solvent (SOL), (2) ultrasound assisted solvent (UA), (3) saponification and solvent (SP), and (4) saponification and ultrasound assisted solvent (SP-UA), were used in sample preparation for quantifying vitamin E (tocopherols) in chicken liver and plasma samples. The extraction yields of SOL, UA, SP, and SP-UA methods obtained by adding delta-tocopherol as internal reference were 95%, 104%, 65%, and 62% for liver and 98%, 103%, 97%, and 94% for plasma, respectively. The methods with saponification significantly affected the stabilities of tocopherols in liver samples. The measured values of alpha- and gamma-tocopherols using the solvent only extraction (SOL) method were much lower than that using any of the other extraction methods. This indicated that less of the tocopherols in those samples were in a form that could be extracted directly by solvent. The measured value of alpha-tocopherol in the liver sample using the ultrasound assisted solvent (UA) method was 1.5-2.5 times of that obtained from the saponification and solvent (SP) method. The differences in measured values of tocopherols in the plasma samples by using the two methods were not significant. However, the measured value of the saponification and ultrasound assisted solvent (SP-UA) method was lower than either the saponification and solvent (SP) or the ultrasound assisted solvent (UA) method. Also, the reproducibility of the ultrasound assisted solvent (UA) method was greater than any of the saponification methods. Compared with the traditional saponification method, the ultrasound assisted solvent method could effectively extract tocopherols from sample matrix without any chemical degradation reactions, especially for complex animal tissue such as liver.

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

    Science.gov (United States)

    Barrett, Elizabeth J; Rodgerson, Dwayne H

    2014-08-01

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

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

    Science.gov (United States)

    Cherepanov, Pavel V; Andreeva, Daria V

    2017-03-01

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

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

    Science.gov (United States)

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

    2017-09-01

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

  1. Study of supercritical CO2 extraction and nanofiltration membrane separation coupling

    International Nuclear Information System (INIS)

    Sarrade, S.

    1994-12-01

    The aim of this thesis is to study the coupling of two extraction techniques, nanofiltering and supercritical fluids, designing and building an experimental device that enables both supercritical CO 2 extraction and nanofiltering membrane separation. The purpose is to reach high splitting up levels on small molecule mixtures. The document is divided in four parts : a bibliographic study on these two techniques; a description of the membranes and the products, as well as the experimental device; the characterization and modelization of transfer mechanism in aqueous solutions; a presentation of the results obtained by coupling the two techniques. (TEC). 45 tabs., 70 figs., 98 refs

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

    International Nuclear Information System (INIS)

    Peng, Yonggang; Ji, Junling; Chen, Dajun

    2015-01-01

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

  3. 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.

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

    Science.gov (United States)

    Ramadoss, Govindarajan; Muthukumar, Karuppan

    2016-01-01

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

  5. Surface modification of chitin using ultrasound-assisted and supercritical CO{sub 2} technologies for cobalt adsorption

    Energy Technology Data Exchange (ETDEWEB)

    Dotto, Guilherme L., E-mail: guilherme_dotto@yahoo.com.br; Cunha, Jeanine M., E-mail: jeaninecunha@gmail.com; Calgaro, Camila O., E-mail: camila.itepjr@gmail.com; Tanabe, Eduardo H., E-mail: edutanabe@yahoo.com.br; Bertuol, Daniel A., E-mail: dbertuol@gmail.com

    2015-09-15

    Highlights: • Chitin was modified by ultrasound-assisted (UA) and supercritical (SCO{sub 2}) technologies. • Chitin, UA-chitin and SCO{sub 2}-chitin were used as adsorbents for Co(II). • UA and SCO{sub 2} treatments provided increase of 20 and 3 times in chitin surface area. • The Co(II) adsorption capacity increased until 67.8%, using UA-chitin. - Abstract: Ultrasound-assisted (UA) and supercritical CO{sub 2} technologies (SCO{sub 2}) were used to modify the chitin surface and, improve its adsorption characteristics regarding to cobalt. Chitin, before and after the treatments, was characterized by N{sub 2} adsorption isotherms (BET), infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and scanning electron microscopy (SEM). Unmodified and surface modified chitins were used as adsorbents to remove cobalt from aqueous solutions. The adsorption study was performed by equilibrium isotherms and kinetic curves. The chitin particle characteristics, such as, surface area, pore volume and porosity were improved by the UA and SCO{sub 2} treatments. The crystallinity index decreased after the UA and SCO{sub 2} treatments, and also, intense surface modifications were observed. Langmuir and Freundlich models were adequate to represent the adsorption equilibrium. The maximum adsorption capacities were 50.03, 83.94 and 63.08 mg g{sup −1} for unmodified chitin, UA surface modified chitin and SCO{sub 2} surface modified chitin. The adsorption kinetic curves were well represented by the pseudo-second order model. UA and SCO{sub 2} technologies are alternatives to modify the chitin surface and improve its adsorption characteristics.

  6. Development of an interface for directly coupled solid-phase extraction and GC-MS analysis

    NARCIS (Netherlands)

    Öllers, M.J.H.; van Lieshout, H.P.M.; Janssen, J.G.M.; Cramers, C.A.M.G.

    Solid-phase extraction (SPE) is widely used as a sample preparation technique in numerous application areas of chromatography. Large-volume injection is an attractive technique for coupling SPE to gas chromatography (GC) because it provides improved detection limits and circumvents the need for

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

    NARCIS (Netherlands)

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

    1990-01-01

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

  8. Lanthanides determination in red wine using ultrasound assisted extraction, flow injection, aerosol desolvation and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Bentlin, Fabrina R.S. [Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501.970 Porto Alegre, RS (Brazil); Santos, Clarissa M.M. dos; Flores, Erico M.M. [Departamento de Quimica Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Pozebon, Dirce, E-mail: dircepoz@iq.ufrgs.br [Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501.970 Porto Alegre, RS (Brazil)

    2012-01-13

    Highlights: Black-Right-Pointing-Pointer Ultrasound was investigated and applied for red wine samples preparation. Black-Right-Pointing-Pointer Aliquots of 50 {mu}L of sample were nebulized and transported to plasma. Black-Right-Pointing-Pointer FI and pneumatic nebulization/aerosol desolvation were used. Black-Right-Pointing-Pointer LODs of the ICP-MS method for lanthanides determination were at ng L{sup -1} level. Black-Right-Pointing-Pointer Lanthanides concentration allowed red wines classification. - Abstract: This paper deals with the determination of the fourteen naturally occurring elements of the lanthanide series in red wine. Ultrasound (US) was used for sample preparation prior lanthanides determination using ICP-MS. Flow injection (FI) and pneumatic nebulization/aerosol desolvation were used for nebulization of aliquots of 50 {mu}L of sample and its subsequent transportation to plasma. Sample preparation procedures, matrix interference and time of sonication were evaluated. Better results for lanthanides in red wine were obtained by sonication with US probe for 90 s and sample 10-fold diluted. The limits of detection of La, Ce, Nd, Sm, Gd, Pr, Eu, Tb, Dy, Ho, Er, Tm, Lu and Yb were 6.57, 10.8, 9.97, 9.38, 2.71, 1.29, 1.22, 0.52, 2.35, 0.96, 2.30, 0.45, 0.24 and 1.35 ng L{sup -1}, respectively. Red wines of different varieties from three countries of South America were discriminated according to the country of origin by means of multivariate analysis of lanthanides concentration.

  9. Lanthanides determination in red wine using ultrasound assisted extraction, flow injection, aerosol desolvation and ICP-MS

    International Nuclear Information System (INIS)

    Bentlin, Fabrina R.S.; Santos, Clarissa M.M. dos; Flores, Érico M.M.; Pozebon, Dirce

    2012-01-01

    Highlights: ► Ultrasound was investigated and applied for red wine samples preparation. ► Aliquots of 50 μL of sample were nebulized and transported to plasma. ► FI and pneumatic nebulization/aerosol desolvation were used. ► LODs of the ICP-MS method for lanthanides determination were at ng L −1 level. ► Lanthanides concentration allowed red wines classification. - Abstract: This paper deals with the determination of the fourteen naturally occurring elements of the lanthanide series in red wine. Ultrasound (US) was used for sample preparation prior lanthanides determination using ICP-MS. Flow injection (FI) and pneumatic nebulization/aerosol desolvation were used for nebulization of aliquots of 50 μL of sample and its subsequent transportation to plasma. Sample preparation procedures, matrix interference and time of sonication were evaluated. Better results for lanthanides in red wine were obtained by sonication with US probe for 90 s and sample 10-fold diluted. The limits of detection of La, Ce, Nd, Sm, Gd, Pr, Eu, Tb, Dy, Ho, Er, Tm, Lu and Yb were 6.57, 10.8, 9.97, 9.38, 2.71, 1.29, 1.22, 0.52, 2.35, 0.96, 2.30, 0.45, 0.24 and 1.35 ng L −1 , respectively. Red wines of different varieties from three countries of South America were discriminated according to the country of origin by means of multivariate analysis of lanthanides concentration.

  10. Lanthanides determination in red wine using ultrasound assisted extraction, flow injection, aerosol desolvation and ICP-MS.

    Science.gov (United States)

    Bentlin, Fabrina R S; dos Santos, Clarissa M M; Flores, Erico M M; Pozebon, Dirce

    2012-01-13

    This paper deals with the determination of the fourteen naturally occurring elements of the lanthanide series in red wine. Ultrasound (US) was used for sample preparation prior lanthanides determination using ICP-MS. Flow injection (FI) and pneumatic nebulization/aerosol desolvation were used for nebulization of aliquots of 50 μL of sample and its subsequent transportation to plasma. Sample preparation procedures, matrix interference and time of sonication were evaluated. Better results for lanthanides in red wine were obtained by sonication with US probe for 90 s and sample 10-fold diluted. The limits of detection of La, Ce, Nd, Sm, Gd, Pr, Eu, Tb, Dy, Ho, Er, Tm, Lu and Yb were 6.57, 10.8, 9.97, 9.38, 2.71, 1.29, 1.22, 0.52, 2.35, 0.96, 2.30, 0.45, 0.24 and 1.35 ng L(-1), respectively. Red wines of different varieties from three countries of South America were discriminated according to the country of origin by means of multivariate analysis of lanthanides concentration. Copyright © 2011 Elsevier B.V. All rights reserved.

  11. Puffed cereals with added chamomile – quantitative analysis of polyphenols and optimization of their extraction method

    Directory of Open Access Journals (Sweden)

    Tomasz Blicharski

    2017-05-01

    For most of the analyzed compounds, the highest yields were obtained by ultrasound assisted extraction. The highest temperature during the ultrasonification process (60oC increased the efficiency of extraction, without degradation of polyphenols. UAE easily arrives at extraction equilibrium and therefore permits shorter periods of time, reducing the energy input. Furthermore, UAE meets the requirements of ‘Green Chemistry’

  12. 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

  13. 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.

  14. Extraction of surface plasmons in organic light-emitting diodes via high-index coupling.

    Science.gov (United States)

    Scholz, Bert J; Frischeisen, Jörg; Jaeger, Arndt; Setz, Daniel S; Reusch, Thilo C G; Brütting, Wolfgang

    2012-03-12

    The efficiency of organic light-emitting diodes (OLEDs) is still limited by poor light outcoupling. In particular, the excitation of surface plasmon polaritons (SPPs) at metal-organic interfaces represents a major loss channel. By combining optical simulations and experiments on simplified luminescent thin-film structures we elaborate the conditions for the extraction of SPPs via coupling to high-index media. As a proof-of-concept, we demonstrate the possibility to extract light from wave-guided modes and surface plasmons in a top-emitting white OLED by a high-index prism.

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

    Science.gov (United States)

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

    2018-01-01

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

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

    Science.gov (United States)

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

    2015-11-01

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

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

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

    Science.gov (United States)

    Rahimi, Masoud; Shahhosseini, Shahrokh; Movahedirad, Salman

    2017-11-01

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

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

    Science.gov (United States)

    Wang, Chongqing; Wang, Hui; Gu, Guohua

    2018-02-15

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

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

    Science.gov (United States)

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

    2018-02-01

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

  1. 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.

  2. Extraction of Z' coupling data from Z' → jj at the LHC and SSC

    International Nuclear Information System (INIS)

    Rizzo, T.G.

    1993-06-01

    A recent analysis has shown that it may be possible at the SSC to extract information about Z' couplings via the decay Z' → jj. This technique was found to be useful for some extended electroweak models provided the Z' is relatively light. In the present paper, the authors generalize this procedure to the LHC and to Z''s which are more massive than 1 TeV

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

    Directory of Open Access Journals (Sweden)

    Lijian Pei

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

  4. Chemical composition of mate tea leaves (Ilex paraguariensis): a study of extraction methods.

    Science.gov (United States)

    Assis Jacques, Rosângela; dos Santos Freitas, Lisiane; Flores Peres, Valéria; Dariva, Cláudio; de Oliveira, José Vladimir; Bastos Caramão, Elina

    2006-12-01

    The objective of this work was to investigate the extraction of Ilex paraguariensis leaves by means of three extraction techniques: pressurized liquid extraction (PLE, also called accelerated solvent extraction--ASE), maceration, and sonication. Samples of mate tea leaves were collected from an experiment conducted under agronomic control at Indfistria e Comércio de Erva-Mate Barão LTDA, Brazil. Six solvents with increasing polarities (n-hexane, toluene, dichloromethane, ethyl acetate, acetone, and methanol) were used in this investigation. Chemical analysis of the extracts was performed by GC coupled with a mass spectrometer detector. The identification and quantification were accomplished by coinjections of certified standards. The results showed that no significant differences in the qualities of the extracts were noticed regarding the extraction methods. On the other hand, the PLE technique was found to be more effective for the extractions of caffeine, phytol, palmitic, and stearic acid. The use of PLE led to a significant decrease in the total extraction time, amount of solvent consumption, and manipulation of samples compared to maceration and ultrasound-assisted extraction methods.

  5. 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

  6. Sequential low and medium frequency ultrasound assists biodegradation of wheat chaff by white rot fungal enzymes.

    Science.gov (United States)

    Oliver, Christine M; Mawson, Raymond; Melton, Laurence D; Dumsday, Geoff; Welch, Jessica; Sanguansri, Peerasak; Singh, Tanoj K; Augustin, Mary Ann

    2014-10-13

    The consequences of ultrasonic pre-treatment using low (40 kHz) and medium (270 kHz) frequency (40 kHz followed by 270 kHz) on the degradation of wheat chaff (8 g 100ml(-1) acetate buffer, pH 5) were evaluated. In addition, the effects of the ultrasonic pre-treatment on the degradation of the wheat chaff when subsequently exposed to enzyme extracts from two white rot fungi (Phanerochaete chrysosporium and Trametes sp.) were investigated. Pre-treatment by sequential low and medium frequency ultrasound had a disruptive effect on the lignocellulosic matrix. Analysis of the phenolic-derived volatiles after enzymatic hydrolysis showed that biodegradation with the enzyme extract obtained from P. chrysosporium was more pronounced compared to that of the Trametes sp. The efficacy of the ultrasonic pre-treatment was attributed to increased enzyme accessibility of the cellulose fibrils due to sonication-induced disruption of the plant surface structure, as shown by changes in the microstructure. Copyright © 2014 Elsevier Ltd. All rights reserved.

  7. Comparison between dispersive solid-phase and dispersive liquid-liquid microextraction combined with spectrophotometric determination of malachite green in water samples based on ultrasound-assisted and preconcentration under multi-variable experimental design optimization.

    Science.gov (United States)

    Alipanahpour Dil, Ebrahim; Ghaedi, Mehrorang; Asfaram, Arash; Zare, Fahimeh; Mehrabi, Fatemeh; Sadeghfar, Fardin

    2017-11-01

    The ultrasound-assisted dispersive solid-phase microextraction (USA-DSPME) and the ultrasound-assisted dispersive liquid-liquid microextraction (USA-DLLME) developed for as an ultra preconcentration and/or technique for the determination of malachite green (MG) in water samples. Central composite design based on analysis of variance and desirability function guide finding best operational conditions and represent dependency of response to variables viz. volume of extraction, eluent and disperser solvent, pH, adsorbent mass and ultrasonication time has significant influence on methods efficiency. Optimum conditions was set for USA-DSPME as: 1mg CNTs/Zn:ZnO@Ni 2 P-NCs; 4min sonication time and 130μL eluent at pH 6.0. Meanwhile optimum point for USA-DLLME conditions were fixed at pH 6.0; 4min sonication time and 130, 650μL and 10mL of extraction solvent (CHCl 3 ), disperser solvent (ethanol) and sample volume, respectively. Under the above specified best operational conditions, the enrichment factors for the USA-DSPME and USA-DLLME were 88.89 and 147.30, respectively. The methods has linear response in the range of 20.0 to 4000.0ngmL -1 with the correlation coefficients (r) between 0.9980 to 0.9995, while its reasonable detection limits viz. 1.386 to 2.348ngmL -1 and good relative standard deviations varied from 1.1% to 2.8% (n=10) candidate this method for successful monitoring of analyte from various media. The relative recoveries of the MG dye from water samples at spiking level of 500ngmL -1 were in the range between 94.50% and 98.86%. The proposed methods has been successfully applied to the analysis of the MG dye in water samples, and a satisfactory result was obtained. Copyright © 2017. Published by Elsevier B.V.

  8. Speciation analysis of organomercurial compounds in Fish Tissue by capillary gas chromatography coupled to microwave-induced plasma atomic emission detection

    Directory of Open Access Journals (Sweden)

    Dorfe Díaz

    Full Text Available This paper describes a novel approach for analysis of mercury speciation in fish using gas chromatography coupled with microwave-induced plasma optical emission spectrometry (GC-MIP-OES in surfatron resonant cavity. Sample treatment was based on quantitative leaching of mercury species from fish tissue with ultrasound-assisted acid-toluene extraction. The extracted mercury species analyzed with GC-MIP-OES attained detection limits of 5 and 9 pg for methylmercury (MeHg and ethylmercury (EtHg, respectively. A complete chromatogram could be completed in 1.5 min. MeHg values obtained with GC-MIP-OES were matched with organic mercury values obtained with selective reduction cold vapour- atomic absorption spectrometry (CV-AAS.

  9. Ultrasound assisted great saphenous vein ligation and division: an office procedure

    Directory of Open Access Journals (Sweden)

    Stefano Ricci

    2014-10-01

    Full Text Available The aim of this proof of concept study is to describe an ultrasound (US assisted simplified surgical procedure for pre-terminal great saphenous vein (GSV high ligation/division avoiding groin dissection and tributary interruption, in an office setting, in association to varices phlebectomy and saphenous vein foam occlusion treatment. Inclusion criteria: primary GSV reflux due to terminal valve, vein diameter >6 mm. By ultrasonography in standing position, the point GSV passing over the adductor longus muscle (about 3 cm from the junction is identified. This E (easy point, relatively superficial, free from tributaries and other structures, allows an easy grasping and extraction of the GSV vein through a 3 mm stab incision provided an ultrasonography assistance. The vein is divided/ligated about 2 cm distal from the ostium, the distal stump is cannulated and foam is injected on the distal segment from the E-point incision in a retrograde fashion, varices are avulsed by phlebectomy. Twenty procedures in 18 patients (venous clinical severity score: mean 3.15 - GSV diameter: mean 7.34 were performed, all the cases without inconveniences, with a duration not exceeding 10 min in addition to the phlebectomy procedure time. No complications as hemorrhage, infection, nerve lesion, lymphatic leak or thrombosis have been registered. At one month the residual saphenous stump length was in average 2.16 cm with complete closure of GSV in all. Three patients have been controlled at 6 months showing GSV complete closure. The procedure described is a simple office US assisted method for GSV ligationdivision, leaving the 2 last cm of the saphenofemoral junction. It could be associated to most of the procedures in use with limited additional time and resources required.

  10. Speciation analysis of mercury by dispersive solid-phase extraction coupled with capillary electrophoresis.

    Science.gov (United States)

    Li, Jinhua; Liu, Junying; Lu, Wenhui; Gao, Fangfang; Wang, Liyan; Ma, Jiping; Liu, Huitao; Liao, Chunyang; Chen, Lingxin

    2018-04-23

    A pretreatment method of dispersive solid-phase extraction (DSPE) along with back-extraction followed by CE-UV detector was developed for the determination of mercury species in water samples. Sulfhydryl-functionalized SiO 2 microspheres (SiO 2 -SH) were synthesized and used as DSPE adsorbents for selective extraction and enrichment of three organic mercury species namely ethylmercury (EtHg), methylmercury (MeHg), and phenylmercury (PhHg), along with L-cysteine (L-cys) containing hydrochloric acid as back-extraction solvent. Several main extraction parameters were systematically investigated including sample pH, amount of adsorbent, extraction and back-extraction time, volume of eluent, and concentration of hydrochloric acid. Under optimal conditions, good linearity was achieved with correlation coefficients over 0.9990, in the range of 4-200 μg/L for EtHg, and 2-200 μg/L for MeHg and PhHg. The LODs were obtained of 1.07, 0.34, and 0.24 μg/L for EtHg, MeHg, and PhHg, respectively, as well as the LOQs were 3.57, 1.13, and 0.79 μg/L, respectively, with enrichment factors ranging from 109 to 184. Recoveries were attained with tap and lake water samples in a range of 62.3-107.2%, with relative standard deviations of 3.5-10.1%. The results proved that the method of SiO 2 -SH based DSPE coupled with CE-UV was a simple, rapid, cost-effective, and eco-friendly alternative for the determination of mercury species in water samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Super-pixel extraction based on multi-channel pulse coupled neural network

    Science.gov (United States)

    Xu, GuangZhu; Hu, Song; Zhang, Liu; Zhao, JingJing; Fu, YunXia; Lei, BangJun

    2018-04-01

    Super-pixel extraction techniques group pixels to form over-segmented image blocks according to the similarity among pixels. Compared with the traditional pixel-based methods, the image descripting method based on super-pixel has advantages of less calculation, being easy to perceive, and has been widely used in image processing and computer vision applications. Pulse coupled neural network (PCNN) is a biologically inspired model, which stems from the phenomenon of synchronous pulse release in the visual cortex of cats. Each PCNN neuron can correspond to a pixel of an input image, and the dynamic firing pattern of each neuron contains both the pixel feature information and its context spatial structural information. In this paper, a new color super-pixel extraction algorithm based on multi-channel pulse coupled neural network (MPCNN) was proposed. The algorithm adopted the block dividing idea of SLIC algorithm, and the image was divided into blocks with same size first. Then, for each image block, the adjacent pixels of each seed with similar color were classified as a group, named a super-pixel. At last, post-processing was adopted for those pixels or pixel blocks which had not been grouped. Experiments show that the proposed method can adjust the number of superpixel and segmentation precision by setting parameters, and has good potential for super-pixel extraction.

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

    Science.gov (United States)

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

    2017-07-01

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

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

    Directory of Open Access Journals (Sweden)

    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.

  14. The coupling of rapidly synergistic cloud point extraction with thermospray flame furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Wen, X.; Deng, Q.; Guo, J.; Zhao, X.; Zhao, Y.; Ji, S.

    2012-01-01

    Rapidly synergistic cloud point extraction (RS-CPE) was coupled with thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) to result in new CPE patterns and accelerated (1 min) protocols. It is demonstrated, for the case of copper (II) ion, that TS-FF-AAS improves the sampling efficiency and the sensitivity of FAAS determinations. Problems of nebulization associated with previous methods based on the coupling of FAAS and RS-CPE are overcome. TS-FF-AAS also improves sensitivity and gives a limit of detection for copper of 0.20 μg L -1 , which is better by a factor of 32. Compared to direct FAAS, the factor is 114. (author)

  15. Developments in coupled solid-phase extraction-capillary electrophoresis 2013-2015.

    Science.gov (United States)

    Ramautar, Rawi; Somsen, Govert W; de Jong, Gerhardus J

    2016-01-01

    An overview of the design and application of coupled solid-phase extraction-capillary electrophoresis (SPE-CE) systems reported in the literature between July 2013 and June 2015 is provided in this paper. The present article is a continuation of our previous review papers on this topic which covered the time period 2000-2013 (Electrophoresis 2008, 29, 108-128; Electrophoresis 2010, 31, 44-54; Electrophoresis 2012, 33, 243-250; Electrophoresis 2014, 35, 128-137). The use of in-line and on-line SPE-CE approaches is treated and outlined in this review. Recent advancements, such as, for example, the use of aptamers as affinity material for in-line SPE-CE, the use of a bead string design for in-line fritless SPE-CE, and new interfacing techniques for the on-line coupling of SPE to CE, are outlined. Selected examples demonstrate the applicability of the coupled SPE-CE systems for biomedical, pharmaceutical, environmental, and food studies. A complete overview of the recent SPE-CE studies is given in table format, providing information on sample type, SPE sorbent, coupling mode, detection mode, and LOD. Finally, some general conclusions and perspectives are provided. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. A novel technology coupling extraction and foam fractionation for separating the total saponins from Achyranthes bidentata.

    Science.gov (United States)

    Ding, Linlin; Wang, Yanji; Wu, Zhaoliang; Liu, Wei; Li, Rui; Wang, Yanyan

    2016-10-02

    A novel technology coupling extraction and foam fractionation was developed for separating the total saponins from Achyranthes bidentata. In the developed technology, the powder of A. bidentata was loaded in a nylon filter cloth pocket with bore diameter of 180 µm. The pocket was fixed in the bulk liquid phase for continuously releasing saponins. Under the optimal conditions, the concentration and the extraction rate of the total saponins in the foamate by the developed technology were 73.5% and 416.2% higher than those by the traditional technology, respectively. The foamates obtained by the traditional technology and the developed technology were analyzed by ultraperformance liquid chromatography-mass spectrometry to determine their ingredients, and the results appeared that the developed technology exhibited a better performance for separating saponins than the traditional technology. The study is expected to develop a novel technology for cost effectively separating plant-derived materials with surface activity.

  17. Simultaneous Determination of Food-Related Biogenic Amines and Precursor Amino Acids Using in Situ Derivatization Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction by Ultra-High-Performance Liquid Chromatography Tandem Mass Spectrometry.

    Science.gov (United States)

    He, Yongrui; Zhao, Xian-En; Wang, Renjun; Wei, Na; Sun, Jing; Dang, Jun; Chen, Guang; Liu, Zhiqiang; Zhu, Shuyun; You, Jinmao

    2016-11-02

    A simple, rapid, sensitive, selective, and environmentally friendly method, based on in situ derivatization ultrasound-assisted dispersive liquid-liquid microextraction (in situ DUADLLME) coupled with ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) using multiple reaction monitoring (MRM) mode has been developed for the simultaneous determination of food-related biogenic amines and amino acids. A new mass-spectrometry-sensitive derivatization reagent 4'-carbonyl chloride rosamine (CCR) was designed, synthesized, and first reported. Parameters and conditions of in situ DUADLLME and UHPLC-MS/MS were optimized in detail. Under the optimized conditions, the in situ DUADLLME was completed speedily (within 1 min) with high derivatization efficiencies (≥98.5%). With the cleanup and concentration of microextraction step, good analytical performance was obtained for the analytes. The results showed that this method was accurate and practical for quantification of biogenic amines and amino acids in common food samples (red wine, beer, wine, cheese, sausage, and fish).

  18. 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.

  19. 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.

  20. Fabricating and Characterizing the Microfluidic Solid Phase Extraction Module Coupling with Integrated ESI Emitters

    Directory of Open Access Journals (Sweden)

    Hangbin Tang

    2018-05-01

    Full Text Available Microfluidic chips coupling with mass spectrometry (MS will be of great significance to the development of relevant instruments involving chemical and bio-chemical analysis, drug detection, food and environmental applications and so on. In our previous works, we proposed two types of microfluidic electrospray ionization (ESI chip coupling with MS: the two-phase flow focusing (FF ESI microfluidic chip and the corner-integrated ESI emitter, respectively. However the pretreatment module integrated with these ESI emitters is still a challenging problem. In this paper, we concentrated on integrating the solid phase micro-extraction (SPME module with our previous proposed on-chip ESI emitters; the fabrication processes of such SPME module are fully compatible with our previous proposed ESI emitters based on the multi-layer soft lithography. We optimized the structure of the integrated chip and characterized its performance using standard samples. Furthermore, we verified its abilities of salt removal, extraction of multiple analytes and separation through on-chip elution using mimic biological urine spiked with different drugs. The results indicated that our proposed integrated module with ESI emitters is practical and effective for real biological sample pretreatment and MS detection.

  1. Exercise capacity in the Bidirectional Glenn physiology: Coupling cardiac index, ventricular function and oxygen extraction ratio.

    Science.gov (United States)

    Vallecilla, Carolina; Khiabani, Reza H; Trusty, Phillip; Sandoval, Néstor; Fogel, Mark; Briceño, Juan Carlos; Yoganathan, Ajit P

    2015-07-16

    In Bi-directional Glenn (BDG) physiology, the superior systemic circulation and pulmonary circulation are in series. Consequently, only blood from the superior vena cava is oxygenated in the lungs. Oxygenated blood then travels to the ventricle where it is mixed with blood returning from the lower body. Therefore, incremental changes in oxygen extraction ratio (OER) could compromise exercise tolerance. In this study, the effect of exercise on the hemodynamic and ventricular performance of BDG physiology was investigated using clinical patient data as inputs for a lumped parameter model coupled with oxygenation equations. Changes in cardiac index, Qp/Qs, systemic pressure, oxygen extraction ratio and ventricular/vascular coupling ratio were calculated for three different exercise levels. The patient cohort (n=29) was sub-grouped by age and pulmonary vascular resistance (PVR) at rest. It was observed that the changes in exercise tolerance are significant in both comparisons, but most significant when sub-grouped by PVR at rest. Results showed that patients over 2 years old with high PVR are above or close to the upper tolerable limit of OER (0.32) at baseline. Patients with high PVR at rest had very poor exercise tolerance while patients with low PVR at rest could tolerate low exercise conditions. In general, ventricular function of SV patients is too poor to increase CI and fulfill exercise requirements. The presented mathematical model provides a framework to estimate the hemodynamic performance of BDG patients at different exercise levels according to patient specific data. Published by Elsevier Ltd.

  2. The endoscopic ultrasound-assisted Rendez-Vous technique for treatment of recurrent pancreatitis due to pancreas divisum and ansa pancreatica

    Directory of Open Access Journals (Sweden)

    Sergio López-Durán

    Full Text Available Endoscopic treatment of pancreatic ductal malformations causing recurrent acute pancreatitis, such as pancreas divisum or ansa pancreatica, is mainly based on the sphincterotomy of the minor papilla. However, the technical complexity of conventional endoscopic retrograde cholangiopancreatography (ERCP is increased in patients presenting anatomical variants like these and it may be unsuccessful. We report the case of a pancreas divisum combined with ansa pancreatica and describe the cannulation and sphincterotomy of the minor papilla using an ultrasound-assisted Rendez-Vous technique.

  3. Effect of solvent on the extraction of phenolic compounds and antioxidant capacity of hazelnut kernel.

    Science.gov (United States)

    Fanali, Chiara; Tripodo, Giusy; Russo, Marina; Della Posta, Susanna; Pasqualetti, Valentina; De Gara, Laura

    2018-03-22

    Hazelnut kernel phenolic compounds were recovered applying two different extraction approaches, namely ultrasound-assisted solid/liquid extraction (UA-SLE) and solid-phase extraction (SPE). Different solvents were tested evaluating total phenolic compounds and total flavonoids contents together to antioxidant activity. The optimum extraction conditions, in terms of the highest value of total phenolic compounds extracted together to other parameters like simplicity and cost were selected for method validation and individual phenolic compounds analysis. The UA-SLE protocol performed using 0.1 g of defatted sample and 15 mL of extraction solvent (1 mL methanol/1 mL water/8 mL methanol 0.1% formic acid/5 mL acetonitrile) was selected. The analysis of hazelnut kernel individual phenolic compounds was obtained by HPLC coupled with DAD and MS detections. Quantitative analysis was performed using a mixture of six phenolic compounds belonging to phenolic classes' representative of hazelnut. Then, the method was fully validated and the resulting RSD% values for retention time repeatability were below 1%. A good linearity was obtained giving R 2 no lower than 0.997.The accuracy of the extraction method was also assessed. Finally, the method was applied to the analysis of phenolic compounds in three different hazelnut kernel varieties observing a similar qualitative profile with differences in the quantity of detected compounds. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Coupling a Transient Solvent Extraction Module with the Separations and Safeguards Performance Model

    Energy Technology Data Exchange (ETDEWEB)

    de Almeida, Valmor F [ORNL; Birdwell Jr, Joseph F [ORNL; DePaoli, David W [ORNL; Gauld, Ian C [ORNL

    2009-10-01

    A past difficulty in safeguards design for reprocessing plants is that no code existed for analysis and evaluation of the design. A number of codes have been developed in the past, but many are dated, and no single code is able to cover all aspects of materials accountancy, process monitoring, and diversion scenario analysis. The purpose of this work was to integrate a transient solvent extraction simulation module developed at Oak Ridge National Laboratory, with the SSPM Separations and Safeguards Performance Model, developed at Sandia National Laboratory, as a first step toward creating a more versatile design and evaluation tool. The SSPM was designed for materials accountancy and process monitoring analyses, but previous versions of the code have included limited detail on the chemical processes, including chemical separations. The transient solvent extraction model is based on the ORNL SEPHIS code approach to consider solute build up in a bank of contactors in the PUREX process. Combined, these capabilities yield a much more robust transient separations and safeguards model for evaluating safeguards system design. This coupling and the initial results are presented. In addition, some observations toward further enhancement of separations and safeguards modeling based on this effort are provided, including: items to be addressed in integrating legacy codes, additional improvements needed for a fully functional solvent extraction module, and recommendations for future integration of other chemical process modules.

  5. Sugaring-out extraction of acetoin from fermentation broth by coupling with fermentation.

    Science.gov (United States)

    Dai, Jian-Ying; Ma, Lin-Hui; Wang, Zhuang-Fei; Guan, Wen-Tian; Xiu, Zhi-Long

    2017-03-01

    Acetoin is a natural flavor and an important bio-based chemical which could be separated from fermentation broth by solvent extraction, salting-out extraction or recovered in the form of derivatives. In this work, a novel method named as sugaring-out extraction coupled with fermentation was tried in the acetoin production by Bacillus subtilis DL01. The effects of six solvents on bacterial growth and the distribution of acetoin and glucose in different solvent-glucose systems were explored. The operation parameters such as standing time, glucose concentration, and volume ratio of ethyl acetate to fermentation broth were determined. In a system composed of fermentation broth, glucose (100%, m/v) and two-fold volume of ethyl acetate, nearly 100% glucose was distributed into bottom phase, and 61.2% acetoin into top phase without coloring matters and organic acids. The top phase was treated by vacuum distillation to remove solvent and purify acetoin, while the bottom phase was used as carbon source to produce acetoin in the next batch of fermentation.

  6. Coupling a transient solvent extraction module with the separations and safeguards performance model.

    Energy Technology Data Exchange (ETDEWEB)

    DePaoli, David W. (Oak Ridge National Laboratory, Oak Ridge, TN); Birdwell, Joseph F. (Oak Ridge National Laboratory, Oak Ridge, TN); Gauld, Ian C. (Oak Ridge National Laboratory, Oak Ridge, TN); Cipiti, Benjamin B.; de Almeida, Valmor F. (Oak Ridge National Laboratory, Oak Ridge, TN)

    2009-10-01

    A number of codes have been developed in the past for safeguards analysis, but many are dated, and no single code is able to cover all aspects of materials accountancy, process monitoring, and diversion scenario analysis. The purpose of this work was to integrate a transient solvent extraction simulation module developed at Oak Ridge National Laboratory, with the Separations and Safeguards Performance Model (SSPM), developed at Sandia National Laboratory, as a first step toward creating a more versatile design and evaluation tool. The SSPM was designed for materials accountancy and process monitoring analyses, but previous versions of the code have included limited detail on the chemical processes, including chemical separations. The transient solvent extraction model is based on the ORNL SEPHIS code approach to consider solute build up in a bank of contactors in the PUREX process. Combined, these capabilities yield a more robust transient separations and safeguards model for evaluating safeguards system design. This coupling and initial results are presented. In addition, some observations toward further enhancement of separations and safeguards modeling based on this effort are provided, including: items to be addressed in integrating legacy codes, additional improvements needed for a fully functional solvent extraction module, and recommendations for future integration of other chemical process modules.

  7. Continuous production of biodiesel from microalgae by extraction coupling with transesterification under supercritical conditions.

    Science.gov (United States)

    Zhou, Dan; Qiao, Baoquan; Li, Gen; Xue, Song; Yin, Jianzhong

    2017-08-01

    Raw material for biodiesel has been expanded from edible oil to non-edible oil. In this study, biodiesel continuous production for two kinds of microalgae Chrysophyta and Chlorella sp. was conducted. Coupling with the supercritical carbon dioxide extraction, the oil of microalgae was extracted firstly, and then sent to the downstream production of biodiesel. The residue after decompression can be reused as the material for pharmaceuticals and nutraceuticals. Results showed that the particle size of microalgae, temperature, pressure, molar ration of methanol to oil, flow of CO 2 and n-hexane all have effects on the yield of biodiesel. With the optimal operation conditions: 40mesh algae, extraction temperature 60°C, flow of n-hexane 0.4ml/min, reaction temperature: 340°C, pressure: 18-20MPa, CO 2 flow of 0.5L/min, molar ration of methanol to oil 84:1, a yield of 56.31% was obtained for Chrysophyta, and 63.78% for Chlorella sp. due to the higher lipid content. Copyright © 2017. Published by Elsevier Ltd.

  8. Electromagnetic Coupling Between High Intensity LHC Beams and the Synchrotron Radiation Monitor Light Extraction System

    CERN Document Server

    Andreazza, W; Bravin, E; Caspers, F; Garlasch`e, M; Gras, J; Goldblatt, A; Lefevre, T; Jones, R; Metral, E; Nosych, A; Roncarolo_, F; Salvant, B; Trad, G; Veness, R; Vollinger, C; Wendt, M

    2013-01-01

    The CERN LHC is equipped with two Synchrotron Radiation Monitor (BSRT) systems used to characterise transverse and longitudinal beam distributions. Since the end of the 2011 LHC run the light extraction system, based on a retractable mirror, has suffered deformation and mechanical failure that is correlated to the increase in beam intensity. Temperature probes have associated these observations to a strong heating of the mirror support with a dependence on the longitudinal bunch length and shape, indicating the origin as electromagnetic coupling between the beam and the structure. This paper combines all this information with the aim of characterising and improving the system in view of its upgrade during the current LHC shutdown. Beam-based observations are presented along with electromagnetic and thermomechanical simulations and complemented by laboratory measurements, including the study of the RF properties of different mirror bulk and coating materials.

  9. 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.

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

    Science.gov (United States)

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

    2016-01-01

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

  11. Tetraquark candidate Zc(3900) from coupled-channel scattering - how to extract hadronic interactions? -

    Science.gov (United States)

    Ikeda, Yoichi

    2018-03-01

    We present recent progress of lattice QCD studies on hadronic interactions which play a crucial role to understand the properties of atomic nuclei and hadron resonances. There are two methods, the plateau method (or the direct method) and the HAL QCD method, to study the hadronic interactions. In the plateau method, the determination of a ground state energy from the temporal correlation functions of multi-hadron systems is a key to reliably extract the physical observables. It turns out that, due to the contamination of excited elastic scattering states nearby, one can easily be misled by a fake plateau into extracting the ground state energy. We introduce a consistency check (sanity check) which can rule out obviously false results obtained from a fake plateau, and find that none of the results obtained at the moment for two-baryon systems in the plateau method pass the test. On the other hand, the HAL QCD method is free from the fake-plateau problem. We investigate the systematic uncertainties of the HAL QCD method, which are found to be well controlled. On the basis of the HAL QCD method, the structure of the tetraquark candidate Zc(3900), which was experimentally reported in e+e- collisions, is studied by the s-wave two-meson coupled-channel scattering. The results show that the Zc(3900) is not a conventional resonance but a threshold cusp. A semi-phenomenological analysis with the coupled-channel interaction to the experimentally observed decay mode is also presented to confirm the conclusion.

  12. Lamb wave extraction of dispersion curves in micro/nano-plates using couple stress theories

    Science.gov (United States)

    Ghodrati, Behnam; Yaghootian, Amin; Ghanbar Zadeh, Afshin; Mohammad-Sedighi, Hamid

    2018-01-01

    In this paper, Lamb wave propagation in a homogeneous and isotropic non-classical micro/nano-plates is investigated. To consider the effect of material microstructure on the wave propagation, three size-dependent models namely indeterminate-, modified- and consistent couple stress theories are used to extract the dispersion equations. In the mentioned theories, a parameter called 'characteristic length' is used to consider the size of material microstructure in the governing equations. To generalize the parametric studies and examine the effect of thickness, propagation wavelength, and characteristic length on the behavior of miniature plate structures, the governing equations are nondimensionalized by defining appropriate dimensionless parameters. Then the dispersion curves for phase and group velocities are plotted in terms of a wide frequency-thickness range to study the lamb waves propagation considering microstructure effects in very high frequencies. According to the illustrated results, it was observed that the couple stress theories in the Cosserat type material predict more rigidity than the classical theory; so that in a plate with constant thickness, by increasing the thickness to characteristic length ratio, the results approach to the classical theory, and by reducing this ratio, wave propagation speed in the plate is significantly increased. In addition, it is demonstrated that for high-frequency Lamb waves, it converges to dispersive Rayleigh wave velocity.

  13. Superoxide radical and UV irradiation in ultrasound assisted oxidative desulfurization (UAOD): A potential alternative for greener fuels

    Science.gov (United States)

    Chan, Ngo Yeung

    This study is aimed at improving the current ultrasound assisted oxidative desulfurization (UAOD) process by utilizing superoxide radical as oxidant. Research was also conducted to investigate the feasibility of ultraviolet (UV) irradiation-assisted desulfurization. These modifications can enhance the process with the following achievements: (1) Meet the upcoming sulfur standards on various fuels including diesel fuel oils and residual oils; (2) More efficient oxidant with significantly lower consumption in accordance with stoichiometry; (3) Energy saving by 90%; (4) Greater selectivity in petroleum composition. Currently, the UAOD process and subsequent modifications developed in University of Southern California by Professor Yen's research group have demonstrated high desulfurization efficiencies towards various fuels with the application of 30% wt. hydrogen peroxide as oxidant. The UAOD process has demonstrated more than 50% desulfurization of refractory organic sulfur compounds with the use of Venturella type catalysts. Application of quaternary ammonium fluoride as phase transfer catalyst has significantly improved the desulfurization efficiency to 95%. Recent modifications incorporating ionic liquids have shown that the modified UAOD process can produce ultra-low sulfur, or near-zero sulfur diesels under mild conditions with 70°C and atmospheric pressure. Nevertheless, the UAOD process is considered not to be particularly efficient with respect to oxidant and energy consumption. Batch studies have demonstrated that the UAOD process requires 100 fold more oxidant than the stoichiometic requirement to achieve high desulfurization yield. The expected high costs of purchasing, shipping and storage of the oxidant would reduce the practicability of the process. The excess use of oxidant is not economically desirable, and it also causes environmental and safety issues. Post treatments would be necessary to stabilize the unspent oxidant residual to prevent the waste

  14. Novel Approaches to Extraction Methods in Recovery of Capsaicin from Habanero Pepper (CNPH 15.192).

    Science.gov (United States)

    Martins, Frederico S; Borges, Leonardo L; Ribeiro, Claudia S C; Reifschneider, Francisco J B; Conceição, Edemilson C

    2017-07-01

    The objective of this study was to compare three capsaicin extraction methods: Shoxlet, Ultrasound-assisted Extraction (UAE), and Shaker-assisted Extraction (SAE) from Habanero pepper, CNPH 15.192. The different parameters evaluated were alcohol degree, time extraction, and solid-solvent ratio using response surface methodology (RSM). The three parameters found significant ( p Soxhlet increased the extraction in 10-25%; however, long extraction times (45 minutes) degraded 2% capsaicin. The extraction of capsaicin was influenced by extraction method and by the operating conditions chosen. The optimized conditions provided savings of time, solvent, and herbal material. Prudent choice of the extraction method is essential to ensure optimal yield of extract, thereby making the study relevant and the knowledge gained useful for further exploitation and application of this resource. Habanero pepper , line CNPH 15.192, possess capsaicin in higher levels when compared with others speciesHigher levels of ethanolic strength are more suitable to obtain a higher levels of capsaicinBox-Behnken design indicates to be useful to explore the best conditions of ultrasound assisted extraction of capsaicin. Abbreviations used: Nomenclature UAE: Ultrasound-assisted Extraction; SAE: Shaker-assisted Extraction.

  15. Optimizing Conditions for Ultrasound Extraction of Fullerenes from Coal Matrices

    Czech Academy of Sciences Publication Activity Database

    Vítek, P.; Jehlička, J.; Frank, Otakar; Hamplová, Věra; Pokorná, Zdeňka; Juha, Libor; Boháček, J.

    2009-01-01

    Roč. 17, č. 2 (2009), s. 109-122 ISSN 1536-383X R&D Projects: GA ČR GA205/07/0772; GA ČR GA205/03/1468 Institutional research plan: CEZ:AV0Z40400503; CEZ:AV0Z10100520 Keywords : fullerene C60 * Ultrasound -assisted extraction * Extraction yield * Fullerene decomposition Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 0.710, year: 2009

  16. 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).

  17. Rapid ultrasound-assisted magnetic microextraction of gallic acid from urine, plasma and water samples by HKUST-1-MOF-Fe3O4-GA-MIP-NPs: UV-vis detection and optimization study.

    Science.gov (United States)

    Asfaram, Arash; Ghaedi, Mehrorang; Dashtian, Kheibar

    2017-01-01

    Magnetite (Fe 3 O 4 nanoparticles (NPs)) HKUST-1 metal organic framework (MOF) composite as a support was used for surface imprinting of gallic acid imprinted polymer (HKUST-1-MOF-Fe 3 O 4 -GA-MIP) using vinyltrimethoxysilane (VTMOS) as the cross-linker. Subsequently, HKUST-1-MOF-Fe 3 O 4 -NPs-GA-MIP characterized by FT-IR, XRD and FE-SEM analysis and applied for fast and selective and sensitive ultrasound assisted dispersive magnetic solid phase microextraction of gallic acid (GA) by UV-Vis (UA-DMSPME-UV-Vis) detection method. Plackett-Burman design (PBD) and central composite design (CCD) according to desirability function (DF) indicate the significant variables among the extraction factors vortex (mixing) time (min), sonication time (min), temperature (°C), eluent volume (L), pH and HKUST-1-MOF-Fe 3 O 4 -NPs-GA-MIP mass (mg) and their contribution on the response. Optimum conditions and values correspond to pH, HKUST-1-MOF-Fe 3 O 4 -NPs-GA-MIP mass, sonication time and the eluent volume were set as follow 3.0, 1.6mg, 4.0min and 180μL, respectively. The average recovery (ER%) of GA was 98.13% with desirability of 0.997, while the present method has best operational performance like wide linear range 8-6000ngmL -1 with a Limit of detection (LOD) of 1.377ngmL -1 , limit of quantification (LOQ) 4.591ngmL -1 and precision (<3.50% RSD). The recovery of GA in urine, human plasma and water samples within the range of 92.3-100.6% that strongly support high applicability of present method for real samples analysis, which candidate this method as promise for further application. Copyright © 2016. Published by Elsevier B.V.

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

    Science.gov (United States)

    Fazelirad, Hamid; Taher, Mohammad Ali

    2013-01-15

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

  19. Numerical simulation of the heat extraction in EGS with thermal-hydraulic-mechanical coupling method based on discrete fractures model

    International Nuclear Information System (INIS)

    Sun, Zhi-xue; Zhang, Xu; Xu, Yi; Yao, Jun; Wang, Hao-xuan; Lv, Shuhuan; Sun, Zhi-lei; Huang, Yong; Cai, Ming-yu; Huang, Xiaoxue

    2017-01-01

    The Enhanced Geothermal System (EGS) creates an artificial geothermal reservoir by hydraulic fracturing which allows heat transmission through the fractures by the circulating fluids as they extract heat from Hot Dry Rock (HDR). The technique involves complex thermal–hydraulic–mechanical (THM) coupling process. A numerical approach is presented in this paper to simulate and analyze the heat extraction process in EGS. The reservoir is regarded as fractured porous media consisting of rock matrix blocks and discrete fracture networks. Based on thermal non-equilibrium theory, the mathematical model of THM coupling process in fractured rock mass is used. The proposed model is validated by comparing it with several analytical solutions. An EGS case from Cooper Basin, Australia is simulated with 2D stochastically generated fracture model to study the characteristics of fluid flow, heat transfer and mechanical response in geothermal reservoir. The main parameters controlling the outlet temperature of EGS are also studied by sensitivity analysis. The results shows the significance of taking into account the THM coupling effects when investigating the efficiency and performance of EGS. - Highlights: • EGS reservoir comprising discrete fracture networks and matrix rock is modeled. • A THM coupling model is proposed for simulating the heat extraction in EGS. • The numerical model is validated by comparing with several analytical solutions. • A case study is presented for understanding the main characteristics of EGS. • The THM coupling effects are shown to be significant factors to EGS's running performance.

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

    Science.gov (United States)

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

    2018-04-01

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

  1. Measurement of jet production with the ATLAS detector and extraction of the strong coupling constant

    CERN Document Server

    Sawyer, Lee; The ATLAS collaboration

    2017-01-01

    The production of jets at hadron colliders provides a stringent test of perturbative QCD at the highest energies. The process can also be used to probe the gluon density function of the proton. Specific topologies can be used to extract the strong coupling constant. The ATLAS collaboration has recently measured the inclusive jet production cross section in data collected at a center-of-mass energy of 8TeV and 13TeV. The measurements have been performed differentially in jet rapidity and transverse momentum. The collaboration also presents a first measurement of the di-jet cross section at a center-of-mass energy of 13TeV as a function of the di-jet mass and rapidity. The results have been compared with state-of-the-art theory predictions at NLO in pQCD, interfaced with different parton distribution functions and can be used to constrain the proton structure. We also present new measurements of transverse energy-energy correlations (TEEC) and their associated asymmetries (ATEEC) in multi-jet events at a center...

  2. Biocompatibility assessment of graphene oxide-hydroxyapatite coating applied on TiO2 nanotubes by ultrasound-assisted pulse electrodeposition.

    Science.gov (United States)

    Fathyunes, Leila; Khalil-Allafi, Jafar; Sheykholeslami, Seyed Omid Reza; Moosavifar, Maryam

    2018-06-01

    In this study, the ultrasound-assisted pulse electrodeposition was introduced to fabricate the graphene oxide (GO)-hydroxyapatite (HA) coating on TiO 2 nanotubes. The results of the X-ray diffraction (XRD), Fourier Transform Infrared spectroscope (FTIR), Transmission Electron Microscope (TEM) and micro-Raman spectroscopy showed the successful synthesis of GO. The Scanning Electron Microscope (SEM) images revealed that in the presence of ultrasonic waves and GO sheets a more compact HA-based coating with refined microstructure could be formed on the pretreated titanium. The results of micro-Raman analysis confirmed the successful incorporation of the reinforcement filler of GO into the coating electrodeposited by the ultrasound-assisted method. The FTIR analysis showed that the GO-HA coating was consisted predominantly of the B-type carbonated HA (CHA) phase. The pretreatment of the substrate and incorporation of the GO sheets into the HA coating had a significant effect on improving the bonding strength at the coating-substrate interface. Moreover, the results of the fibroblast cell culture and 3‑(4,5‑dimethylthiazolyl‑2)‑2, 5‑diphenyltetrazolium bromide (MTT) assay after 2 days demonstrated a higher percentage of cell activity for the GO-HA coated sample. Finally, the 7-day exposure to simulated body fluid (SBF) showed a faster rate of apatite precipitation on the GO-HA coating, as compared to the HA coating and pretreated titanium. Copyright © 2018 Elsevier B.V. All rights reserved.

  3. Synthesis and characterization of ultrasound assisted “graphene oxide–magnetite” hybrid, and investigation of its adsorption properties for Sr(II) and Co(II) ions

    Energy Technology Data Exchange (ETDEWEB)

    Tayyebi, Ahmad; Outokesh, Mohammad, E-mail: Outokesh@sharif.edu; Moradi, Shahab; Doram, Amir

    2015-10-30

    Graphical abstract: - Highlights: • Narrow size magnetite NPs were synthesized by ultrasound assisted coprecipitaion method. • A formation mechanism for deposition of magnetite NPs on graphene oxide is proposed. • The formation mechanism supported using X-ray photoelectron spectroscopy analysis. • The modified Langevin equation was used for size estimation of magnetite NPs on M–GO. • Adsorption properties of M–GO for Co(II) and Sr(II) were investigated. - Abstract: Magnetite nanoparticles with a size distribution of 15–21 nm were synthesized and decorated onto surface of graphene oxide by ultrasound assisted precipitation. Size and size distribution of the obtained M–GO hybrid were appreciably finer than the hybrids prepared by stirring method. M–GO is a superparamagnetic material with saturation magnetization of 31 emu g{sup −1}. The Langevin equation was successfully applied for estimation of size of Fe{sub 3}O{sub 4} nanoparticles in M–GO hybrid, with maximum error of 17.5%. The study put forward a formation mechanism for M–GO, based on instrumental analyses. Adsorption isotherms of Sr{sup 2+} and Co{sup 2+} ions, which were fitted by Langmuir monolayer model, displayed two-fold higher capacity for Co{sup 2+} ions, presumably due to its similarity to Fe{sup 2+} (of Fe{sub 3}O{sub 4} component). Uptake of both Co{sup 2+} and Sr{sup 2+} ions were endothermic, and spontaneous, however the former proceeded through inner-shell complex formation, while the latter took place via ion exchange mechanism. Rate of adsorption of Co{sup 2+} was faster, but for both ions, chemical reaction was the rate determining step. Sorption of Sr{sup 2+} and Co{sup 2+} ions greatly increased at pHs above 5, where (1) surface zeta potential changed its sign, and (2) deprotonating reactions at the surface became complete.

  4. Fe(II)–Al(III) layered double hydroxides prepared by ultrasound-assisted co-precipitation method for the reduction of bromate

    International Nuclear Information System (INIS)

    Zhong, Yu; Yang, Qi; Luo, Kun; Wu, Xiuqiong; Li, Xiaoming; Liu, Yang; Tang, Wangwang; Zeng, Guangming; Peng, Bo

    2013-01-01

    Highlights: ► Fe(II)–Al(III) LDHs were synthesized by ultrasound-assisted co-precipitation method. ► The Fe–Al (30 min) exhibited highly reduction reactivity on bromate. ► Pseudo-first-order model described the experimental data well. ► The mechanisms of bromate removal were proposed. -- Abstract: Bromate is recognized as an oxyhalide disinfection byproduct in drinking water. In this paper, Fe(II)–Al(III) layered double hydroxides (Fe–Al LDHs) prepared by the ultrasound-assisted co-precipitation method were used for the reduction of bromate in solution. The Fe–Al LDHs particles were characterized by X-ray diffractometer, scanning electron microscopy and thermogravimetry–differential scanning calorimetry. It was found that ultrasound irradiation assistance promoted the formation of the hydrotalcite-like phase and then improved the removal efficiency of bromate. In addition, the effects of solid-to-solution ratio, contact time, initial bromate concentration, initial pH, coexisting anions on the bromate removal were investigated. The results showed the bromate with an initial concentration of 1.56 μmol/L could be completely removed from solution by Fe–Al LDHs within 120 min. When the initial bromate concentration was 7.81 μmol/L, the Fe–Al LDHs with irradiation time of 30 min exhibited the optimum removal efficiency and the bromate removal capacity (q e ) was 6.80 μmol/g. In addition, the appearance of sulfate and production of bromide were observed simultaneously in this process, which suggested that ion-exchange between sulfate and bromate, and the reduction of bromate to bromide by Fe 2+ were the main mechanisms responsible for the bromate removal by Fe–Al LDHs

  5. A fast, simple and green method for the extraction of carbamate pesticides from rice by microwave assisted steam extraction coupled with solid phase extraction.

    Science.gov (United States)

    Song, Weitao; Zhang, Yiqun; Li, Guijie; Chen, Haiyan; Wang, Hui; Zhao, Qi; He, Dong; Zhao, Chun; Ding, Lan

    2014-01-15

    This paper presented a fast, simple and green sample pretreatment method for the extraction of 8 carbamate pesticides in rice. The carbamate pesticides were extracted by microwave assisted water steam extraction method, and the extract obtained was immediately applied on a C18 solid phase extraction cartridge for clean-up and concentration. The eluate containing target compounds was finally analysed by high performance liquid chromatography with mass spectrometry. The parameters affecting extraction efficiency were investigated and optimised. The limits of detection ranging from 1.1 to 4.2ngg(-1) were obtained. The recoveries of 8 carbamate pesticides ranged from 66% to 117% at three spiked levels, and the inter- and intra-day relative standard deviation values were less than 9.1%. Compared with traditional methods, the proposed method cost less extraction time and organic solvent. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

    Science.gov (United States)

    Werner, Justyna

    2018-05-15

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

  7. Development of new apple beverages rich in isothiocyanates by using extracts obtained from ultrasound-treated cauliflower by-products

    DEFF Research Database (Denmark)

    Amofa-Diatuo, Tracy; Anang, Daniel M.; Barba Orellana, Francisco Jose

    2017-01-01

    The objective of this study was to develop a new apple juice beverage enriched with isothiocyanates (ITC) - rich extracts obtained from cauliflower by-products. Ultrasound-assisted extraction (UAE) at different amplitudes (20-100%) and extraction times (0-10. min) at a frequency of 24. kHz was em......The objective of this study was to develop a new apple juice beverage enriched with isothiocyanates (ITC) - rich extracts obtained from cauliflower by-products. Ultrasound-assisted extraction (UAE) at different amplitudes (20-100%) and extraction times (0-10. min) at a frequency of 24. k......) and UAE (20%, 3. min), respectively. Moreover, the highest recovery of total phenolic compounds (TPC) (≈105. mg gallic acid equivalent (GAE)/L) μM) was found after UAE (100% amplitude, 3. min) of TPC from stems. ITC-rich extracts obtained from caulifower by-products at the optimum UAE conditions were...

  8. [Analysis of saponins from panax notoginseng using pressurized solvent extraction coupled with liquid chromatography-electrospray mass spectrum].

    Science.gov (United States)

    Wan, Jianbo; Li, Changming; Li, Shaopin; Kong, Lingyi; Wang, Yitao

    2005-10-01

    To establish a method for qualitative analysis of saponins from Panax notoginseng using pressurized solvent extraction coupled with LC-ESI-MS. The PSE technology was applied to the process of extraction for Panax notoginseng, and the negative ion detection and multiple reaction monitoring model were used. The saponins were investigated based on total ion chromatogram (TIC) and MRM chromatogram. According to the fragment character of saponins, the molecular weight and their structures could be identified. The method can be used for qualitative analysis of saponins from Panax notoginseng.

  9. Pressurized liquid extraction using water/isopropanol coupled with solid-phase extraction cleanup for industrial and anthropogenic waste-indicator compounds in sediment

    Science.gov (United States)

    Burkhardt, M.R.; ReVello, R.C.; Smith, S.G.; Zaugg, S.D.

    2005-01-01

    A broad range of organic compounds is recognized as environmentally relevant for their potential adverse effects on human and ecosystem health. This method was developed to better determine the distribution of 61 compounds that are typically associated with industrial and household waste as well as some that are toxic and known (or suspected) for endocrine-disrupting potential extracted from environmental sediment samples. Pressurized liquid extraction (PLE) coupled with solid-phase extraction (SPE) was used to reduce sample preparation time, reduce solvent consumption to one-fifth of that required using dichloromethane-based Soxhlet extraction, and to minimize background interferences for full scan GC/MS analysis. Recoveries from spiked Ottawa sand, commercially available topsoil, and environmental stream sediment, fortified at 4-720 ??g per compound, averaged 76 ?? 13%. Initial method detection limits for single-component compounds ranged from 12.5 to 520 ??g/kg, based on 25 g samples. Results from 103 environmental sediment samples show that 36 out of 61 compounds (59%) were detected in at least one sample with concentrations ranging from 20 to 100,000 ??g/kg. The most frequently detected compound, beta-sitosterol, a plant sterol, was detected in 87 of the 103 (84.5%) environmental samples with a concentration range 360-100,000 ??g/kg. Results for a standard reference material using dichloromethane Soxhlet-based extraction are also compared. ?? 2004 Published by Elsevier B.V.

  10. The determination of organochlorine pesticides based on dynamic microwave-assisted extraction coupled with on-line solid-phase extraction of high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Chen Ligang; Ding Lan; Jin Haiyan; Song Daqian; Zhang Huarong; Li Jiantao; Zhang Kun; Wang Yutang; Zhang Hanqi

    2007-01-01

    A rapid technique based on dynamic microwave-assisted extraction coupled with on-line solid-phase extraction of high-performance liquid chromatography (DMAE-SPE-HPLC) has been developed. A TM 010 microwave resonance cavity built in the laboratory was applied to concentrate the microwave energy. The sample placed in the zone of microwave irradiation was extracted with 95% acetonitrile (ACN) aqueous solution which was driven by a peristaltic pump at a flow rate of 1.0 mL min -1 . The extraction can be completed in a recirculating system in 10 min. When a number of extraction cycles were completed, the extract (1 mL) was diluted on-line with water. Then the extract was loaded into an SPE column where the analytes were retained while the unretained matrix components were washed away. Subsequently, the analytes were automatically transferred from the SPE column to the analytical column and determined by UV detector at 238 nm. The technique was used for determination of organochlorine pesticides (OCPs) in grains, including wheat, rice, corn and bean. The limits of detection of OCPs are in the range of 19-37 ng g -1 . The recoveries obtained by analyzing the four spiked grain samples are in the range of 86-105%, whereas the relative standard deviation (R.S.D.) values are <8.7% ranging from 1.2 to 8.7%. Our method was demonstrated to be fast, accurate, and precise. In addition, only small quantities of solvent and sample were required

  11. Extraction inductively coupled plasma-optical emission spectrometry (ICP-OES). Determination of traces of phosphorus in tungsten

    International Nuclear Information System (INIS)

    Bauer, G.; Wegscheider, W.; Mueller, K.

    1989-01-01

    A method for the separation and preconcentration of traces of phosphorus from tungsten was developed. Solid phase extraction of the phosphovanadomolybdate complex performed on a micro-column was applied. Phosphorus was determined by optical emission spectroscopy (OES) with inductively coupled plasma (ICP) excitation. A limit of detection of 0,4 μg/g P with respect to the solid phase is obtained. By directly coupling the extraction/elution step to the ICP instrument a detection limit of 0,06 μg/g P in W was achieved. Besides, the complexity of spectral evaluation in ICP-OES determinations of traces in spectralline-rich matrices is discussed. (Authors)

  12. Couplings

    Science.gov (United States)

    Stošić, Dušan; Auroux, Aline

    Basic principles of calorimetry coupled with other techniques are introduced. These methods are used in heterogeneous catalysis for characterization of acidic, basic and red-ox properties of solid catalysts. Estimation of these features is achieved by monitoring the interaction of various probe molecules with the surface of such materials. Overview of gas phase, as well as liquid phase techniques is given. Special attention is devoted to coupled calorimetry-volumetry method. Furthermore, the influence of different experimental parameters on the results of these techniques is discussed, since it is known that they can significantly influence the evaluation of catalytic properties of investigated materials.

  13. Cat's claw oxindole alkaloid isomerization induced by common extraction methods

    Directory of Open Access Journals (Sweden)

    Samuel Kaiser

    2013-01-01

    Full Text Available Cat's claw oxindole alkaloids are prone to isomerization in aqueous solution. However, studies on their behavior in extraction processes are scarce. This paper addressed the issue by considering five commonly used extraction processes. Unlike dynamic maceration (DM and ultrasound-assisted extraction, substantial isomerization was induced by static maceration, turbo-extraction and reflux extraction. After heating under reflux in DM, the kinetic order of isomerization was established and equations were fitted successfully using a four-parameter Weibull model (R² > 0.999. Different isomerization rates and equilibrium constants were verified, revealing a possible matrix effect on alkaloid isomerization.

  14. Preconcentration of uranium in water samples using dispersive liquid-liquid micro- extraction coupled with solid-phase extraction and determination with inductively coupled plasma-optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    M. Rezaee,

    2015-10-01

    Full Text Available A new liquid phase microextraction method based on the dispersion of an extraction solvent into aqueous phase coupled with solid-phase extraction was investigated for the extraction, preconcentration and determination of uranium in water samples. 1-(2-Pyridylazo-2-naphthol reagent (PAN at pH 6.0 was used as a chelating agent prior to extraction. After concentration and purification of the samples in SPE C18 sorbent, 1.5 mL elution sample containing 40.0 µL chlorobenzene was injected into the 5.0 mL pure water. After extraction and centrifuging, the sedimented phase was evaporated and the residue was dissolved in nitric acid (0.5 M and was injected by injection valve into the ICP-OES. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition were studied and optimized. Under the optimum conditions, the calibration graph was linear in the range of 0.5-500 µg L-1. The detection limit was 0.1 µg L-1. The relative standard deviation (RSD at 5.0 µg L-1 concentration level was 6.6%. Finally, the developed method was successfully applied to the extraction and determination of uranium in the well, river, mineral, waste and tap water samples and satisfactory results were obtained.DOI: http://dx.doi.org/10.4314/bcse.v29i3.4

  15. Arsenic removal from As-hyperaccumulator Pteris vittata biomass: Coupling extraction with precipitation.

    Science.gov (United States)

    da Silva, Evandro B; de Oliveira, Letuzia M; Wilkie, Ann C; Liu, Yungen; Ma, Lena Q

    2018-02-01

    Proper disposal of As-hyperaccumulator Pteris vittata biomass (Chinese brake fern) enhances its application in phytoremediation. The goal of this study was to optimize As removal from P. vittata (PV) biomass by testing different particle sizes, extractants, extraction times and solid-to-liquid ratios. PV biomass was extracted using different extractants followed by different Mg-salts to recover soluble As via precipitation. Water-soluble As in PV biomass varied from 6.8% to 61% of total As depending on extraction time, with 99% of As being arsenate (AsV). Extraction with 2.1% HCl, 2.1% H 3 PO 4 , 1 M NaOH and 50% ethanol recovered 81, 78, 47 and 14% of As from PV biomass. A follow-up extraction using HCl recovered 27-32% with ethanol recovering only 5%. Though ethanol showed the lowest extractable As, residual As in the biomass was also the lowest. Among the extractants, 35% ethanol was the best to remove As from PV biomass. Approximately 90% As was removed from PV biomass using particle size phytoremediation more feasible. Published by Elsevier Ltd.

  16. Direct coupling of electromembrane extraction to mass spectrometry – Advancing the probe functionality toward measurements of zwitterionic drug metabolites

    DEFF Research Database (Denmark)

    Kige Rye, Torstein; Fuchs, David; Pedersen-Bjergaard, Stig

    2017-01-01

    A triple-flow electromembrane extraction (EME) probe was developed and coupled directly to electrospray-ionization mass spectrometry (ESI-MS). Metabolic reaction mixtures (pH 7.4) containing drug substances and related metabolites were continuously drawn (20 μL/min) into the EME probe in one flow......-nitrophenyl octyl ether (and for some experiments containing 30% triphenyl phosphate (TPP)), and into 20 μL min-1 of formic acid as acceptor phase, which was introduced through a third flow channel. The acceptor phase was pumped directly to the MS system, and the ion intensity of extracted analytes......, the system can potentially be used for direct analysis of various kinds of chemical reactions that have to be run at pH conditions unfavorable for direct analyte extractions....

  17. 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

  18. Direct coupling of electromembrane extraction to mass spectrometry - Advancing the probe functionality toward measurements of zwitterionic drug metabolites.

    Science.gov (United States)

    Rye, Torstein Kige; Fuchs, David; Pedersen-Bjergaard, Stig; Petersen, Nickolaj Jacob

    2017-08-29

    A triple-flow electromembrane extraction (EME) probe was developed and coupled directly to electrospray-ionization mass spectrometry (ESI-MS). Metabolic reaction mixtures (pH 7.4) containing drug substances and related metabolites were continuously drawn (20 μL/min) into the EME probe in one flow channel, and mixed inside the probe with 7.5 μL min -1 of 1 M formic acid as make-up flow from a second flow channel. Following this acidification, the drug substances and their related metabolites were continuously extracted by EME at 400 V, across a supported liquid membrane (SLM) comprising 2-nitrophenyl octyl ether (and for some experiments containing 30% triphenyl phosphate (TPP)), and into 20 μL min -1 of formic acid as acceptor phase, which was introduced through a third flow channel. The acceptor phase was pumped directly to the MS system, and the ion intensity of extracted analytes was followed continuously as function of time. The triple-flow EME probe was used for co-extraction of positively charged parent drugs and their zwitterionic drug metabolites (hydroxyzine and its carboxylic acid metabolite cetirizine; and vortioxetine and its carboxylic acid metabolite Lu AA34443). While the zwitterionic metabolites could not be extracted at pH 7.4, it was shown that by acidifying the sample solution the zwitterionic metabolites could be extracted effectively. Various extraction parameters like make-up flow, extraction voltage and SLM composition were optimized for simultaneous extraction of parent drugs and metabolites. It was found that TPP added to the SLM improved extraction efficiencies of certain drug metabolites. Finally the optimized and characterized triple-flow EME probe was used for online studying the in-vitro metabolism of hydroxyzine and vortioxetine by rat liver microsomes. Due to the automated pre-extraction acidification of the rat liver microsomal solutions, it was possible to continuously monitor formation of the zwitterionic drug

  19. Use of ultrasound radiation for extraction of bioactive compounds from natural sources. Current events and perspectives

    International Nuclear Information System (INIS)

    Rodriguez Riera, Zalua; Robaina Mesa, Malvis; Jauregui Haza, Ulises

    2014-01-01

    In recent years, clean technologies have been developed for high efficiency extracting of isolation of biologically active compounds from natural sources, without the loss of biological activity, with good yield and high purity. Ultrasound-assisted extraction has low instrumental requirements and their implementation is very appropriate where the stability of the active component to be removed is affected by the high temperatures of conventional processes. In this paper it is evaluated the state of the art of ultrasound-assisted extraction of bioactive compounds from various natural sources, its mechanism, the parameters governing its use and research perspectives in this field. Ultrasonic cavitation phenomenon promotes cell wall rupture, reduction of particle size and tissue permeability, which facilitates the diffusion of the solvent into the inert part of the plant material and increasing the mass transferred through membranes. This mechanism explains the high efficiency of ultrasound-assisted extraction as it allows to reduce the time, temperature and amounts of solvent extraction process with high yields and high purity of the extracted product. Currently there is a great demand for the use of ultrasound to industrial and current research lead to the development of larger scale reactors and the theoretical modeling of the parameters that determine efficient extraction

  20. Effective coupling functions extracted from the scattering experiments with polarized protons at moderate energies

    International Nuclear Information System (INIS)

    Barut, A.O.; Anders, T.B.; Jachmann, W.

    1992-06-01

    The experimental data for the polarization asymmetries of pp-scattering available at the scattering angle θ = 90 deg. and at various moderate energies, as well as at E = 2.4434 GeV and various scattering angles are described by smooth phenomenological coupling functions for scalar, vector, tensor and the ''magnetic moment'' couplings as well as the corresponding parity conserving axial couplings. The analysis shows a predominant role of the ''axial magnetic moment'', the axial scalar, and the axial vector interactions. Moreover, the data contain oscillations of the type sin(qw 0 -π)/(qw 0 -π), where q is the square root of the energy-momentum transfer. The oscillations have amplitudes of 5%, and a constant frequency w o = 2π/0.88 m p . They arise from oscillating modulations up to 25% of the non-axial coupling functions. 8 refs, 21 figs, 4 tabs

  1. Tetraquark candidate Zc(3900 from coupled-channel scattering - how to extract hadronic interactions? -

    Directory of Open Access Journals (Sweden)

    Ikeda Yoichi

    2018-01-01

    On the basis of the HAL QCD method, the structure of the tetraquark candidate Zc(3900, which was experimentally reported in e+e- collisions, is studied by the s-wave two-meson coupled-channel scattering. The results show that the Zc(3900 is not a conventional resonance but a threshold cusp. A semi-phenomenological analysis with the coupled-channel interaction to the experimentally observed decay mode is also presented to confirm the conclusion.

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

    Science.gov (United States)

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

    2017-09-10

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

  3. Postharvest Ultrasound-Assisted Freeze-Thaw Pretreatment Improves the Drying Efficiency, Physicochemical Properties, and Macamide Biosynthesis of Maca (Lepidium meyenii).

    Science.gov (United States)

    Chen, Jin-Jin; Gong, Peng-Fei; Liu, Yi-Lan; Liu, Bo-Yan; Eggert, Dawn; Guo, Yuan-Heng; Zhao, Ming-Xia; Zhao, Qing-Sheng; Zhao, Bing

    2018-04-01

    A novel technique of ultrasound-assisted freeze-thaw pretreatment (UFP) was developed to improve the drying efficiency of maca and bioactive amide synthesis in maca. The optimal UFP conditions are ultrasonic processing 90 min at 30 °C with 6 freeze-thaw cycles. Samples with freeze-thaw pretreatment (FP), ultrasound pretreatment (UP), and UFP were prepared for further comparative study. A no pretreatment (NP) sample was included as a control. The results showed that UFP improved the drying efficiency of maca slices, showing the highest effective moisture diffusivity (1.75 × 10 -9 m 2 /s). This result was further supported by low-field nuclear magnetic resonance (LF-NMR) analysis and scanning electron microscopy (SEM). The rehydration capacity and protein content of maca slices were improved by UFP. More importantly, contents of bioactive macamides and their biosynthetic precursors were increased in 2.5- and 10-fold, respectively. In conclusion, UFP is an efficient technique to improve drying efficiency, physicochemical properties, and bioactive macamides of maca, which can be applied in the industrial manufacture of maca products. © 2018 Institute of Food Technologists®.

  4. Ultrasound-assisted leaching of rare earths from the weathered crust elution-deposited ore using magnesium sulfate without ammonia-nitrogen pollution.

    Science.gov (United States)

    Yin, Shaohua; Pei, Jiannan; Jiang, Feng; Li, Shiwei; Peng, Jinhui; Zhang, Libo; Ju, Shaohua; Srinivasakannan, Chandrasekar

    2018-03-01

    The in situ leaching process of China's unique ion-adsorption rare earth ores has caused severe environmental damages due to the use of (NH 4 ) 2 SO 4 solution. This study reports that magnesium sulfate (MgSO 4 ) as a leaching agent would replace (NH 4 ) 2 SO 4 by ultrasonically assisted leaching to deal with the ammonia-nitrogen pollution problem and enhance leaching process. At leaching conditions of 3wt% MgSO 4 concentration, 3:1L/S ratio and 30min, the total rare earth leaching efficiency reaches 75.5%. Ultrasound-assisted leaching experiments show that the leaching efficiency of rare earths is substantially increased by introducing ultrasound, and nearly completely leached out after two stage leaching process. Thus, ultrasonic-assisted leaching process with MgSO 4 is not only effective but also environmentally friendly, and beneficial to leach rare earths at laboratory scale. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Determination of personal care products and hormones in leachate and groundwater from Polish MSW landfills by ultrasound-assisted emulsification microextraction and GC-MS.

    Science.gov (United States)

    Kapelewska, Justyna; Kotowska, Urszula; Wiśniewska, Katarzyna

    2016-01-01

    Determination of the endocrine disrupting compounds (EDCs) in leachate and groundwater samples from the landfill sites is very important because of the proven harmful effects of these compounds on human and animal organisms. A method combining ultrasound-assisted emulsification microextraction (USAEME) and gas chromatography-mass spectrometry (GC-MS) was developed for simultaneous determination of seven personal care products (PCPs): methylparaben (MP), ethylparaben (EP), propylparaben (PP), buthylparaben (BP), benzophenone (BPh), 3-(4-methylbenzylidene)camphor (4-MBC), N,N-diethyltoluamide (DEET), and two hormones: estrone (E1) and β-estradiol (E2) in landfill leachate and groundwater samples. The limit of detection (LOD)/limit of quantification (LOQ) values in landfill leachate and groundwater samples were in the range of 0.003-0.083/0.009-0.277 μg L(-1) and 0.001-0.015/0.002-0.049 μg L(-1), respectively. Quantitative recoveries and satisfactory precision were obtained. All studied compounds were found in the landfill leachates from Polish municipal solid waste (MSW) landfills; the concentrations were between 0.66 and 202.42 μg L(-1). The concentration of pollutants in groundwater samples was generally below 0.1 μg L(-1).

  6. Ultrasound assisted production of fatty acid methyl esters from transesterification of triglycerides with methanol in the presence of KOH catalyst: optimization, mechanism and kinetics.

    Science.gov (United States)

    Thanh, Le Tu; Okitsu, Kenji; Maeda, Yasuaki; Bandow, Hiroshi

    2014-03-01

    Ultrasound assisted transesterification of triglycerides (TG) with methanol in the presence of KOH catalyst was investigated, where the changes in the reactants and products (diglycerides (DG), monoglycerides (MG), fatty acid methyl esters (FAME) and glycerin (GL)) concentrations were discussed to understand the reaction mechanism and kinetics under ultrasound irradiation. The optimum reaction condition for the FAME production was the concentration of KOH 1.0 wt.%, molar ratio of TG to methanol of 1:6, and irradiation time of 25 min. The rate constants during the TG transesterification with methanol into GL and FAME were estimated by a curve fitting method with simulated curves to the obtained experimental results. The rate constants of [Formula: see text] were estimated to be 0.21, 0.008, 0.23, 0.005, 0.14 and 0.001 L mol(-1)min(-1), respectively. The rate determining step for the TG transesterification with methanol into GL and FAME was the reaction of MG with methanol into GL and FAME. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Sensitive Detection of Organophosphorus Pesticides in Medicinal Plants Using Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction Combined with Sweeping Micellar Electrokinetic Chromatography.

    Science.gov (United States)

    Wei, Jin-Chao; Hu, Ji; Cao, Ji-Liang; Wan, Jian-Bo; He, Cheng-Wei; Hu, Yuan-Jia; Hu, Hao; Li, Peng

    2016-02-03

    A simple, rapid, and sensitive method using ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) combined with sweeping micellar electrokinetic chromatography (sweeping-MEKC) has been developed for the determination of nine organophosphorus pesticides (chlorfenvinphos, parathion, quinalphos, fenitrothion, azinphos-ethyl, parathion-methyl, fensulfothion, methidathion, and paraoxon). The important parameters that affect the UA-DLLME and sweeping efficiency were investigated. Under the optimized conditions, the proposed method provided 779.0-6203.5-fold enrichment of the nine pesticides compared to the normal MEKC method. The limits of detection ranged from 0.002 to 0.008 mg kg(-1). The relative standard deviations of the peak area ranged from 1.2 to 6.5%, indicating the good repeatability of the method. Finally, the developed UA-DLLME-sweeping-MEKC method has been successfully applied to the analysis of the investigated pesticides in several medicinal plants, including Lycium chinense, Dioscorea opposite, Codonopsis pilosula, and Panax ginseng, indicating that this method is suitable for the determination of trace pesticide residues in real samples with complex matrices.

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

    Directory of Open Access Journals (Sweden)

    Claude Daneault

    2012-09-01

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

  9. 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

  10. SIMPLE METHOD FOR ESTIMATING POLYCHLORINATED BIPHENYL CONCENTRATIONS ON SOILS AND SEDIMENTS USING SUBCRITICAL WATER EXTRACTION COUPLED WITH SOLID-PHASE MICROEXTRACTION. (R825368)

    Science.gov (United States)

    A rapid method for estimating polychlorinated biphenyl (PCB) concentrations in contaminated soils and sediments has been developed by coupling static subcritical water extraction with solid-phase microextraction (SPME). Soil, water, and internal standards are placed in a seale...

  11. Improved extraction of hydrologic information from geophysical data through coupled hydrogeophysical inversion

    Energy Technology Data Exchange (ETDEWEB)

    Hinnell, A.C.; Ferre, T.P.A.; Vrugt, J.A.; Huisman, J.A.; Moysey, S.; Rings, J.; Kowalsky, M.B.

    2009-11-01

    There is increasing interest in the use of multiple measurement types, including indirect (geophysical) methods, to constrain hydrologic interpretations. To date, most examples integrating geophysical measurements in hydrology have followed a three-step, uncoupled inverse approach. This approach begins with independent geophysical inversion to infer the spatial and/or temporal distribution of a geophysical property (e.g. electrical conductivity). The geophysical property is then converted to a hydrologic property (e.g. water content) through a petrophysical relation. The inferred hydrologic property is then used either independently or together with direct hydrologic observations to constrain a hydrologic inversion. We present an alternative approach, coupled inversion, which relies on direct coupling of hydrologic models and geophysical models during inversion. We compare the abilities of coupled and uncoupled inversion using a synthetic example where surface-based electrical conductivity surveys are used to monitor one-dimensional infiltration and redistribution.

  12. Direct coupling of a flow-flow electromembrane extraction probe to LC-MS

    DEFF Research Database (Denmark)

    Fuchs, David; Gabel-Jensen, Charlotte; Jensen, Henrik

    2016-01-01

    the fully automated EME-LC-MS system offers a significant time saving and in addition demonstrates increased sensitivity as the analytes were automatically enriched during the extraction process. The experiment revealed 6 to 16 times higher S/N ratios of the EME-LC-MS method compared to protein...... precipitation followed by LC-MS and thus concomitantly lower LOD and LOQ. The setup integrates a complete analytical workflow of rapid extraction, enrichment, separation and detection of analytes in a fully automated manner. These attributes make the developed system a powerful alternative approach for a wide...

  13. Isolation of dihydroatemisinic acid from the artemisia annua l. by-product by combining Ultrasound-assisted extraction with response surface methodology

    Science.gov (United States)

    Malaria is one of the world’s most important parasitic diseases, affecting 300-500 million people worldwide and killing more than one million per year. Artemisinin is currently the only raw material for the production of artemisinin combination therapies (ACT), the only medicine that cures drug-resi...

  14. Simultaneous determination of 13 carbohydrates using high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry.

    Science.gov (United States)

    Zhao, Dan; Feng, Feng; Yuan, Fei; Su, Jin; Cheng, Yan; Wu, Hanqiu; Song, Kun; Nie, Bo; Yu, Lian; Zhang, Feng

    2017-04-01

    A simple, accurate, and highly sensitive method was developed for the determination of 13 carbohydrates in polysaccharide of Spirulina platensis based on high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry. Samples were extracted with deionized water using ultrasonic-assisted extraction, and the ultrasound-assisted extraction conditions were optimized by Box-Behnken design. Then the extracted polysaccharide was hydrolyzed by adding 1 mol/L trifluoroacetic acid before determination by high-performance anion-exchange chromatography coupled with pulsed amperometric detection and confirmed by high-performance anion-exchange chromatography coupled with mass spectrometry. The high-performance anion-exchange chromatography coupled with pulsed amperometric detection method was performed on a CarboPac PA20 column by gradient elution using deionized water, 0.1 mol/L sodium hydroxide solution, and 0.4 mol/L sodium acetate solution. Excellent linearity was observed in the range of 0.05-10 mg/L. The average recoveries ranged from 80.7 to 121.7%. The limits of detection and limits of quantification for 13 carbohydrates were 0.02-0.10 and 0.2-1.2  μg/kg, respectively. The developed method has been successfully applied to ambient samples, and the results indicated that high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry could provide a rapid and accurate method for the simultaneous determination of carbohydrates. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Effect of irradiation power and time on ultrasound assisted co-precipitation of nanostructured CuO–ZnO–Al2O3 over HZSM-5 used for direct conversion of syngas to DME as a green fuel

    International Nuclear Information System (INIS)

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

    2014-01-01

    Graphical abstract: Nanostructured CuO–ZnO–Al 2 O 3 /HZSM-5 catalyst has been prepared by an ultrasound-assisted co-precipitation hybrid method. Effect of power and irradiation time have been studied by changing the time (30–45–60 min) and power of sonication (50–100–150 W) during the synthesis which lead to different physiochemical properties of the catalyst. The XRD, FESEM, EDX, FTIR and BET analyses exhibited smaller particles with higher surface area and less population of particle aggregates at longer and highly irradiated catalysts. Study on the performance of investigated catalysts in direct synthesis of DME from syngas showed ultrasound-assisted co-precipitated synthesized catalysts have superior reactivity and stability compared with non-sonicated catalyst. Among sonicated catalysts, with increasing power and time of irradiation, the catalyst represents higher activity and DME selectivity. - Highlights: • Synthesis of CuO–ZnO–Al 2 O 3 /HZSM-5 by ultrasound assisted co-precipitation method. • Significant changes in morphology and surface area after ultrasound irradiations. • Smaller dispersed particle aggregates in longer and more intense irradiated catalysts. • Improvement in reactivity and stability of the longer and more intense ultrasound irradiated CZAZ catalyst. - Abstract: Nanostructured CuO–ZnO–Al 2 O 3 /HZSM-5 catalyst has been prepared by an ultrasound-assisted co-precipitation hybrid method. The effect of irradiation power and irradiation time have been studied by changing time (30, 45, 60 min) and power of the sonication (50, 100, 150 W) during the synthesis which led to different physiochemical properties of the nanocatalyst. The XRD, FESEM, EDX, FTIR and BET analyses exhibited smaller particles with higher surface area and less population of particle aggregates at longer and highly irradiated nanocatalysts. The nanocatalyst irradiated at 150 W for 60 min (the longest irradiation time and the most intense power

  16. Highly efficient removal of chromium(VI) by Fe/Ni bimetallic nanoparticles in an ultrasound-assisted system.

    Science.gov (United States)

    Zhou, Xiaobin; Jing, Guohua; Lv, Bihong; Zhou, Zuoming; Zhu, Runliang

    2016-10-01

    Highly active Fe/Ni bimetallic nanocomposites were prepared by using the liquid-phase reduction method, and they were proven to be effective for Cr(VI) removal coupled with US irradiation. The US-assisted Fe/Ni bimetallic system could maintain a good performance for Cr(VI) removal at a wide pH range of 3-9. Based on the characterization of the Fe/Ni nanoparticles before and after reaction, the high efficiency of the mixed system could attribute to the synergistic effects of the catalysis of Ni(0) and US cavitation. Ni(0) could facilitate the Cr(VI) reduction through electron transfer and catalytic hydrogenation. Meanwhile, US could fluidize the Fe/Ni nanoparticles to increase the actual reactive surface area and clean off the co-precipitated Fe(III)-Cr(III) hydroxides to maintain the active sites on the surface of the Fe/Ni nanoparticles. Thus, compared with shaking, the US-assisted Fe/Ni system was more efficient on Cr(VI) removal, which achieved 94.7% removal efficiency of Cr(VI) within 10 min. The pseudo-first-order rate constant (kobs) in US-assisted Fe/Ni system (0.5075 min(-1)) was over 5 times higher than that under shaking (0.0972 min(-1)). Moreover, the Fe/Ni nanoparticles still have a good performance under US irradiation after 26 days aging as well as regeneration. Copyright © 2016 Elsevier Ltd. All rights reserved.

  17. A simple crunching of the AGS 'bare' machine ORM data - February 2007 - to extract some aspects of AGS transverse coupling at injection and extraction

    International Nuclear Information System (INIS)

    Ahrens, L.

    2010-01-01

    The objective of this note is to (once again) explore the AGS 'ORM' (orbit response matrix) data taken (by Operations) early during the 2007 run with an AGS bare machine and gold beam. Indeed the present motivation is to extract as much information about the AGS inherent transverse coupling as possible - from general arguments and the copious ORM data. And taking this one step further, (though not accomplished yet) the goal really should be to tell the model how to describe this coupling. 'Bare' as used here means the AGS with no quadrupole, sextupole or octupole magnets powered. Only the main (combined-function) magnet string and dipole bumps necessary to optimize beam survival are powered. 'ORM data' means the systematic recording of the equilibrium orbit beam position monitor response to powering individual dipole corrector magnets. The 'matrix' results from looking at the effect of each of the (12 superperiods X 4 dipoles per superperiod) 'kicks' on each of the (12 X 6) pick up electrodes (pues) in each transverse plane. So then we have two (48 X 72) matrices of numbers from the ORM data. (Though 'pue' usually refers to the hardware in the vacuum chamber and 'bpm' to the beam position monitoring system, the two labels will be used casually here.) The exercise is carried out at two magnet rigidities, injection (AGS field ∼434 Gauss) and extraction to RHIC (∼9730 Gauss), - a ratio of rigidities of about 22.4. Since we stick with a bare machine, we are also stuck with the bare tunes which means the tunes are rather close together and near 8.75. Injection: (h,v) ∼ (8.73, 8.76).

  18. Pyrazine-functionalized calix[4]arenes: synthesis by palladium-catalyzed cross-coupling with phosphorus pronucleophiles and metal ion extraction properties

    NARCIS (Netherlands)

    Nikishkin, N.; Huskens, Jurriaan; Ansari, S.A.; Mohapatra, P.K.; Verboom, Willem

    2013-01-01

    A series of pyrazine-based calix[4]arene extractants was prepared by a stepwise functionalization, comprising palladium-catalyzed exhaustive cross-coupling of di- and tetrasubstituted calix[4]arenes bearing chloropyrazine moieties. The extraction behavior of the synthesized ligands was studied on

  19. Development of a simple extraction cell with bi-directional continuous flow coupled on-line to ICP-MS for assessment of elemental associations in solid samples

    DEFF Research Database (Denmark)

    Buanuam, Janya; Tiptanasup, Kasipa; Shiowatana, Juwadee

    2006-01-01

    A continuous-flow system comprising a novel, custom-built extraction module and hyphenated with inductively coupled plasma-mass spectrometric (ICP-MS) detection is proposed for assessing metal mobilities and geochemical associations in soil compartments as based on using the three step BCR (now...... the Measurements and Testing Programme of the European Commission) sequential extraction scheme. Employing a peristaltic pump as liquid driver, alternate directional flows of the extractants are used to overcome compression of the solid particles within the extraction unit to ensure a steady partitioning flow rate...... and thus to maintain constant operationally defined extraction conditions. The proposed flow set-up is proven to allow for trouble-free handling of soil samples up to 1 g and flow rates ≤ 10 mL min–1. The miniaturized extraction system was coupled to ICP-MS through a flow injection interface in order...

  20. Development of a portable, modular unit for the optimization of ultrasound-assisted oxidative desulfurization of diesel

    Science.gov (United States)

    Wan, Meng-Wei

    Due to the stringent rules requiring ultra-low sulfur content in diesel fuels, it is necessary to develop alternative methods of desulfurization of fossil fuel derived oil, such as diesel. Current technology is not sufficient to solve this problem. Ultrasound applied to oxidative desulfurization which combined three complementary techniques: ultrasonication, phase transfer catalysis (PTC) and transition metal catalyzed oxidation, has accomplished high sulfur removal in a short contact time at ambient temperature and atmospheric pressure. This research has successfully demonstrated that the higher oxidation efficiency of BT to BTO and free of any by-products by using tetraoctylammonium fluoride as phase transfer agent. The oxidation rate of BT to BTO increased with increasing the carbon chain length of QAS cations. Under the same length of carbon chain, the oxidation rate of BT to BTO increased with decreasing the molecular size of QAS anions. Moreover, for diesel fuels containing various levels of sulfur content, UAOD process followed by solvent extraction has demonstrated that the sulfur reduction can reach above 95 % removal efficiency or final sulfur content below 15 ppm in mild condition. For large-scale commercial production, this research has successfully developed and operated a continuous desulfurization unit, which consists of a sonoractor, an RF amplifier, a function generator, a pretreatment tank, and a pipeline system. A single unit only needed 2' x 4' x 1' space for installation. The results indicated that the remarkable 92% removal efficiency for the sulfur in marine logistic diesel, even at a treatment rate as high as 25 lb/hour which is approximately 2 barrels per day. Therefore, this sonoreactor demonstrated the feasibility of large-scale operation even in a relatively small installation with low capital investment and maintenance cost. It also ensures the safety considerations by operating with diluted hydrogen peroxide under ambient temperature

  1. Determination of Five Major 8-Prenylflavones in Leaves of Epimedium by Solid-Phase Extraction Coupled with Capillary Electrophoresis

    Science.gov (United States)

    Xie, Juan-ping; Xiang, Ji-ming; Zhu, Zhong-liang

    2016-01-01

    A simple, accurate and reproducible method which is based on the capillary electrophoresis, coupled with solid-phase extraction, has been developed for simultaneous determination of multiple 8-prenylflavones from Chinese Herba Epimedii. In this study, the author has mainly illustrated the experimental process and research results of five major components including epimedin C, icariin, diphylloside A, epimedoside A and icarisoside A that have been extracted and identified from Herba Epimedii for the first time. Experimental conditions have been optimized to achieve the best separation efficiency for the following factors: the buffer pH, buffer concentration and applied voltage. The experiment can be conducted through two separable stages: the first stage is to obtain the crude extracts through the solid-phase extraction; and the second stage is to further separate five major components by using the capillary electrophoresis. The separation of the five components and the analysis of the experiment are relatively fast and can be completed within 20 min. The concentration ranges of the construction of standard curves of five major 8-prenylflavones are 32.0–395.0, 23.4–292.0, 42.1–526.0, 18.8–233.5 and 29.7–371.0 µg mL−1 respectively, which have showed acceptable linearity with a correlation coefficient, r ≥ 0.999. The coefficient varies within 2.0% for both intra- and inter-days tests. The recoveries of five components range from 92.3 to 104.1%. The relative standard deviations of recoveries of five components range from 1.2 and 2.8%. This new method will facilitate the extraction and expedite the determination of medical components from Herba Epimedii. PMID:26865656

  2. Electromembrane extraction of heavy metal cations followed by capillary electrophoresis with capacitively coupled contactless conductivity detection

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Strieglerová, Lenka; Gebauer, Petr; Boček, Petr

    2011-01-01

    Roč. 32, č. 9 (2011), s. 1025-1032 ISSN 0173-0835 R&D Projects: GA ČR GA203/08/1536; GA ČR GAP206/10/1219; GA AV ČR IAA400310703 Institutional research plan: CEZ:AV0Z40310501 Keywords : capillary electrophoresis * electromembrane extraction * heavy metal cations Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.303, year: 2011

  3. Measurement of jet production with the ATLAS detector and extraction of the strong coupling constant

    CERN Document Server

    Marceca, Gino; The ATLAS collaboration

    2017-01-01

    The inclusive-jet cross-section at 8 TeV and the inclusive-jet and dijet cross-sections at 13 TeV with the ATLAS detector are presented. NLO QCD calculations, and NNLO for the inclusive-jet measurement at 13 TeV, are compared to the measurements. The extraction of $\\alpha_{s}$ from the measurement of the transverse energy-energy correlation at 8 TeV with the ATLAS detector is also presented.

  4. Oxidative Desulfurization of Gasoline by Ionic Liquids Coupled with Extraction by Organic Solvents

    OpenAIRE

    Abro, Rashid; Gao, Shurong; Chen, Xiaochun; Yu, Guangren; Abdeltawab, Ahmed A.; Al-Deyab, Salem S.

    2016-01-01

    In this work, desulfurization of real fluidized catalytic cracking (FCC) gasoline was investigated in dual steps; first in oxidative desulfurization (ODS) using imidazolium and pyrrolidonium based Brønsted acidic ionic liquids (ILs) as solvent and catalyst and hydrogen peroxide as oxidant. In second step, extractive desulfurization took place using organic solvents of furfural, furfural alcohol and ethylene glycol. Variety of factors such as temperature, time, mass ratio of oil/ILs and regene...

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

    Directory of Open Access Journals (Sweden)

    Kent E. Wardle

    2013-01-01

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

  6. [Ultrasound-assisted approach to blocking the intercostal nerves in the mid-axillary line for non-reconstructive breast and axilla surgery].

    Science.gov (United States)

    Diéguez García, P; Fajardo Pérez, M; López Álvarez, S; Alfaro de la Torre, P; Pensado Castiñeiras, A P

    2013-01-01

    Several nerve blocks have recently been used for pain treatment in breast surgery. The main objective of our study was to determine the efficacy and safety of ultrasound-assisted blocking of the anterior and lateral cutaneous branches of the intercostal nerves in the mid-axillary line for non-reconstructive breast and axilla surgery. A prospective observational study was conducted on 30 patients scheduled for non-reconstructive breast and axilla surgery. An intercostal branches block was performed in the mid-axillary line with 0,5% levobupivacaine (3ml in each intercostal space). Clinical efficacy was assessed by standard intraoperative hemodynamic response to surgical stimulus and the need for opioids, and in the postoperative period, by assessing pain intensity as a verbal numerical scale and the need for rescue treatment. We also evaluated the quality of sleep the first night after surgery, any adverse events that occurred, and the satisfaction of patients and surgeons with the anesthetic technique. The intercostal branches block in the mid-axillary line was effective in most cases, with only 2 patients requiring intraoperative opioids, and in one case analgesic rescue was necessary in the postoperative period. The duration of postoperative analgesia was 19±4h. There were no notable adverse events or complications. The satisfaction with the chosen technique was assessed as "very good" in all patients, and by 97% of the surgeons. Intercostal branches block in the mid-axillary line provides adequate intraoperative and postoperative analgesia for non-reconstructive breast and axilla surgery. It is a simple, reproducible technique in most patients of this study, with an easy to understand ultrasound anatomy, in which adequate analgesia could be provided through a single puncture, and may be an alternative to neuroaxial blocks. Copyright © 2013 Sociedad Española de Anestesiología, Reanimación y Terapéutica del Dolor. Published by Elsevier España. All rights

  7. A Retrospective Comparison of Ultrasound-Assisted Catheter-Directed Thrombolysis and Catheter-Directed Thrombolysis Alone for Treatment of Proximal Deep Vein Thrombosis

    Energy Technology Data Exchange (ETDEWEB)

    Tichelaar, Vladimir Y. I. G., E-mail: ynse.i.tichelaar@uit.no; Brodin, Ellen E.; Vik, Anders; Isaksen, Trond [UiT – The Arctic University of Norway, K. G. Jebsen – Thrombosis Research and Expertise Centre (TREC), Department of Clinical Medicine (Norway); Skjeldestad, Finn Egil [UiT – The Arctic University of Norway, Research Group Epidemiology of Chronic Diseases, Department of Community Medicine (Norway); Kumar, Satish; Trasti, Nora C.; Singh, Kulbir [University Hospital of North Norway, Department of Radiology (Norway); Hansen, John-Bjarne [UiT – The Arctic University of Norway, K. G. Jebsen – Thrombosis Research and Expertise Centre (TREC), Department of Clinical Medicine (Norway)

    2016-08-15

    BackgroundRecent studies have suggested that catheter-directed thrombolysis (CDT) reduces development of post-thrombotic syndrome (PTS). Ultrasound-assisted CDT (USCDT) might enhance the efficiency of thrombolysis. We aimed to compare USCDT with CDT on efficacy, safety, development of PTS, and quality of life after long-term follow-up.MethodsWe describe a retrospective case series of 94 consecutive patients admitted with iliofemoral or more proximal deep vein thrombosis (DVT) to the University Hospital from 2002 to 2011, treated either with CDT or USCDT. Scheduled follow-up visits took place between April 2013 and January 2014. Venography measured the degree of residual luminal obstruction of the affected veins. Each patient completed the Short Form 36-item health survey assessment and the Venous Insufficiency Epidemiological and Economic Study-Quality of Life/Symptoms questionnaires. PTS was assessed using the Villalta scale.ResultsRisk factors of DVT were equally distributed between groups. In the USCDT group, we observed a significant decline in the duration of thrombolytic treatment (<48 h: 27 vs. 10 %), shortened hospital stay (median 6.0 days (IQR 5.0–9.0) vs. 8.0 (IQR 5.8–12.0)), and less implantation of (intravenous) stents (30 vs. 55 %). There was no difference in patency (76 vs. 79 % fully patent), prevalence of PTS (52 vs. 55 %), or quality of life between groups after long-term follow-up (median 65 months, range: 15–141).ConclusionsIn this observational study, USCDT was associated with shortened treatment duration, shorter hospital stay, and less intravenous stenting, compared to CDT alone without affecting the long-term prevalence of PTS or quality of life.

  8. Ultrasound assisted two-stage biodiesel synthesis from non-edible Schleichera triguga oil using heterogeneous catalyst: Kinetics and thermodynamic analysis.

    Science.gov (United States)

    Sarve, Antaram N; Varma, Mahesh N; Sonawane, Shriram S

    2016-03-01

    Present work deals with the ultrasound-assisted biodiesel production from low cost, substantial acid value kusum (Schleichera triguga) oil using a two-step method of esterification in presence of acid (H2SO4) catalyst followed by transesterification using a basic heterogeneous barium hydroxide (Ba(OH)2) catalyst. The initial acid value of kusum oil was reduced from 21.65 to 0.84 mg of KOH/g of oil, by acid catalyzed esterification with 4:1 methanol to oil molar ratio, catalyst concentration 1% (v/v), ultrasonic irradiation time 20 min at 40 °C. Then, Ba(OH)2 concentration of 3% (w/w), methanol to oil molar ratio of 9:1, ultrasonic irradiation time of 80 min, and temperature of 50 °C was found to be the optimum conditions for transesterification step and triglyceride conversion of 96.8% (wt) was achieved. This paper also examined the kinetics as well as the evaluation of thermodynamic parameters for both esterification and transesterification reactions. The lower value of activation energy and higher values of kinetic constants indicated a fast rate of reaction, which could be attributed to the physical effect of emulsification, in which the microturbulence generated due to radial motion of bubbles, creates an intimate mixing of the immiscible reactants causing the increase in the interfacial area, giving faster reaction kinetics. The positive values of Gibbs-free energy (ΔG), enthalpy (ΔH) and negative value of entropy (ΔS) revealed that both the esterification and transesterification were non-spontaneous, endothermic and endergonic reactions. Therefore, the present work has not only established the escalation obtained due to ultrasonication but also exemplified the two-step approach for synthesis of biodiesel from non-edible kusum oil based on the use of heterogeneous catalyst for the transesterification step. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Ultrasonically assisted hydrothermal synthesis of activated carbon-HKUST-1-MOF hybrid for efficient simultaneous ultrasound-assisted removal of ternary organic dyes and antibacterial investigation: Taguchi optimization.

    Science.gov (United States)

    Azad, F Nasiri; Ghaedi, M; Dashtian, K; Hajati, S; Pezeshkpour, V

    2016-07-01

    Activated carbon (AC) composite with HKUST-1 metal organic framework (AC-HKUST-1 MOF) was prepared by ultrasonically assisted hydrothermal method and characterized by FTIR, SEM and XRD analysis and laterally was applied for the simultaneous ultrasound-assisted removal of crystal violet (CV), disulfine blue (DSB) and quinoline yellow (QY) dyes in their ternary solution. In addition, this material, was screened in vitro for their antibacterial actively against Methicillin-resistant Staphylococcus aureus (MRSA) and Pseudomonas aeruginosa (PAO1) bacteria. In dyes removal process, the effects of important variables such as initial concentration of dyes, adsorbent mass, pH and sonication time on adsorption process optimized by Taguchi approach. Optimum values of 4, 0.02 g, 4 min, 10 mg L(-1) were obtained for pH, AC-HKUST-1 MOF mass, sonication time and the concentration of each dye, respectively. At the optimized condition, the removal percentages of CV, DSB and QY were found to be 99.76%, 91.10%, and 90.75%, respectively, with desirability of 0.989. Kinetics of adsorption processes follow pseudo-second-order model. The Langmuir model as best method with high applicability for representation of experimental data, while maximum mono layer adsorption capacity for CV, DSB and QY on AC-HKUST-1 estimated to be 133.33, 129.87 and 65.37 mg g(-1) which significantly were higher than HKUST-1 as sole material with Qm to equate 59.45, 57.14 and 38.80 mg g(-1), respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Ultrasound-assisted synthesis of zinc molybdate nanocrystals and molybdate-doped epoxy/PDMS nanocomposite coatings for Mg alloy protection.

    Science.gov (United States)

    Eduok, Ubong; Szpunar, Jerzy

    2018-06-01

    Zinc molybdate (ZM) is a safer anticorrosive additive for cooling systems when compared with chromates and lead salts, due to its insolubility in aqueous media. For most molybdate pigments, their molybdate anion (MoO 4 -2 ) acts as an anionic inhibitor and its passivation capacity is comparable with chromate anion (CrO 4 -2 ). To alleviate the environmental concerns involving chromates-based industrial protective coatings, we have proposed new alternative in this work. We have synthesized ZM nanocrystals via ultrasound-assisted process and encapsulated them within an epoxy/PDMS coating towards corrosion protection. The surface morphology and mechanical properties of these ZM doped epoxy/PDMS nanocomposite coatings is exhaustively discussed to show the effect of ZM content on protective properties. The presence of ZM nanocrystals significantly contributed to the corrosion barrier performance of the coating while the amount of ZM nanocrystals needed to prepare an epoxy coating with optimum barrier performance was established. Beyond 2 wt% ZM concentration, the siloxane-structured epoxy coating network became saturated with ZM pigments. This further broadened inherent pores channels, leading to the percolation of corrosion chloride ions through the coating. SEM evidence has revealed proof of surface delamination on ZM3 coating. A model mechanism of corrosion resistance has been proposed for ZM doped epoxy/PDMS nanocomposite coatings from exhaustive surface morphological investigations and evidence. This coating matrix may have emerging applications in cooling systems as anticorrosive surface paints as well as create an avenue for environmental corrosion remediation. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. A Retrospective Comparison of Ultrasound-Assisted Catheter-Directed Thrombolysis and Catheter-Directed Thrombolysis Alone for Treatment of Proximal Deep Vein Thrombosis

    International Nuclear Information System (INIS)

    Tichelaar, Vladimir Y. I. G.; Brodin, Ellen E.; Vik, Anders; Isaksen, Trond; Skjeldestad, Finn Egil; Kumar, Satish; Trasti, Nora C.; Singh, Kulbir; Hansen, John-Bjarne

    2016-01-01

    BackgroundRecent studies have suggested that catheter-directed thrombolysis (CDT) reduces development of post-thrombotic syndrome (PTS). Ultrasound-assisted CDT (USCDT) might enhance the efficiency of thrombolysis. We aimed to compare USCDT with CDT on efficacy, safety, development of PTS, and quality of life after long-term follow-up.MethodsWe describe a retrospective case series of 94 consecutive patients admitted with iliofemoral or more proximal deep vein thrombosis (DVT) to the University Hospital from 2002 to 2011, treated either with CDT or USCDT. Scheduled follow-up visits took place between April 2013 and January 2014. Venography measured the degree of residual luminal obstruction of the affected veins. Each patient completed the Short Form 36-item health survey assessment and the Venous Insufficiency Epidemiological and Economic Study-Quality of Life/Symptoms questionnaires. PTS was assessed using the Villalta scale.ResultsRisk factors of DVT were equally distributed between groups. In the USCDT group, we observed a significant decline in the duration of thrombolytic treatment (<48 h: 27 vs. 10 %), shortened hospital stay (median 6.0 days (IQR 5.0–9.0) vs. 8.0 (IQR 5.8–12.0)), and less implantation of (intravenous) stents (30 vs. 55 %). There was no difference in patency (76 vs. 79 % fully patent), prevalence of PTS (52 vs. 55 %), or quality of life between groups after long-term follow-up (median 65 months, range: 15–141).ConclusionsIn this observational study, USCDT was associated with shortened treatment duration, shorter hospital stay, and less intravenous stenting, compared to CDT alone without affecting the long-term prevalence of PTS or quality of life.

  12. 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.

  13. Quality assessment of trace Cd and Pb contaminants in Thai herbal medicines using ultrasound-assisted digestion prior to flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Watsaka Siriangkhawut

    2017-10-01

    Full Text Available A simple, efficient, and reliable ultrasound-assisted digestion (UAD procedure was used for sample preparation prior to quantitative determination of trace Cd and Pb contaminants in herbal medicines using flame atomic absorption spectrometry. The parameters influencing UAD such as the solvent system, sample mass, presonication time, sonication time, and digestion temperature were evaluated. The efficiency of the proposed UAD procedure was evaluated by comparing with conventional acid digestion (CAD procedure. Under the optimum conditions, linear calibration graphs in a range of 2–250 μg/L for Cd, and 50–1000 μg/L for Pb were obtained with detection limits of 0.56 μg/L and 10.7 μg/L for Cd and Pb, respectively. The limit of quantification for Cd and Pb were 1.87 μg/L and 40.3 μg/L, respectively. The repeatability for analysis of 10 μg/L for Cd and 100 μg/L for Pb was 2.3% and 2.6%, respectively. The accuracy of the proposed method was evaluated by rice flour certified reference materials. The proposed method was successfully applied for analysis of trace Cd and Pb in samples of various types of medicinal plant and traditional medicine consumed in Thailand. Most herbal medicine samples were not contaminated with Cd or Pb. The contaminant levels for both metals were still lower than the maximum permissible levels of elements in medicinal plant materials and finished herbal products sets by the Ministry of Public Health of Thailand. The exception was the high level of Cd contamination found in two samples of processed medicinal plants.

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

    Science.gov (United States)

    Xia, Qinghai; Yang, Yaling; Liu, Mousheng

    2012-10-01

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

  15. Determination of chlorinated polycyclic aromatic hydrocarbons in water by solid-phase extraction coupled with gas chromatography and mass spectrometry.

    Science.gov (United States)

    Wang, Xianli; Kang, Haiyan; Wu, Junfeng

    2016-05-01

    Given the potential risks of chlorinated polycyclic aromatic hydrocarbons, the analysis of their presence in water is very urgent. We have developed a novel procedure for determining chlorinated polycyclic aromatic hydrocarbons in water based on solid-phase extraction coupled with gas chromatography and mass spectrometry. The extraction parameters of solid-phase extraction were optimized in detail. Under the optimal conditions, the proposed method showed wide linear ranges (1.0-1000 ng/L) with correlation coefficients ranging from 0.9952 to 0.9998. The limits of detection and the limits of quantification were in the range of 0.015-0.591 and 0.045-1.502 ng/L, respectively. Recoveries ranged from 82.5 to 102.6% with relative standard deviations below 9.2%. The obtained method was applied successfully to the determination of chlorinated polycyclic aromatic hydrocarbons in real water samples. Most of the chlorinated polycyclic aromatic hydrocarbons were detected and 1-monochloropyrene was predominant in the studied water samples. This is the first report of chlorinated polycyclic aromatic hydrocarbons in water samples in China. The toxic equivalency quotients of chlorinated polycyclic aromatic hydrocarbons in the studied tap water were 9.95 ng the toxic equivalency quotient m(-3) . 9,10-Dichloroanthracene and 1-monochloropyrene accounted for the majority of the total toxic equivalency quotients of chlorinated polycyclic aromatic hydrocarbons in tap water. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Comparison of inductively coupled plasma mass spectrometry and colorimetric determination of total and extractable phosphorus in soils

    International Nuclear Information System (INIS)

    Ivanov, Krasimir; Zaprjanova, Penka; Petkova, Milena; Stefanova, Violeta; Kmetov, Veselin; Georgieva, Deyana; Angelova, Violina

    2012-01-01

    The most widely used method for determination of total phosphorus in soils is perchloric acid digestion, followed by a colorimetric assay to measure the concentration of P in solution. The first part of this study compares an alternative digestion method, using aqua regia (ISO 11466 and EPA Method 3052), with perchloric acid digestion procedure, and also compares inductively coupled plasma mass spectroscopy (ICP-MS) with colorimetry for the measurement of P on the basis of five internationally certified standard soils and 20 real-life soils with widely different extractability of phosphorus. The phosphorus concentration was determined by means of the reduced phosphomolybdenum blue and ICP-MS. The relationship between methods has been examined statistically. Good agreement of the results from colorimetry and ICP-MS was established for all certified soils. The microwave-assisted digestion with aqua regia was comparable, both in precision and accuracy, with the hot plate aqua regia method. The phosphorus concentration found with the HF + HClO 4 digestion method was in good agreement with the certified mean values, while the superiority in extracting phosphorus, when compared to other methods, was obvious. Soil testing for plant-available phosphorus in Bulgaria and many European countries is most commonly conducted using acid Ca-lactate extraction (Egner–Riehm test) and alkaline sodium bicarbonate extraction (BDS ISO 11263:2002), based on Olsen test, followed by a colorimetric assay to measure the concentration of P in solution. The second part of this study reports the differences between Egner–Riehm test and BDS ISO 11263:2002 measured colorimetrically and by ICP-MS. Fifty soils were selected from South Bulgaria to represent a wide range of soil properties. It was established that ICP-MS consistently yielded significantly higher P concentrations than the colorimetric method in both extraction tests, and the relative differences were greatest in soils with lower P

  17. Comparison of inductively coupled plasma mass spectrometry and colorimetric determination of total and extractable phosphorus in soils

    Energy Technology Data Exchange (ETDEWEB)

    Ivanov, Krasimir, E-mail: kivanov1@abv.bg [Department of Chemistry, University of Agriculture, Plovdiv (Bulgaria); Zaprjanova, Penka [Tobacco and Tobacco Products Institute, Plovdiv (Bulgaria); Petkova, Milena [Department of Chemistry, University of Agriculture, Plovdiv (Bulgaria); Stefanova, Violeta; Kmetov, Veselin; Georgieva, Deyana [Department of Analytical Chemistry, Plovdiv University ' Paisii Hilendarski,' Plovdiv (Bulgaria); Angelova, Violina [Department of Chemistry, University of Agriculture, Plovdiv (Bulgaria)

    2012-05-15

    The most widely used method for determination of total phosphorus in soils is perchloric acid digestion, followed by a colorimetric assay to measure the concentration of P in solution. The first part of this study compares an alternative digestion method, using aqua regia (ISO 11466 and EPA Method 3052), with perchloric acid digestion procedure, and also compares inductively coupled plasma mass spectroscopy (ICP-MS) with colorimetry for the measurement of P on the basis of five internationally certified standard soils and 20 real-life soils with widely different extractability of phosphorus. The phosphorus concentration was determined by means of the reduced phosphomolybdenum blue and ICP-MS. The relationship between methods has been examined statistically. Good agreement of the results from colorimetry and ICP-MS was established for all certified soils. The microwave-assisted digestion with aqua regia was comparable, both in precision and accuracy, with the hot plate aqua regia method. The phosphorus concentration found with the HF + HClO{sub 4} digestion method was in good agreement with the certified mean values, while the superiority in extracting phosphorus, when compared to other methods, was obvious. Soil testing for plant-available phosphorus in Bulgaria and many European countries is most commonly conducted using acid Ca-lactate extraction (Egner-Riehm test) and alkaline sodium bicarbonate extraction (BDS ISO 11263:2002), based on Olsen test, followed by a colorimetric assay to measure the concentration of P in solution. The second part of this study reports the differences between Egner-Riehm test and BDS ISO 11263:2002 measured colorimetrically and by ICP-MS. Fifty soils were selected from South Bulgaria to represent a wide range of soil properties. It was established that ICP-MS consistently yielded significantly higher P concentrations than the colorimetric method in both extraction tests, and the relative differences were greatest in soils with lower

  18. Extraction and analysis of silver and gold nanoparticles from biological tissues using single particle inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Gray, Evan P; Coleman, Jessica G; Bednar, Anthony J; Kennedy, Alan J; Ranville, James F; Higgins, Christopher P

    2013-12-17

    Expanded use of engineered nanoparticles (ENPs) in consumer products increases the potential for environmental release and unintended biological exposures. As a result, measurement techniques are needed to accurately quantify ENP size, mass, and particle number distributions in biological matrices. This work combines single particle inductively coupled plasma mass spectrometry (spICPMS) with tissue extraction to quantify and characterize metallic ENPs in environmentally relevant biological tissues for the first time. ENPs were extracted from tissues via alkaline digestion using tetramethylammonium hydroxide (TMAH). Method development was performed using ground beef and was verified in Daphnia magna and Lumbriculus variegatus . ENPs investigated include 100 and 60 nm Au and Ag stabilized by polyvynylpyrrolidone (PVP). Mass- and number-based recovery of spiked Au and Ag ENPs was high (83-121%) from all tissues tested. Additional experiments suggested ENP mixtures (60 and 100 nm Ag ENPs) could be extracted and quantitatively analyzed. Biological exposures were also conducted to verify the applicability of the method for aquatic organisms. Size distributions and particle number concentrations were determined for ENPs extracted from D. magna exposed to 98 μg/L 100 nm Au and 4.8 μg/L 100 nm Ag ENPs. The D. magna nanoparticulate body burden for Au ENP uptake was 613 ± 230 μg/kgww, while the measured nanoparticulate body burden for D. magna exposed to Ag ENPs was 59 ± 52 μg/kgww. Notably, the particle size distributions determined from D. magna tissues suggested minimal shifts in the size distributions of ENPs accumulated, as compared to the exposure media.

  19. Microwave assisted extraction of iodine and bromine from edible seaweed for inductively coupled plasma-mass spectrometry determination.

    Science.gov (United States)

    Romarís-Hortas, Vanessa; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Pilar

    2009-08-15

    The feasibility of microwave energy to assist the solubilisation of edible seaweed samples by tetramethylammonium hydroxide (TMAH) has been investigated to extract iodine and bromine. Inductively coupled plasma-mass spectrometry (ICP-MS) has been used as a multi-element detector. Variables affecting the microwave assisted extraction/solubilisation (temperature, TMAH volume, ramp time and hold time) were firstly screened by applying a fractional factorial design (2(5-1)+2), resolution V and 2 centre points. When extracting both halogens, results showed statistical significance (confidence interval of 95%) for TMAH volume and temperature, and also for the two order interaction between both variables. Therefore, these two variables were finally optimized by a 2(2)+star orthogonal central composite design with 5 centre points and 2 replicates, and optimum values of 200 degrees C and 10 mL for temperature and TMAH volume, respectively, were found. The extraction time (ramp and hold times) was found statistically non-significant, and values of 10 and 5 min were chosen for the ramp time and the hold time, respectively. This means a fast microwave heating cycle. Repeatability of the over-all procedure has been found to be 6% for both elements, while iodine and bromine concentrations of 24.6 and 19.9 ng g(-1), respectively, were established for the limit of detection. Accuracy of the method was assessed by analyzing the NIES-09 (Sargasso, Sargassum fulvellum) certified reference material (CRM) and the iodine and bromine concentrations found have been in good agreement with the indicative values for this CRM. Finally, the method was applied to several edible dried and canned seaweed samples.

  20. Multivariate analysis of the volatile components in tobacco based on infrared-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Yanqin; Pan, Yuanjiang; Zhou, Guojun; Chu, Guohai; Jiang, Jian; Yuan, Kailong; Xia, Qian; Cheng, Changhe

    2016-11-01

    A novel infrared-assisted extraction coupled to headspace solid-phase microextraction followed by gas chromatography with mass spectrometry method has been developed for the rapid determination of the volatile components in tobacco. The optimal extraction conditions for maximizing the extraction efficiency were as follows: 65 μm polydimethylsiloxane-divinylbenzene fiber, extraction time of 20 min, infrared power of 175 W, and distance between the infrared lamp and the headspace vial of 2 cm. Under the optimum conditions, 50 components were found to exist in all ten tobacco samples from different geographical origins. Compared with conventional water-bath heating and nonheating extraction methods, the extraction efficiency of infrared-assisted extraction was greatly improved. Furthermore, multivariate analysis including principal component analysis, hierarchical cluster analysis, and similarity analysis were performed to evaluate the chemical information of these samples and divided them into three classifications, including rich, moderate, and fresh flavors. The above-mentioned classification results were consistent with the sensory evaluation, which was pivotal and meaningful for tobacco discrimination. As a simple, fast, cost-effective, and highly efficient method, the infrared-assisted extraction coupled to headspace solid-phase microextraction technique is powerful and promising for distinguishing the geographical origins of the tobacco samples coupled to suitable chemometrics. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Alternative and Efficient Extraction Methods for Marine-Derived Compounds

    Directory of Open Access Journals (Sweden)

    Clara Grosso

    2015-05-01

    Full Text Available Marine ecosystems cover more than 70% of the globe’s surface. These habitats are occupied by a great diversity of marine organisms that produce highly structural diverse metabolites as a defense mechanism. In the last decades, these metabolites have been extracted and isolated in order to test them in different bioassays and assess their potential to fight human diseases. Since traditional extraction techniques are both solvent- and time-consuming, this review emphasizes alternative extraction techniques, such as supercritical fluid extraction, pressurized solvent extraction, microwave-assisted extraction, ultrasound-assisted extraction, pulsed electric field-assisted extraction, enzyme-assisted extraction, and extraction with switchable solvents and ionic liquids, applied in the search for marine compounds. Only studies published in the 21st century are considered.

  2. Extraction Methods for the Isolation of Isoflavonoids from Plant Material

    Directory of Open Access Journals (Sweden)

    Blicharski Tomasz

    2017-03-01

    Full Text Available The purpose of this review is to describe and compare selected traditional and modern extraction methods employed in the isolation of isoflavonoids from plants. Conventional methods such as maceration, percolation, or Soxhlet extraction are still frequently used in phytochemical analysis. Despite their flexibility, traditional extraction techniques have significant drawbacks, including the need for a significant investment of time, energy, and starting material, and a requirement for large amounts of potentially toxic solvents. Moreover, these techniques are difficult to automate, produce considerable amount of waste and pose a risk of degradation of thermolabile compounds. Modern extraction methods, such as: ultrasound-assisted extraction, microwave-assisted extraction, accelerated solvent extraction, supercritical fluid extraction, and negative pressure cavitation extraction, can be regarded as remedies for the aforementioned problems. This manuscript discusses the use of the most relevant extraction techniques in the process of isolation of isoflavonoids, secondary metabolites that have been found to have a plethora of biological and pharmacological activities.

  3. EXTRACT

    DEFF Research Database (Denmark)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra

    2016-01-01

    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have the...... and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed.Database URL: https://extract.hcmr.gr/......., organism, tissue and disease terms. The evaluators in the BioCreative V Interactive Annotation Task found the system to be intuitive, useful, well documented and sufficiently accurate to be helpful in spotting relevant text passages and extracting organism and environment terms. Comparison of fully manual...

  4. Extraction of butyltins from sediments and their determination by liquid chromatography interfaced to inductively coupled plasma atomic emission detector

    International Nuclear Information System (INIS)

    Rivaro, P.; Frache, R.

    2000-01-01

    A liquid-liquid extraction of the butyltin compounds from sediment, suitable for their subsequent following determination by high performance liquid chromatography-hydride generation inductively coupled plasma atomic emission detector system, is proposed. Recoveries of 86%, 80% and 42% for tributyltin (TBT), dibutyltin (DBT) and monobutyltin (MBT) respectively were achieved. The relative detection limits of butyltin compounds by this method ranged from 27 to 62 ng of tin per gram of dry sediment. The method was applied to real sediment samples collected in the Venice lagoon (Italy). The results showed that, despite the restrictions on the use of butyltin contained in antifoulting paints, a considerable amount of organotin compounds is still present in Venice sediments [it

  5. Determination of chiral pharmaceuticals and illicit drugs in wastewater and sludge using microwave assisted extraction, solid-phase extraction and chiral liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Evans, Sian E; Davies, Paul; Lubben, Anneke; Kasprzyk-Hordern, Barbara

    2015-07-02

    This is the first study presenting a multi-residue method allowing for comprehensive analysis of several chiral pharmacologically active compounds (cPACs) including beta-blockers, antidepressants and amphetamines in wastewater and digested sludge at the enantiomeric level. Analysis of both the liquid and solid matrices within wastewater treatment is crucial to being able to carry out mass balance within these systems. The method developed comprises filtration, microwave assisted extraction and solid phase extraction followed by chiral liquid chromatography coupled with tandem mass spectrometry to analyse the enantiomers of 18 compounds within all three matrices. The method was successfully validated for 10 compounds within all three matrices (amphetamine, methamphetamine, MDMA, MDA, venlafaxine, desmethylvenlafaxine, citalopram, metoprolol, propranolol and sotalol), 7 compounds validated for the liquid matrices only (mirtazapine, salbutamol, fluoxetine, desmethylcitalopram, atenolol, ephedrine and pseudoephedrine) and 1 compound (alprenolol) passing the criteria for solid samples only. The method was then applied to wastewater samples; cPACs were found at concentration ranges in liquid matrices of: 1.7 ng L(-1) (metoprolol) - 1321 ng L(-1) (tramadol) in influent,

  6. 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.

  7. 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.

  8. Examples of coupled human and environmental systems from the extractive industry and hydropower sector interfaces.

    Science.gov (United States)

    Castro, Marcia C; Krieger, Gary R; Balge, Marci Z; Tanner, Marcel; Utzinger, Jürg; Whittaker, Maxine; Singer, Burton H

    2016-12-20

    Large-scale corporate projects, particularly those in extractive industries or hydropower development, have a history from early in the twentieth century of creating negative environmental, social, and health impacts on communities proximal to their operations. In many instances, especially for hydropower projects, the forced resettlement of entire communities was a feature in which local cultures and core human rights were severely impacted. These projects triggered an activist opposition that progressively expanded and became influential at both the host community level and with multilateral financial institutions. In parallel to, and spurred by, this activism, a shift occurred in 1969 with the passage of the National Environmental Policy Act in the United States, which required Environmental Impact Assessment (EIA) for certain types of industrial and infrastructure projects. Over the last four decades, there has been a global movement to develop a formal legal/regulatory EIA process for large industrial and infrastructure projects. In addition, social, health, and human rights impact assessments, with associated mitigation plans, were sequentially initiated and have increasingly influenced project design and relations among companies, host governments, and locally impacted communities. Often, beneficial community-level social, economic, and health programs have voluntarily been put in place by companies. These flagship programs can serve as benchmarks for community-corporate-government partnerships in the future. Here, we present examples of such positive phenomena and also focus attention on a myriad of challenges that still lie ahead.

  9. PDF constraints and extraction of the strong coupling constant from the inclusive jet cross section at 7 TeV

    CERN Document Server

    CMS Collaboration

    2013-01-01

    The recent CMS measurement of the inclusive jet cross section at 7~TeV extends the accessible phase space in jet transverse momentum up to 2 TeV and ranges up to 2.5 in absolute jet rapidity. At the same time the experimental uncertainties are smaller than in previous publications such that these data constrain the parton distribution functions of the proton, notably for the gluon at high fractions of the proton momentum, and provide valuable input to determine the strong coupling at high momentum scales. The impact on the extraction of the parton distribution functions is investigated. Using predictions from theory at next-to-leading order, complemented with electroweak corrections, the strong coupling constant is determined from the inclusive jet cross section to be $\\alpha_S(M_Z) = 0.1185 \\pm 0.0019\\,\\mathrm{(exp.)} \\pm 0.0028\\,\\mathrm{(\\mathrm{PDF})} \\pm 0.0004\\,\\mathrm{(\\mathrm{NP})} ^{+0.0055}_{-0.0022}\\,\\mathrm{(\\mathrm{scale})}$, which is in agreement with the world average.

  10. Ultrasound-assisted green economic synthesis of hydroxyapatite nanoparticles using eggshell biowaste and study of mechanical and biological properties for orthopedic applications.

    Science.gov (United States)

    Ingole, Vijay H; Hany Hussein, Kamal; Kashale, Anil A; Ghule, Kalyani; Vuherer, Tomaž; Kokol, Vanja; Chang, Jia-Yaw; Ling, Yong-Chien; Vinchurkar, Aruna; Dhakal, Hom N; Ghule, Anil V

    2017-11-01

    Nanostructured hydroxyapatite (HAp) is the most favorable candidate biomaterial for bone tissue engineering because of its bioactive and osteoconductive properties. Herein, we report for the first time ultrasound-assisted facile and economic approach for the synthesis of nanocrystalline hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 ) using recycled eggshell biowaste referred as EHAp. The process involves the reaction of eggshell biowaste as a source of calcium and ammonium dihydrogen orthophosphate as a phosphate source. Ultrasound-mediated chemical synthesis of hydroxyapatite (HAp) is also carried out using similar approach wherein commercially available calcium hydroxide and ammonium dihydrogen orthophosphate were used as calcium and phosphate precursors, respectively and referred as CHAp for better comparison. The prepared materials were characterized by X-ray diffraction, field emission scanning electron microscopy, Fourier transform infrared spectroscopy, and Raman spectroscopy to determine crystal structure, particle morphology, and the presence of chemical functional groups. The nanocrystalline EHAp and CHAp were observed to have spherical morphology with uniform size distribution. Furthermore, mechanical properties such as Vickers hardness, fracture toughness, and compression tests have been studied of the EHAp and CHAp samples showing promising results. Mechanical properties show the influence of calcination at 600°C EHAp and CHAp material. After calcination, in the case of EHAp material an average hardness, mechanical strength, elastic modulus, and fracture toughness were found 552 MPa, 46.6 MPa, 2824 MPa, and 3.85 MPa m 1/2 , respectively, while in the case of CHAp 618 MPa, 47.5 MPa, 2071 MPa, and 3.13 MPa m 1/2 . In vitro cell studies revealed that the EHAp and CHAp nanoparticles significantly increased the attachment and proliferation of the hFOB cells. Here, we showed that EHAp and CHAp provide promising biocompatible materials that do not affect the cell

  11. [Determination of short chain chlorinated paraffins in leather products by solid phase extraction coupled with gas chromatography-mass spectrometry].

    Science.gov (United States)

    Zhang, Weiya; Wan, Xin; Li, Lixia; Wang, Chengyun; Jin, Shupei; Xing, Jun

    2014-10-01

    The short chain chlorinated paraffins (SCCPs) are the additives frequently used in the leather production in China, but they have been put into the list of forbidden chemicals issued by European Union recently. In fact, there is not a commonly recognized method for the determination of the SCCPs in the leather products due to the serious matrix interferences from the leather products and the complex chemical structures of the SCCPs. A method of solid phase extraction coupled with gas chromatography-mass spectrometry (SPE-GC-MS) was established for the determination of the SCCPs in the leather products after the optimization of the SPE conditions. It was found that the interferences from the leather products were thor- oughly separated from the analyte of the SCCPs on a home-made solid phase extraction (SPE) column filled with silica packing while eluted with a mixed solvent of n-hexane-methylene chloride (2:1, v/v). With this method, the recoveries for the SCCPs spiked in the real leather samples varied from 90.47% to 99.00% with the relative standard deviations (RSDs) less than 6.7%, and the limits of detection (LODs) were between 0.069 and 0.110 mg/kg. This method is suitable for qualitative and quantitative analysis of SCCPs in the leather products.

  12. Determination of semicarbazide in fish by molecularly imprinted stir bar sorptive extraction coupled with high performance liquid chromatography.

    Science.gov (United States)

    Tang, Tang; Wei, Fangdi; Wang, Xu; Ma, Yujie; Song, Yueyue; Ma, Yunsu; Song, Quan; Xu, Guanhong; Cen, Yao; Hu, Qin

    2018-02-15

    A novel molecularly imprinted stir bar (MI-SB) for sorptive extraction of semicarbazide (SEM) was prepared in present paper. The coating of the stir bar was characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, dynamic adsorption and static adsorption tests. The saturated adsorption of MI-SB was about 4 times over that of non-imprinted stir bar (NI-SB). The selectivity of MI-SB for SEM was much better than NI-SB. A method to determine SEM was established by coupling MI-SB sorptive extraction with HPLC-UV. The liner range was 1-100ng/mL for SEM with a correlation coefficient of 0.9985. The limit of detection was about 0.59ng/mL, which was below the minimum required performance limit of SEM in meat products regulated by European Union. The method was applied to the determination of SEM in fish samples with satisfactory results. Copyright © 2018 Elsevier B.V. All rights reserved.

  13. Fundamental studies of the plasma extraction and ion beam formation processes in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Niu, Hongsen.

    1995-01-01

    The fundamental and practical aspects are described for extracting ions from atmospheric pressure plasma sources into an analytical mass spectrometer. Methodologies and basic concepts of inductively coupled plasma mass spectrometry (ICP-MS) are emphasized in the discussion, including ion source, sampling interface, supersonic expansion, slumming process, ion optics and beam focusing, and vacuum considerations. Some new developments and innovative designs are introduced. The plasma extraction process in ICP-MS was investigated by Langmuir measurements in the region between the skimmer and first ion lens. Electron temperature (T e ) is in the range 2000--11000 K and changes with probe position inside an aerosol gas flow. Electron density (n e ) is in the range 10 8 --10 10 -cm at the skimmer tip and drops abruptly to 10 6 --10 8 cm -3 near the skimmer tip and drops abruptly to 10 6 --10 8 cm -3 downstream further behind the skimmer. Electron density in the beam leaving the skimmer also depends on water loading and on the presence and mass of matrix elements. Axially resolved distributions of electron number-density and electron temperature were obtained to characterize the ion beam at a variety of plasma operating conditions. The electron density dropped by a factor of 101 along the centerline between the sampler and skimmer cones in the first stage and continued to drop by factors of 10 4 --10 5 downstream of skimmer to the entrance of ion lens. The electron density in the beam expansion behind sampler cone exhibited a 1/z 2 intensity fall-off (z is the axial position). An second beam expansion originated from the skimmer entrance, and the beam flow underwent with another 1/z 2 fall-off behind the skimmer. Skimmer interactions play an important role in plasma extraction in the ICP-MS instrument

  14. Bead Injection Extraction Chromatography using High-capacity Lab-on-Valve as a Front End to Inductively Coupled Plasma Mass Spectrometry for Rapid Urine Radiobioassay

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2013-01-01

    A novel bead injection (BI) extraction chromatographic microflow system exploiting high-capacity lab-on-valve (LOV) platform coupled with inductively coupled plasma mass spectrometric detection is developed for rapid and automated determination of plutonium in human urine. A microconduit (1 m......L) incorporated within the LOV processing unit is loaded on-line with a metered amount of disposable extraction chromatographic resin (up to 330 mg of TEVA) through programmable beads transport. Selective capture and purification of plutonium onto the resin beads is then performed by pressure driven flow after...

  15. Determination of mercury species in biological samples by inductively coupled plasma mass spectrometry combined with solvent extraction and ultrasonication

    International Nuclear Information System (INIS)

    Sun, J.; Li, Y.F.; Wang, J.X.; Chen, C.Y.; Li, B.; Gao, Y.X.; Chai, Z.F.

    2005-01-01

    Mercury (Hg) is a well-known toxic element. The toxic effects of Hg depend on its chemical forms. The most important chemical forms are elemental Hg (Hg 0 ), inorganic Hg (Hg 2+ ) and methylmercury (CH 3 Hg + ). In the biogeochemical cycle of Hg, these species may interchange in atmospheric, aquatic and terrestrial environments. Among them, methylmercury is considerably higher toxic than elemental mercury and inorganic mercury because it is recognized as one of major health hazards for human due to its teratogenic, immunotoxic, and neurotoxic effects. Therefore, determinations of not only total mercury, but also methylmercury content in biological samples is necessary. In large numbers of analytical methods, inductively coupled plasma mass spectrometry (ICP-MS) using conventional sample introduction with a peristaltic pump is widely used for the determination of trace metals in a wide variety of different sample matrices. ICP-MS can offer high sensitivity, low detection limit, reasonable accuracy and precision, and can easily be automated. However, mercury is considered as an element with analytical problems. One problem is well known in Hg analysis that the memory effect increases the blank counts and worsens the analytical performance of ICP-MS. The possibility of Hg losses during sample decomposition procedure due to its volatility is another important issue. Additionally, its high first ionization potential and numerous isotopes have limited its sensitivity in ICP-MS analysis. In order to solve the above questions, the present work was carried out to develop a method based on ICP-MS coupled with solvent extraction for determination of mercury species in biological samples. At first step, we investigated different solvent extraction methods including acid leaching, CuSO 4 extraction, alkaline-methanol extraction, and surfactant extraction with ultrasonication for methylmercury determination using the certified reference materials GBW07601 (Human Hair). Next, we

  16. Development of a magnetic solid-phase extraction coupled with high-performance liquid chromatography method for the analysis of polyaromatic hydrocarbons.

    Science.gov (United States)

    Ma, Yan; Xie, Jiawen; Jin, Jing; Wang, Wei; Yao, Zhijian; Zhou, Qing; Li, Aimin; Liang, Ying

    2015-07-01

    A novel magnetic solid phase extraction coupled with high-performance liquid chromatography method was established to analyze polyaromatic hydrocarbons in environmental water samples. The extraction conditions, including the amount of extraction agent, extraction time, pH and the surface structure of the magnetic extraction agent, were optimized. The results showed that the amount of extraction agent and extraction time significantly influenced the extraction performance. The increase in the specific surface area, the enlargement of pore size, and the reduction of particle size could enhance the extraction performance of the magnetic microsphere. The optimized magnetic extraction agent possessed a high surface area of 1311 m(2) /g, a large pore size of 6-9 nm, and a small particle size of 6-9 μm. The limit of detection for phenanthrene and benzo[g,h,i]perylene in the developed analysis method was 3.2 and 10.5 ng/L, respectively. When applied to river water samples, the spiked recovery of phenanthrene and benzo[g,h,i]perylene ranged from 89.5-98.6% and 82.9-89.1%, respectively. Phenanthrene was detected over a concentration range of 89-117 ng/L in three water samples withdrawn from the midstream of the Huai River, and benzo[g,h,i]perylene was below the detection limit. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

    2016-03-01

    An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Development and characterization of a small electromembrane extraction probe coupled with mass spectrometry for real-time and online monitoring of in vitro drug metabolism

    DEFF Research Database (Denmark)

    Dugstad, Helene Bonkerud; Petersen, Nickolaj J.; Jensen, Henrik

    2014-01-01

    A small and very simple electromembrane extraction probe (EME-probe) was developed and coupled directly to electrospray ionization mass spectrometry (ESI-MS), and this system was used to monitor in real time in vitro metabolism by rat liver microsomes of drug substances from a small reaction...... (soft extraction). Soft extraction was mandatory in order not to affect the reaction kinetics by sample composition changes induced by the EME-probe. The EME-probe/MS-system was used to establish kinetic profiles for the in vitro metabolism of promethazine, amitriptyline and imipramine as model...

  19. Future Oil Spills and Possibilities for Intervention: A Model for the Coupled Human-Environmental Resource Extraction System

    Science.gov (United States)

    Shughrue, C. M.; Werner, B.; Nugnug, P. T.

    2010-12-01

    The catastrophic Deepwater Horizon oil spill highlights the risks for widespread environmental damage resulting from petroleum resource extraction. Possibilities for amelioration of these risks depend critically on understanding the dynamics and nonlinear interactions between various components of the coupled human-environmental resource extraction system. We use a complexity analysis to identify the levels of description and time scales at which these interactions are strongest, and then use the analysis as the basis for an agent-based numerical model with which decadal trends can be analyzed. Oil industry economic and technological activity and associated oil spills are components of a complex system that is coupled to natural environment, legislation, regulation, media, and resistance systems over annual to decadal time scales. In the model, oil spills are produced stochastically with a range of magnitudes depending on a reliability-engineering-based assessment of failure for the technology employed, human factors including compliance with operating procedures, and risks associated with the drilling environment. Oil industry agents determine drilling location and technological investment using a cost-benefit analysis relating projected revenue from added production to technology cost and government regulation. Media outlet agents reporting on the oil industry and environmental damage from oil spills assess the impacts of aggressively covering a story on circulation increases, advertiser concerns and potential loss of information sources. Environmental advocacy group agents increase public awareness of environmental damage (through media and public contact), solicit memberships and donations, and apply direct pressure on legislators for policy change. Heterogeneous general public agents adjust their desire for change in the level of regulation, contact their representatives or participate in resistance via protest by considering media sources, personal

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

    Science.gov (United States)

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

  1. Speciation Analysis of Trace Mercury in Sea Cucumber Species of Apostichopus japonicus Using High-Performance Liquid Chromatography Conjunction With Inductively Coupled Plasma Mass Spectrometry.

    Science.gov (United States)

    Liu, Hao; Luo, Jiaoyang; Ding, Tong; Gu, Shanyong; Yang, Shihai; Yang, Meihua

    2018-03-25

    In this paper, a simple and cost-effective method using high-performance liquid chromatography in conjunction with inductively coupled plasma mass spectrometry with a rapid ultrasound-assisted extraction was used for analysis speciation of trace mercury in sea cucumber species of Apostichopus japonicus. The effective separation of inorganic mercury, methylmercury, and ethylmercury was achieved within 10 min using Agilent ZORBAX SB-C 18 analytical and guard columns with an isocratic mobile phase consisting of 8% methanol and 92% H 2 O containing 0.12% L-cysteine (m/v) and 0.01 mol/L ammonium acetate. Mercury species were extracted from A. japonicus samples using a solution containing 2-mercaptoethanol, L-cysteine, and hydrochloric acid and sonicating for 0.5 h. The limits of detection of inorganic mercury, methylmercury, and ethylmercury were 0.12, 0.08, and 0.20 μg/L, and the minimum detectable concentrations (measured at 0.500 g sample volume in 10.00 mL) were 2.4, 1.6, and 4.0 μg/kg, respectively. Analysis of a scallop certified reference material (GBW 10024) revealed accordance between the experimental and certified values. This study provides a reference for the evaluation of mercury speciation in sea cucumber and other seafood.

  2. Simultaneous determination of 9 heterocyclic aromatic amines in pork products by liquid chromatography coupled with triple quadrupole tandem mass spectrometry

    Science.gov (United States)

    Shen, X. C.; Zhang, Y. L.; Cui, Y. Q.; Xu, L. Y.; Li, X.; Qi, J. H.

    2017-07-01

    Heterocyclic aromatic amines (HAAs) are potent mutagens that formed at high temperature in cooked, protein-rich food. Owing to their frequent intake, an accurate method is essential to access human health risk of HAAs exposure through detecting these compounds in various heat-treated meat products. In this study, a liquid chromatography-electrospray tandem mass spectrometry (LC--ESI-MS/MS) method was developed to perform the determination of 9 mutagenic heterocyclic amines (HAAs) in meat samples with multiple reaction monitoring (MRM) mode. Ultrasound assisted extraction and diatomaceous earth was employed to extract HAAs from food samples, and the analytes were purified and enriched using tandem solid phase extraction, with propyl sulfonic acid coupled to a C18 cartridge. Two parameters, extraction time and eluent, were carefully optimized to improve the extraction and purification efficiency. The LC separation was carried out using a Zorbax SB-C18 (3.5 μm particle size, 2.1 × 150 mm i.d.) column and optimized some parameters, such as pH, concentration and volume. Under the optimal experimental conditions, recoveries ranged from 52.97% to 97.11% with good quality parameters: limit of detection values between 0.02 and 0.24 ng mL-1, linearity (R2>0.998), and run-to-run and day-to-day precisions lower than 9.81% achieved. To evaluate the performance of the method in high throughput analysis of complex meat samples, the LC-MS/MS method was applied to the analysis of HAAs in three food samples, and the results demonstrated that the method can be used for the trace determination of HAAs in pork samples.

  3. Sensitivity enhancement in direct coupling of supported liquid membrane extractions to capillary electrophoresis by means of transient isotachophoresis and large electrokinetic injections

    Czech Academy of Sciences Publication Activity Database

    Pantůčková, Pavla; Kubáň, Pavel; Boček, Petr

    2015-01-01

    Roč. 1389, APR (2015), s. 1-7 ISSN 0021-9673 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : capillary electrophoresis * in-line coupling * supported liquid membrane extraction Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.926, year: 2015

  4. Determination of {sup 236}U in environmental samples by single extraction chromatography coupled to triple-quadrupole inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Guosheng [Department of Radiation Chemistry, Institute of Radiation Emergency Medicine, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori, 036-8564 (Japan); Division of Nuclear Technology and Applications, Institute of High Energy Physics, Chinese Academy of Sciences (China); Beijing Engineering Research Center of Radiographic Techniques and Equipment, Beijing, 100049 (China); Tazoe, Hirofumi [Department of Radiation Chemistry, Institute of Radiation Emergency Medicine, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori, 036-8564 (Japan); Yamada, Masatoshi, E-mail: myamada@hirosaki-u.ac.jp [Department of Radiation Chemistry, Institute of Radiation Emergency Medicine, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori, 036-8564 (Japan)

    2016-11-09

    In order to measure trace {sup 236}U and {sup 236}U/{sup 238}U in environmental samples with a high matrix effect, a novel and simple method was developed that makes the digestion and purification procedures compatible with advanced triple-quadrupole inductively coupled plasma-mass spectrometry. A total dissolution of sample with HF + HNO{sub 3} + HClO{sub 4} was followed by chromatographic separation with a single resin column containing normal type DGA resin (N,N,N′,N’-tetra-n-octyldiglycolamide) as the extractant system. The analytical accuracy and precision of {sup 236}U/{sup 238}U ratios, measured as {sup 236}U{sup 16}O{sup +}/{sup 238}U{sup 16}O{sup +}, were examined by using the reference materials IAEA-135, IAEA-385, IAEA-447, and JSAC 0471. The low method detection limit (3.50 × 10{sup −6} Bq kg{sup −1}) makes it possible to perform routine monitoring of environmental {sup 236}U due to global fallout combined with the Fukushima Daiichi Nuclear Power Plant accident fallout (>10{sup −5} Bq kg{sup −1}). Finally, the developed method was successfully applied to measure {sup 236}U/{sup 238}U ratios and {sup 236}U activities in soil samples contaminated by the accident. The low {sup 236}U/{sup 238}U atom ratios ((1.50–13.5) × 10{sup −8}) and {sup 236}U activities ((2.25–14.1) × 10{sup −2} mBq kg{sup −1}) indicate {sup 236}U contamination was mainly derived from global fallout in the examined samples. - Highlights: • A simple {sup 236}U/{sup 238}U analytical method has been developed. • The separation required just one DGA column chromatography. • {sup 236}U/{sup 238}U atom ratios in soil were measured by ICP-MS/MS. • {sup 236}U/{sup 238}U atom ratios of (1.50–13.5) × 10{sup −8} were observed in Japanese samples. • {sup 236}U activities of (2.25–14.1) × 10{sup −2} mBq kg{sup −1} were found in Japanese samples.

  5. Sequential cloud point extraction for the speciation of mercury in seafood by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li Yingjie [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)], E-mail: binhu@whu.edu.cn

    2007-10-15

    A novel nonchromatographic speciation technique for the speciation of mercury by sequential cloud point extraction (CPE) combined with inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. The method based on Hg{sup 2+} was complexed with I{sup -} to form HgI{sub 4}{sup 2-}, and the HgI{sub 4}{sup 2-} reacted with the methyl green (MG) cation to form hydrophobic ion-associated complex, and the ion-associated complex was then extracted into the surfactant-rich phase of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114), which are subsequently separated from methylmercury (MeHg{sup +}) in the initial solution by centrifugation. The surfactant-rich phase containing Hg(II) was diluted with 0.5 mol L{sup -1} HNO{sub 3} for ICP-OES determination. The supernatant is also subjected to the similar CPE procedure for the preconcentration of MeHg{sup +} by the addition of a chelating agent, ammonium pyrrolidine dithiocarbamate (APDC), in order to form water-insolvable complex with MeHg{sup +}. The MeHg{sup +} in the micelles was directly analyzed after disposal as describe above. Under the optimized conditions, the extraction efficiency was 93.5% for Hg(II) and 51.5% for MeHg{sup +} with the enrichment factor of 18.7 for Hg(II) and 10.3 for MeHg{sup +}, respectively. The limits of detection (LODs) were 56.3 ng L{sup -1} for Hg(II) and 94.6 ng L{sup -1} for MeHg{sup +} (as Hg) with the relative standard deviations (RSDs) of 3.6% for Hg(II) and 4.5% for MeHg{sup +} (C = 10 {mu}g L{sup -1}, n = 7), respectively. The developed technique was applied to the speciation of mercury in real seafood samples and the recoveries for spiked samples were found to be in the range of 93.2-108.7%. For validation, a certified reference material of DORM-2 (dogfish muscle) was analyzed and the determined values are in good agreement with the certified values.

  6. Sequential cloud point extraction for the speciation of mercury in seafood by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Li Yingjie; Hu Bin

    2007-01-01

    A novel nonchromatographic speciation technique for the speciation of mercury by sequential cloud point extraction (CPE) combined with inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. The method based on Hg 2+ was complexed with I - to form HgI 4 2- , and the HgI 4 2- reacted with the methyl green (MG) cation to form hydrophobic ion-associated complex, and the ion-associated complex was then extracted into the surfactant-rich phase of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114), which are subsequently separated from methylmercury (MeHg + ) in the initial solution by centrifugation. The surfactant-rich phase containing Hg(II) was diluted with 0.5 mol L -1 HNO 3 for ICP-OES determination. The supernatant is also subjected to the similar CPE procedure for the preconcentration of MeHg + by the addition of a chelating agent, ammonium pyrrolidine dithiocarbamate (APDC), in order to form water-insolvable complex with MeHg + . The MeHg + in the micelles was directly analyzed after disposal as describe above. Under the optimized conditions, the extraction efficiency was 93.5% for Hg(II) and 51.5% for MeHg + with the enrichment factor of 18.7 for Hg(II) and 10.3 for MeHg + , respectively. The limits of detection (LODs) were 56.3 ng L -1 for Hg(II) and 94.6 ng L -1 for MeHg + (as Hg) with the relative standard deviations (RSDs) of 3.6% for Hg(II) and 4.5% for MeHg + (C = 10 μg L -1 , n = 7), respectively. The developed technique was applied to the speciation of mercury in real seafood samples and the recoveries for spiked samples were found to be in the range of 93.2-108.7%. For validation, a certified reference material of DORM-2 (dogfish muscle) was analyzed and the determined values are in good agreement with the certified values

  7. Solid-Phase Extraction Coupled to a Paper-Based Technique for Trace Copper Detection in Drinking Water.

    Science.gov (United States)

    Quinn, Casey W; Cate, David M; Miller-Lionberg, Daniel D; Reilly, Thomas; Volckens, John; Henry, Charles S

    2018-03-20

    Metal contamination of natural and drinking water systems poses hazards to public and environmental health. Quantifying metal concentrations in water typically requires sample collection in the field followed by expensive laboratory analysis that can take days to weeks to obtain results. The objective of this work was to develop a low-cost, field-deployable method to quantify trace levels of copper in drinking water by coupling solid-phase extraction/preconcentration with a microfluidic paper-based analytical device. This method has the advantages of being hand-powered (instrument-free) and using a simple "read by eye" quantification motif (based on color distance). Tap water samples collected across Fort Collins, CO, were tested with this method and validated against ICP-MS. We demonstrate the ability to quantify the copper content of tap water within 30% of a reference technique at levels ranging from 20 to 500 000 ppb. The application of this technology, which should be sufficient as a rapid screening tool, can lead to faster, more cost-effective detection of soluble metals in water systems.

  8. Use of ultrasound radiation for extraction of bioactive compounds from natural sources. Current events and perspectives; Empleo de la radiacion ultrasonica para la extraccion de compuestos bioactivos provenientes de fuentes naturales. Estado actual y perspectivas

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez Riera, Zalua [Instituto Superior de Tecnologia y Ciencias Aplicadas (INSTEC), La Habana (Cuba); Robaina Mesa, Malvis [Centro de Investigacion y Desarrollo de Medicamentos, La Habana (Cuba); Jauregui Haza, Ulises, E-mail: zalua@instec.cu [Instituto Superior de Tecnologia y Ciencias Aplicadas (INSTEC), La Habana (Cuba)

    2014-07-01

    In recent years, clean technologies have been developed for high efficiency extracting of isolation of biologically active compounds from natural sources, without the loss of biological activity, with good yield and high purity. Ultrasound-assisted extraction has low instrumental requirements and their implementation is very appropriate where the stability of the active component to be removed is affected by the high temperatures of conventional processes. In this paper it is evaluated the state of the art of ultrasound-assisted extraction of bioactive compounds from various natural sources, its mechanism, the parameters governing its use and research perspectives in this field. Ultrasonic cavitation phenomenon promotes cell wall rupture, reduction of particle size and tissue permeability, which facilitates the diffusion of the solvent into the inert part of the plant material and increasing the mass transferred through membranes. This mechanism explains the high efficiency of ultrasound-assisted extraction as it allows to reduce the time, temperature and amounts of solvent extraction process with high yields and high purity of the extracted product. Currently there is a great demand for the use of ultrasound to industrial and current research lead to the development of larger scale reactors and the theoretical modeling of the parameters that determine efficient extraction.

  9. Speciation analysis of inorganic arsenic by magnetic solid phase extraction on-line with inductively coupled mass spectrometry determination.

    Science.gov (United States)

    Montoro Leal, P; Vereda Alonso, E; López Guerrero, M M; Cordero, M T Siles; Cano Pavón, J M; García de Torres, A

    2018-07-01

    Arsenic, one of the main environmental pollutants and potent natural poison, is a chemical element that is spread throughout the Earth's crust. It is well known that the toxicity of arsenic is highly dependent on its chemical forms. Generally, the inorganic species are more toxic than its organics forms, and As(III) is 60 times more toxic than As(V). In environmental waters, arsenic exists predominantly in two chemical forms: As(III) and As(V). In view of these facts, fast, sensitive, accurate and simple analytical methods for the speciation of inorganic arsenic in environmental waters are required. In this work, a new magnetic solid phase extraction with a hydride generation system was coupled on line with inductively coupled plasma mass spectrometry (MSPE-HG-ICP-MS). The new system was based on the retention of As(III) and As(V) in two knotted reactors filled with (Fe 3 O 4 ) magnetic nanoparticles functionalized with [1,5-bis (2-pyridyl) 3-sulfophenylmethylene] thiocarbonohydrazide (PSTH-MNPs). As(III) and total inorganic As were sequentially eluted in different reduction conditions. The concentration of As(V) was obtained by subtracting As(III) from total As. The system runs in a fully automated way and the method has proved to have a wide linear range and to be precise, sensitive and fast. The detection limits found were 2.7 and 3.2 ng/L for As(III) and total As, respectively; with relative standard deviations (RSDs) of 2.5% and 2.7% and a sample throughput of 14.4 h -1 . In order to validate the developed method, several certified reference samples of environmental waters including sea water, were analyzed and the determined values were in good agreement with the certified values. The proposed method was successfully applied to the speciation analysis of inorganic arsenic in well-water and sea water. Copyright © 2018 Elsevier B.V. All rights reserved.

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

    Directory of Open Access Journals (Sweden)

    Júlio Cezar Flores JOHNER

    2016-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Kempka Thomas

    2015-04-01

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

  12. An improved facile method for extraction and determination of steroidal saponins in Tribulus terrestris by focused microwave-assisted extraction coupled with GC-MS.

    Science.gov (United States)

    Li, Tianlin; Zhang, Zhuomin; Zhang, Lan; Huang, Xinjian; Lin, Junwei; Chen, Guonan

    2009-12-01

    An improved fast method for extraction of steroidal saponins in Tribulus terrestris based on the use of focus microwave-assisted extraction (FMAE) is proposed. Under optimized conditions, four steroidal saponins were extracted from Tribulus terrestris and identified by GC-MS, which are Tigogenin (TG), Gitogenin (GG), Hecogenin (HG) and Neohecogenin (NG). One of the most important steroidal saponins, namely TG was quantified finally. The recovery of TG was in the range of 86.7-91.9% with RSDTribulus terrestris from different areas of occurrence. The difference in chromatographic characteristics of steroidal saponins was proved to be related to the different areas of occurrence. The results showed that FMAE-GC-MS is a simple, rapid, solvent-saving method for the extraction and determination of steroidal saponins in Tribulus terrestris.

  13. Negative-Pressure Cavitation Extraction of Secoisolariciresinol Diglycoside from Flaxseed Cakes

    Directory of Open Access Journals (Sweden)

    Hao Tian

    2015-06-01

    Full Text Available The negative-pressure cavitation extraction (NPCE technique was applied firstly to extract secoisolariciresinol diglucoside (SDG from flaxseed cakes. The significant extraction parameters were screened by fractional factorial design (FFD. The optimal parameters were determined using the central composite design (CCD with the two variables, NaOH amount and the liquid/solid ratio. The conditions of the extraction were optimized by using response surface methodology (RSM. Under the optimal conditions, the extraction yield and the extraction purity of SDG was 16.25 mg/g and 3.86%, respectively. The efficiency of NPCE was compared with that of conventional extraction methods. Our results demonstrated that NPCE was comparable to the well-known ultrasound-assisted extraction in term of extraction yield and purity. This extraction technique has advantages of less time-consuming, low solvent usage and high throughput capability.

  14. Optimization of ultrasound and microwave assisted extractions of polyphenols from black rice (Oryza sativa cv. Poireton) husk.

    Science.gov (United States)

    Jha, Pankaj; Das, Arup Jyoti; Deka, Sankar Chandra

    2017-11-01

    Phenolic compounds were extracted from the husk of milled black rice (cv. Poireton) by using a combination of ultrasound assisted extraction and microwave assisted extraction. Extraction parameters were optimized by response surface methodology according to a three levels, five variables Box-Behnken design. The appropriate process variables (extraction temperature and extraction time) to maximize the ethanolic extraction of total phenolic compounds, flavonoids, anthocyanins and antioxidant activity of the extracts were obtained. Extraction of functional components with varying ethanol concentration and microwave time were significantly affected by the process variables. The best possible conditions obtained by RSM for all the factors included 10.02 min sonication time, 49.46 °C sonication temperature, 1:40.79 (w/v) solute solvent ratio, 67.34% ethanol concentration, and 31.11 s microwave time. Under the given solutions, the maximum extraction of phenolics (1.65 mg/g GAE), flavonoids (3.04 mg/100 g), anthocyanins (3.39 mg/100 g) and antioxidants (100%) were predicted, while the experimental values included 1.72 mg/g GAE of total phenolics, 3.01 mg/100 g of flavonoids, 3.36 mg/100 g of anthocyanins and 100% antioxidant activity. The overall results indicated positive impact of co-application of microwave and ultrasound assisted extractions of phenolic compounds from black rice husk.

  15. Accelerated solvent extraction followed by on-line solid-phase extraction coupled to ion trap LC/MS/MS for analysis of benzalkonium chlorides in sediment samples

    Science.gov (United States)

    Ferrer, I.; Furlong, E.T.

    2002-01-01

    Benzalkonium chlorides (BACs) were successfully extracted from sediment samples using a new methodology based on accelerated solvent extraction (ASE) followed by an on-line cleanup step. The BACs were detected by liquid chromatography/ion trap mass spectrometry (LC/MS) or tandem mass spectrometry (MS/MS) using an electrospray interface operated in the positive ion mode. This methodology combines the high efficiency of extraction provided by a pressurized fluid and the high sensitivity offered by the ion trap MS/MS. The effects of solvent type and ASE operational variables, such as temperature and pressure, were evaluated. After optimization, a mixture of acetonitrile/water (6:4 or 7:3) was found to be most efficient for extracting BACs from the sediment samples. Extraction recoveries ranged from 95 to 105% for C12 and C14 homologues, respectively. Total method recoveries from fortified sediment samples, using a cleanup step followed by ASE, were 85% for C12BAC and 79% for C14-BAC. The methodology developed in this work provides detection limits in the subnanogram per gram range. Concentrations of BAC homologues ranged from 22 to 206 ??g/kg in sediment samples from different river sites downstream from wastewater treatment plants. The high affinity of BACs for soil suggests that BACs preferentially concentrate in sediment rather than in water.

  16. Polytetrafluorethylene film-based liquid-three phase micro extraction coupled with differential pulse voltammetry for the determination of atorvastatin calcium.

    Science.gov (United States)

    Ensafi, Ali A; Khoddami, Elaheh; Rezaei, Behzad

    2013-01-01

    In this paper, we describe a new combination method based on polytetrafluorethylene (PTFE) film-based liquid three-phase micro extraction coupled with differential pulse voltammetry (DPV) for the micro extraction and quantification of atorvastatin calcium (ATC) at the ultra-trace level. Different factors affecting the liquid-three phases micro extraction of atorvastatin calcium, including organic solvent, pH of the donor and acceptor phases, concentration of salt, extraction time, stirring rate and electrochemical factors, were investigated, and the optimal extraction conditions were established. The final stable signal was achieved after a 50 min extraction time, which was used for analytical applications. An enrichment factor of 21 was achieved, and the relative standard deviation (RSD) of the method was 4.5% (n = 4). Differential pulse voltammetry exhibited two wide linear dynamic ranges of 20.0-1000.0 pmol L(-1) and 0.001-11.0 µmol L(-1) of ATC. The detection limit was found to be 8.1 pmol L(-1) ATC. Finally, the proposed method was used as a new combination method for the determination of atorvastatin calcium in real samples, such as human urine and plasma.

  17. Critical comparison of the on-line and off-line molecularly imprinted solid-phase extraction of patulin coupled with liquid chromatography.

    Science.gov (United States)

    Lhotská, Ivona; Holznerová, Anežka; Solich, Petr; Šatínský, Dalibor

    2017-12-01

    Reaching trace amounts of mycotoxin contamination requires sensitive and selective analytical tools for their determination. Improving the selectivity of sample pretreatment steps covering new and modern extraction techniques is one way to achieve it. Molecularly imprinted polymers as selective sorbent for extraction undoubtedly meet these criteria. The presented work is focused on the hyphenation of on-line molecularly imprinted solid-phase extraction with a chromatography system using a column-switching approach. Making a critical comparison with a simultaneously developed off-line extraction procedure, evaluation of pros and cons of each method, and determining the reliability of both methods on a real sample analysis were carried out. Both high-performance liquid chromatography methods, using off-line extraction on molecularly imprinted polymer and an on-line column-switching approach, were validated, and the validation results were compared against each other. Although automation leads to significant time savings, fewer human errors, and required no handling of toxic solvents, it reached worse detection limits (15 versus 6 μg/L), worse recovery values (68.3-123.5 versus 81.2-109.9%), and worse efficiency throughout the entire clean-up process in comparison with the off-line extraction method. The difficulties encountered, the compromises made during the optimization of on-line coupling and their critical evaluation are presented in detail. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Urban Heat Island Simulations in Guangzhou, China, Using the Coupled WRF/UCM Model with a Land Use Map Extracted from Remote Sensing Data

    Directory of Open Access Journals (Sweden)

    Guang Chen

    2016-07-01

    Full Text Available The Weather Research and Forecasting (WRF model coupled with an Urban Canopy Model (UCM was used for studying urban environmental issues. Because land use data employed in the WRF model do not agree with the current situation around Guangzhou, China, the performance of WRF/UCM with new land-use data extracted from Remote Sensing (RS data was evaluated in early August 2012. Results from simulations reveal that experiments with the extracted data are capable of reasonable reproductions of the majority of the observed temporal characteristics of the 2-m temperature, and can capture the characteristics of Urban Heat Island (UHI. The “UCM_12” simulation, which employed the extracted land-use data with the WRF/UCM model, provided the best reproduction of the 2-m temperature data evolution and the smallest minimum absolute average error when compared with the other two experiments without coupled UCM. The contributions of various factors to the UHI effect were analyzed by comparing the energy equilibrium processes of “UCM_12” in urban and suburban areas. Analysis revealed that energy equilibrium processes with new land use data can explain the diurnal character of the UHI intensity variation. Furthermore, land use data extracted from RS can be used to simulate the UHI.

  19. Arsenic species determination in human scalp hair by pressurized hot water extraction and high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Morado Piñeiro, Andrés; Moreda-Piñeiro, Jorge; Alonso-Rodríguez, Elia; López-Mahía, Purificación; Muniategui-Lorenzo, Soledad; Prada-Rodríguez, Darío

    2013-02-15

    Analytical methods for the determination of total arsenic and arsenic species (mainly As(III) and As(V)) in human scalp hair have been developed. Inductively coupled plasma-mass spectrometry (ICP-MS) and high performance liquid chromatography (HPLC) coupled to ICP-MS have been used for total arsenic and arsenic species determination, respectively. The proposed methods include a "green", fast, high efficient and automated species leaching procedure by pressurized hot water extraction (PHWE). The operating parameters for PHWE including modifier concentration, extraction temperature, static time, extraction steps, pressure, mean particle size, diatomaceous earth (DE) mass/sample mass ratio and flush volume were studied using design of experiments (Plackett-Burman design PBD). Optimum condition implies a modifier concentration (acetic acid) of 150 mM and powdered hair samples fully mixed with diatomaceous earth (DE) as a dispersing agent at a DE mass/sample mass ratio of 5. The extraction has been carried out at 100°C and at an extraction pressure of 1500 psi for 5 min in four extraction step. Under optimised conditions, limits of quantification of 7.0, 6.3 and 50.3 ng g(-1) for total As, As(III) and As(V), respectively were achieved. Repeatability of the overall procedure (4.4, 7.2 and 2.1% for total As, As(III) and As(V), respectively) was achieved. The analysis of GBW-07601 (human hair) certified reference material was used for validation. The optimised method has been finally applied to several human scalp hair samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  20. Identification and quantification of metallothionein isoforms and superoxide dismutase in spiked liver extracts using HPLC-ESI-MS offline coupling and HPLC-ICP-MS online coupling.

    Science.gov (United States)

    Nischwitz, V; Michalke, B; Kettrup, A

    2003-01-01

    A two-dimensional chromatographic method for the characterization of metallothionein isoforms (MT) and superoxide dismutase (SOD) in spiked liver extracts was developed for the optimization of extraction procedures from liver samples. Element-specific detection (ICP-MS) and molecule-specific detection (ESI-MS) were applied for maximum species information. A special focus was laid on the quantitative data evaluation (species stoichiometry, calibration with and without matrix, recovery), which is neglected in most MT/SOD publications with hyphenated techniques. Linearity, precision (residual standard deviation of calibration curves <10%), and detection limits (<0.6 mg L(-1) for MT isoforms and 13 mg L(-1) for SOD) prove the suitability of the method for quantification. An alternative quantification is proposed for the extension towards other lesser or even unknown trace element species, especially the native porcine MT and SOD.

  1. Determination of ketamine and its main metabolites by liquid chromatography coupled to tandem mass spectrometry in pig plasma: Comparison of extraction methods.

    Science.gov (United States)

    Ramiole, Cindy; D'Hayer, Benoit; Boudy, Vincent; Legagneux, Josette; Fonsart, Julien; Houzé, Pascal

    2017-11-30

    A rapid, sensitive and specific liquid chromatography coupled to tandem mass spectrometry method was developed for the simultaneous quantification pig plasma of ketamine and its two principal metabolites, norketamine and dehydronorketamine. Three extraction procoles were assessed including acetonitrile precipitation, Oase™ microplate extraction, and liquid-liquid extraction. Oase™ microplate extraction induced no significant matrix effect, important signal/noise ratio and good recoveries, ranging from 82 to 87% for the considered compounds. Using this extraction procedure, the assay was linear in the dynamic range 10-3000ng/mL (R 2 >0.99) regardless of the analytes. Intra- and inter-day accuracies were less than 12% for all compounds and intra- and inter-day precisions expressed as RSD were within ketamine, norketamine and dehydronorketamine concentrations up to 15,000ng/mL can be determined with good precision using appropriate sample dilution. The assay was successfully applied to pig plasma samples to determine the pharmacokinetics of ketamine and the consecutive metabolites after buccal administration of a 4mg/kg ketamine base solutions. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Online micro-solid-phase extraction based on boronate affinity monolithic column coupled with high-performance liquid chromatography for the determination of monoamine neurotransmitters in human urine.

    Science.gov (United States)

    Yang, Xiaoting; Hu, Yufei; Li, Gongke

    2014-05-16

    Quantification of monoamine neurotransmitters is very important in diagnosing and monitoring of patients with neurological disorders. We developed an online analytical method to selectively determine urinary monoamine neurotransmitters, which coupled the boronate affinity monolithic column micro-solid-phase extraction with high-performance liquid chromatography (HPLC). The boronate affinity monolithic column was prepared by in situ polymerization of vinylphenylboronic acid (VPBA) and N,N'-methylenebisacrylamide (MBAA) in a stainless capillary column. The prepared monolithic column showed good permeability, high extraction selectivity and capacity. The column-to-column reproducibility was satisfactory and the enrichment factors were 17-243 for four monoamine neurotransmitters. Parameters that influence the online extraction efficiency, including pH of sample solution, flow rate of extraction and desorption, extraction volume and desorption volume were investigated. Under the optimized conditions, the developed method exhibited low limit of detection (0.06-0.80μg/L), good linearity (with R(2) between 0.9979 and 0.9993). The recoveries in urine samples were 81.0-105.5% for four monoamine neurotransmitters with intra- and inter-day RSDs of 2.1-8.2% and 3.7-10.6%, respectively. The online analytical method was sensitive, accurate, selective, reliable and applicable to analysis of trace monoamine neurotransmitters in human urine sample. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Determination of Cd, Pb, Zn and Cu in Sediment Compartments by Sequential Extraction and Isotope Dilution Inductively Coupled Plasma Mass Spectrometry (ID-ICP-MS

    Directory of Open Access Journals (Sweden)

    Gardolinski Paulo C. F. C.

    2002-01-01

    Full Text Available Trace concentrations of Cd, Cu, Pb and Zn in four different sediment fractions extracted in sequence were determined by isotope dilution inductively coupled mass spectrometry (IDICPMS. The metals from each fraction were extracted following the sequential extraction procedure recommended by the Bureau Commun de Référence (BCR of the Commission of the European Communities. As an alternative to external calibration, the elements were quantified by spiking the extracted solutions with 112Cd, 63Cu, 208Pb and 66Zn and application of isotope dilution. The proposed approach was applied to a sample collected from a lake and two standard reference materials, NIST2704 river sediment from the National Institute of Standards & Technology and the BCR-277 estuarine sediment. Detection limits, for each extracted solution, varied from 0.31 to 0.53 mug L¹ for Cd, 0.92 to 2.9 mug L¹ for Cu, 0.22 to 1.1 mug L¹ for Pb and 1.3 to 7.6 mug L¹ for Zn. The sum of the metals concentration in the different fractions was compatible with 95% confidence level found amounts obtained with complete digestion of the samples and with the certified values of the standard reference materials.

  4. Syringe needle-based sampling coupled with liquid-phase extraction for determination of the three-dimensional distribution of l-ascorbic acid in apples.

    Science.gov (United States)

    Tang, Sheng; Lee, Hian Kee

    2016-05-15

    A novel syringe needle-based sampling approach coupled with liquid-phase extraction (NBS-LPE) was developed and applied to the extraction of l-ascorbic acid (AsA) in apple. In NBS-LPE, only a small amount of apple flesh (ca. 10mg) was sampled directly using a syringe needle and placed in a glass insert for liquid extraction of AsA by 80 μL oxalic acid-acetic acid. The extract was then directly analyzed by liquid chromatography. This new procedure is simple, convenient, almost organic solvent free, and causes far less damage to the fruit. To demonstrate the applicability of NBS-LPE, AsA levels at different sampling points in a single apple were determined to reveal the spatial distribution of the analyte in a three-dimensional model. The results also showed that this method had good sensitivity (limit of detection of 0.0097 mg/100g; limit of quantification of 0.0323 mg/100g), acceptable reproducibility (relative standard deviation of 5.01% (n=6)), a wide linear range of between 0.05 and 50mg/100g, and good linearity (r(2)=0.9921). This interesting extraction technique and modeling approach can be used to measure and monitor a wide range of compounds in various parts of different soft-matrix fruits and vegetables, including single specimens. Copyright © 2015 Elsevier Ltd. All rights reserved.

  5. Electrotechnologies, microwaves, and ultrasounds combined with binary mixtures of ethanol and water to extract steviol glycosides and antioxidant compounds from Stevia rebaudiana leaves

    DEFF Research Database (Denmark)

    Carbonell-Capella, Juana M.; Šic Žlabur, Jana; Rimac Brnčić, Suzana

    2017-01-01

    /g) was obtained after ultrasound-assisted extraction, while microwave allowed the highest yields of rebaudioside A (22.7 ± 0.1 mg/g). However, pulsed electric field technology was the most efficient to recover stevioside (44.2 ± 0.1 mg/g) and rebaudioside A (22.4 ± 0.3 mg/g) when using 50% ethanol-water. Results...... leaves in food industry is usually performed using thermal extraction under agitation after drying and grinding. Although efficient, this technique generates an extract not only rich in targeted compounds but also in impurities, which complicates the downstream processing steps. Selective extraction...

  6. A comparison of sorptive extraction techniques coupled to a new quantitative, sensitive, high throughput GC-MS/MS method for methoxypyrazine analysis in wine.

    Science.gov (United States)

    Hjelmeland, Anna K; Wylie, Philip L; Ebeler, Susan E

    2016-02-01

    Methoxypyrazines are volatile compounds found in plants, microbes, and insects that have potent vegetal and earthy aromas. With sensory detection thresholds in the low ng L(-1) range, modest concentrations of these compounds can profoundly impact the aroma quality of foods and beverages, and high levels can lead to consumer rejection. The wine industry routinely analyzes the most prevalent methoxypyrazine, 2-isobutyl-3-methoxypyrazine (IBMP), to aid in harvest decisions, since concentrations decrease during berry ripening. In addition to IBMP, three other methoxypyrazines IPMP (2-isopropyl-3-methoxypyrazine), SBMP (2-sec-butyl-3-methoxypyrazine), and EMP (2-ethyl-3-methoxypyrazine) have been identified in grapes and/or wine and can impact aroma quality. Despite their routine analysis in the wine industry (mostly IBMP), accurate methoxypyrazine quantitation is hindered by two major challenges: sensitivity and resolution. With extremely low sensory detection thresholds (~8-15 ng L(-1) in wine for IBMP), highly sensitive analytical methods to quantify methoxypyrazines at trace levels are necessary. Here we were able to achieve resolution of IBMP as well as IPMP, EMP, and SBMP from co-eluting compounds using one-dimensional chromatography coupled to positive chemical ionization tandem mass spectrometry. Three extraction techniques HS-SPME (headspace-solid phase microextraction), SBSE (stirbar sorptive extraction), and HSSE (headspace sorptive extraction) were validated and compared. A 30 min extraction time was used for HS-SPME and SBSE extraction techniques, while 120 min was necessary to achieve sufficient sensitivity for HSSE extractions. All extraction methods have limits of quantitation (LOQ) at or below 1 ng L(-1) for all four methoxypyrazines analyzed, i.e., LOQ's at or below reported sensory detection limits in wine. The method is high throughput, with resolution of all compounds possible with a relatively rapid 27 min GC oven program. Copyright © 2015

  7. 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)

  8. Metal-coated semiconductor nanostructures and simulation of photon extraction and coupling to optical fibers for a solid-state single-photon source

    International Nuclear Information System (INIS)

    Suemune, Ikuo; Nakajima, Hideaki; Liu, Xiangming; Odashima, Satoru; Asano, Tomoya; Iijima, Hitoshi; Huh, Jae-Hoon; Idutsu, Yasuhiro; Sasakura, Hirotaka; Kumano, Hidekazu

    2013-01-01

    We have realized metal-coated semiconductor nanostructures for a stable and efficient single-photon source (SPS) and demonstrated improved single-photon extraction efficiency by the selection of metals and nanostructures. We demonstrate with finite-difference time-domain (FDTD) simulations that inclination of a pillar sidewall, which changes the structure to a nanocone, is effective in improving the photon extraction efficiency. We demonstrate how such nanocone structures with inclined sidewalls are fabricated with reactive ion etching. With the optimized design, a photon extraction efficiency to outer airside as high as ∼97% generated from a quantum dot in a nanocone structure is simulated, which is the important step in realizing SPS on-demand operations. We have also examined the direct contact of such a metal-embedded nanocone structure with a single-mode fiber facet as a simple and practical method for preparing fiber-coupled SPS and demonstrated practical coupling efficiencies of ∼16% with FDTD simulation. (paper)

  9. Determination of isoquercitrin in rat plasma by high performance liquid chromatography coupled with a novel synergistic cloud point extraction.

    Science.gov (United States)

    Zhou, Jun; Sun, Jiang Bing; Wang, Qiao Feng

    2018-01-01

    A novel improved preconcentration method known as synergistic cloud point extraction was established for isoquercitrin preconcentration and determination in rat plasma prior to its determination by high performance liquid chromatography. Synergistic cloud point extraction greatly simplified isoquercitrin extraction and detection. This method was accomplished at room temperature (about 22°C) in 1min with the nonionic surfactant Tergitol TMN-6 as the extractant, n-octanol as cloud point revulsant and synergic reagent. Parameters that affect the synergistic cloud point extraction processes, such as the concentrations of Tergitol TMN-6, volume of n-octanol, sample pH, salt content and extraction time were investigated and optimized. Under the optimum conditions, the calibration curve for the analyte was linear in the range from 5 to 500ngmL -1 with the correlation coefficients greater than 0.9996. Meanwhile, limit of detection (S/N=3) was less than 1.6ngmL -1 and limit of quantification (S/N=10) was less than 5ngmL -1 . It demonstrated that the method can be successfully applied to the pharmacokinetic investigation of isoquercitrin. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. The influence of coupled synchrotron-betatron resonances on the extracted beam of the stretcher ring ELSA

    International Nuclear Information System (INIS)

    Neckenig, M.

    1987-09-01

    For the correction of the chromaticity for horizontal and vertical direction each four sextupoles are installed in ELSA. At a working point near 14/3 their influence on the quantity of the stable region of the transverse phase space is essentially smaller than that of the extraction sextupoles. On the other hand the latter lie at positions of low dispersion so that their influence on the chromaticity is negligible; therefore chromaticity correction and choice of the stable phase-space region are not strongly mutually dependent which will be of advance for the later operation. In extraction with corrected chromaticity the electrons are extracted only because of their different position in the transverse phase space which leads to a timely alteration of the η coordinate and by this to a migration of the extracted beam. Consequences of this are the strongly against extraction without chromaticity correction increased emittance and the doubled momentum uncertainty of the beam. Of advance however is the high extraction efficiency of 80% and the small number of the electrons remaining in the ring (below 2%). (orig./HSI) [de

  11. Surfactant-enhanced liquid-liquid microextraction coupled to micro-solid phase extraction onto highly hydrophobic magnetic nanoparticles

    International Nuclear Information System (INIS)

    Giannoulis, Kiriakos M.; Giokas, Dimosthenis L.; Tsogas, George Z.; Vlessidis, Athanasios G.; Zhu, Qing; Pan, Qinmin

    2013-01-01

    We are presenting a simplified alternative method for dispersive liquid-liquid microextraction (DLLME) by resorting to the use of surfactants as emulsifiers and micro solid-phase extraction (μ-SPE). In this combined procedure, DLLME of hydrophobic components is initially accomplished in a mixed micellar/microemulsion extractant phase that is prepared by rapidly mixing a non-ionic surfactant and 1-octanol in aqueous medium. Then, and in contrast to classic DLLME, the extractant phase is collected by highly hydrophobic polysiloxane-coated core-shell Fe 2 O 3 (at)C magnetic nanoparticles. Hence, the sample components are the target analyte in the DLLME which, in turn, becomes the target analyte of the μ-SPE step. This 2-step approach represents a new and simple DLLME procedure that lacks tedious steps such as centrifugation, thawing, or delicate collection of the extractant phase. As a result, the analytical process is accelerated and the volume of the collected phase does not depend on the volume of the extraction solvent. The method was applied to extract cadmium in the form of its pyrrolidine dithiocarbamate chelate from spiked water samples prior to its determination by FAAS. Detection limits were brought down to the low μg L −1 levels by preconcentrating 10 mL samples with satisfactory recoveries (96.0–108.0 %). (author)

  12. Flourensia cernua: Hexane Extracts a Very Active Mycobactericidal Fraction from an Inactive Leaf Decoction against Pansensitive and Panresistant Mycobacterium tuberculosis

    Directory of Open Access Journals (Sweden)

    Gloria María Molina-Salinas

    2011-01-01

    Full Text Available The efficacy of decoction in extracting mycobactericidal compounds from Flourensia cernua (Hojasé leaves and fractionation with solvents having ascending polarity was compared with that of (i ethanol extraction by still maceration, extraction with a Soxhlet device, shake-assisted maceration, or ultrasound-assisted maceration, followed by fractionation with n-hexane, ethyl acetate, and n-butanol; (ii sequential extraction with n-hexane, ethyl acetate, and n-butanol, by still maceration, using a Soxhlet device, shake-assisted maceration, or ultrasound-assisted maceration. The in vitro mycobactericidal activity of each preparation was measured against drug-sensitive (SMtb and drug-resistant (RMtb Mycobacterium tuberculosis strains. The results of which were expressed as absolute mycobactericidal activity (AMA. These data were normalized to the ΣAMA of the decoction fraction set. Although decoction was inactive, the anti-RMtb normalized ΣAMA (NAMA of its fractions was comparable with the anti-RMtb NAMA of the still maceration extracts and significantly higher than the anti-SMtb and anti-RMtb NAMAs of every other ethanol extract and serial extract and fraction. Hexane extracted, from decoction, material having 55.17% and 92.62% of antituberculosis activity against SMtb and RMtb, respectively. Although the mycobactericidal activity of decoction is undetectable; its efficacy in extracting F. cernua active metabolites against M. tuberculosis is substantially greater than almost all pharmacognostic methods.

  13. Screening of extraction methods for glycoproteins from jellyfish ( Rhopilema esculentum) oral-arms by high performance liquid chromatography

    Science.gov (United States)

    Ren, Guoyan; Li, Bafang; Zhao, Xue; Zhuang, Yongliang; Yan, Mingyan; Hou, Hu; Zhang, Xiukun; Chen, Li

    2009-03-01

    In order to select an optimum extraction method for the target glycoprotein (TGP) from jellyfish ( Rhopilema esculentum) oral-arms, a high performance liquid chromatography (HPLC)-assay for the determination of the TGP was developed. Purified target glycoprotein was taken as a standard glycoprotein. The results showed that the calibration curves for peak area plotted against concentration for TGP were linear ( r = 0.9984, y = 4.5895 x+47.601) over concentrations ranging from 50 to 400 mgL-1. The mean extraction recovery was 97.84% (CV2.60%). The fractions containing TGP were isolated from jellyfish ( R. esculentum) oral-arms by four extraction methods: 1) water extraction (WE), 2) phosphate buffer solution (PBS) extraction (PE), 3) ultrasound-assisted water extraction (UA-WE), 4) ultrasound-assisted PBS extraction (UA-PE). The lyophilized extract was dissolved in Milli-Q water and analyzed directly on a short TSK-GEL G4000PWXL (7.8 mm×300 mm) column. Our results indicated that the UA-PE method was the optimum extraction method selected by HPLC.

  14. Natural colorants: Pigment stability and extraction yield enhancement via utilization of appropriate pretreatment and extraction methods.

    Science.gov (United States)

    Ngamwonglumlert, Luxsika; Devahastin, Sakamon; Chiewchan, Naphaporn

    2017-10-13

    Natural colorants from plant-based materials have gained increasing popularity due to health consciousness of consumers. Among the many steps involved in the production of natural colorants, pigment extraction is one of the most important. Soxhlet extraction, maceration, and hydrodistillation are conventional methods that have been widely used in industry and laboratory for such a purpose. Recently, various non-conventional methods, such as supercritical fluid extraction, pressurized liquid extraction, microwave-assisted extraction, ultrasound-assisted extraction, pulsed-electric field extraction, and enzyme-assisted extraction have emerged as alternatives to conventional methods due to the advantages of the former in terms of smaller solvent consumption, shorter extraction time, and more environment-friendliness. Prior to the extraction step, pretreatment of plant materials to enhance the stability of natural pigments is another important step that must be carefully taken care of. In this paper, a comprehensive review of appropriate pretreatment and extraction methods for chlorophylls, carotenoids, betalains, and anthocyanins, which are major classes of plant pigments, is provided by using pigment stability and extraction yield as assessment criteria.

  15. EXTRACTION AND QUANTITATIVE DETERMINATION OF ASCORBIC ACID FROM BANANA PEEL MUSA ACUMINATA ‘KEPOK’

    Directory of Open Access Journals (Sweden)

    Khairul Anwar Mohamad Said

    2016-04-01

    Full Text Available This paper discusses the extraction of an antioxidant compound, which is ascorbic acid or vitamin C, from a banana peel using an ultrasound-assisted extraction (UAE method. The type of banana used was Musa acuminata also known as “PisangKepok” in Malaysia. The investigation includes the effect of solvent/solid ratio (4.5, 5 g and 10  ml/g, sonication time (15, 30 and 45 mins and temperature variation (30 , 45  and 60oC on the extraction of ascorbic acid compounds from the banana peel to determine the best or optimum condition of the operation. Out of all extract samples analyzed by redox titration method using iodine solution, it was found that the highest yield was 0.04939 ± 0.00080 mg that resulted from an extraction at 30oC for 15 mins with 5 ml/g solvent-to-solute ratio.KEYWORDS:  Musa acuminata; ultrasound-assisted extraction; vitamin C; redox titration

  16. Algal Proteins: Extraction, Application, and Challenges Concerning Production

    Directory of Open Access Journals (Sweden)

    Stephen Bleakley

    2017-04-01

    Full Text Available Population growth combined with increasingly limited resources of arable land and fresh water has resulted in a need for alternative protein sources. Macroalgae (seaweed and microalgae are examples of under-exploited “crops”. Algae do not compete with traditional food crops for space and resources. This review details the characteristics of commonly consumed algae, as well as their potential for use as a protein source based on their protein quality, amino acid composition, and digestibility. Protein extraction methods applied to algae to date, including enzymatic hydrolysis, physical processes, and chemical extraction and novel methods such as ultrasound-assisted extraction, pulsed electric field, and microwave-assisted extraction are discussed. Moreover, existing protein enrichment methods used in the dairy industry and the potential of these methods to generate high value ingredients from algae, such as bioactive peptides and functional ingredients are discussed. Applications of algae in human nutrition, animal feed, and aquaculture are examined.

  17. Algal Proteins: Extraction, Application, and Challenges Concerning Production

    Science.gov (United States)

    Bleakley, Stephen; Hayes, Maria

    2017-01-01

    Population growth combined with increasingly limited resources of arable land and fresh water has resulted in a need for alternative protein sources. Macroalgae (seaweed) and microalgae are examples of under-exploited “crops”. Algae do not compete with traditional food crops for space and resources. This review details the characteristics of commonly consumed algae, as well as their potential for use as a protein source based on their protein quality, amino acid composition, and digestibility. Protein extraction methods applied to algae to date, including enzymatic hydrolysis, physical processes, and chemical extraction and novel methods such as ultrasound-assisted extraction, pulsed electric field, and microwave-assisted extraction are discussed. Moreover, existing protein enrichment methods used in the dairy industry and the potential of these methods to generate high value ingredients from algae, such as bioactive peptides and functional ingredients are discussed. Applications of algae in human nutrition, animal feed, and aquaculture are examined. PMID:28445408

  18. Portable Solid Phase Micro-Extraction Coupled with Ion Mobility Spectrometry System for On-Site Analysis of Chemical Warfare Agents and Simulants in Water Samples

    Directory of Open Access Journals (Sweden)

    Liu Yang

    2014-11-01

    Full Text Available On-site analysis is an efficient approach to facilitate analysis at the location of the system under investigation as it can result in more accurate, more precise and quickly available analytical data. In our work, a novel self-made thermal desorption based interface was fabricated to couple solid-phase microextraction with ion mobility spectrometry for on-site water analysis. The portable interface can be connected with the front-end of an ion mobility spectrometer directly without other modifications. The analytical performance was evaluated via the extraction of chemical warfare agents and simulants in water samples. Several parameters including ionic strength and extraction time have been investigated in detail. The application of the developed method afforded satisfactory recoveries ranging from 72.9% to 114.4% when applied to the analysis of real water samples.

  19. Portable Solid Phase Micro-Extraction Coupled with Ion Mobility Spectrometry System for On-Site Analysis of Chemical Warfare Agents and Simulants in Water Samples

    Science.gov (United States)

    Yang, Liu; Han, Qiang; Cao, Shuya; Yang, Jie; Yang, Junchao; Ding, Mingyu

    2014-01-01

    On-site analysis is an efficient approach to facilitate analysis at the location of the system under investigation as it can result in more accurate, more precise and quickly available analytical data. In our work, a novel self-made thermal desorption based interface was fabricated to couple solid-phase microextraction with ion mobility spectrometry for on-site water analysis. The portable interface can be connected with the front-end of an ion mobility spectrometer directly without other modifications. The analytical performance was evaluated via the extraction of chemical warfare agents and simulants in water samples. Several parameters including ionic strength and extraction time have been investigated in detail. The application of the developed method afforded satisfactory recoveries ranging from 72.9% to 114.4% when applied to the analysis of real water samples. PMID:25384006

  20. Combining Recurrence Analysis and Automatic Movement Extraction from Video Recordings to Study Behavioral Coupling in Face-to-Face Parent-Child Interactions.

    Science.gov (United States)

    López Pérez, David; Leonardi, Giuseppe; Niedźwiecka, Alicja; Radkowska, Alicja; Rączaszek-Leonardi, Joanna; Tomalski, Przemysław

    2017-01-01

    The analysis of parent-child interactions is crucial for the understanding of early human development. Manual coding of interactions is a time-consuming task, which is a limitation in many projects. This becomes especially demanding if a frame-by-frame categorization of movement needs to be achieved. To overcome this, we present a computational approach for studying movement coupling in natural settings, which is a combination of a state-of-the-art automatic tracker, Tracking-Learning-Detection (TLD), and nonlinear time-series analysis, Cross-Recurrence Quantification Analysis (CRQA). We investigated the use of TLD to extract and automatically classify movement of each partner from 21 video recordings of interactions, where 5.5-month-old infants and mothers engaged in free play in laboratory settings. As a proof of concept, we focused on those face-to-face episodes, where the mother animated an object in front of the infant, in order to measure the coordination between the infants' head movement and the mothers' hand movement. We also tested the feasibility of using such movement data to study behavioral coupling between partners with CRQA. We demonstrate that movement can be extracted automatically from standard definition video recordings and used in subsequent CRQA to quantify the coupling between movement of the parent and the infant. Finally, we assess the quality of this coupling using an extension of CRQA called anisotropic CRQA and show asymmetric dynamics between the movement of the parent and the infant. When combined these methods allow automatic coding and classification of behaviors, which results in a more efficient manner of analyzing movements than manual coding.

  1. Analysis of volatiles in silver carp by headspace solid phase micro-extraction coupled with GC-MS

    International Nuclear Information System (INIS)

    Yang Yuping; Xiong Guangquan; Cheng Wei; Liao Tao; Lin Ruotai; Geng Shengrong; Li Xin; Li Xiaoding; Wu Wenjin

    2010-01-01

    In this paper, a method for the determination of volatiles using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) was presented. The extraction conditions were optimized with reference to these volatiles as hexanal, heptanal, benzaldehyde, 1-Octen-3-ol, octanal, nonanal, decenal, 2,4-heptadienal and 2,4-decadienal. The extraction of fish muscle followed by incubation on a StableFlex divinyl benzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber during 50 in at 60 obtained the most effective extraction of the analytes. The methods by HS-SPME and GC-MS were effective in detecting volatiles in the gills, scales, viscera and fish muscles. The types of volatiles in the gill were more than other organs and the number of odors compounds was 63, and the number of volatiles in scales, viscera and fish muscles was 48, 44 and 42 respectively. (authors)

  2. Simultaneous extraction and determination of phthalate esters in aqueous solution by yolk-shell magnetic mesoporous carbon-molecularly imprinted composites based on solid-phase extraction coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Rui; Liu, Yuxin; Yan, Xiangyang; Liu, Shaomin

    2016-12-01

    A rapid, sensitive and accurate method for the simultaneous extraction and determination of five types of trace phthalate esters (PAEs) in environmental water and beverage samples using magnetic molecularly imprinted solid-phase extraction (MMIP-SPE) coupled with gas chromatography-mass spectrometry (GC-MS) was developed. A novel type of molecularly imprinted polymers on the surface of yolk-shell magnetic mesoporous carbon (Fe 3 O 4 @void@C-MIPs) was used as an efficient adsorbent for selective adsorption of phthalate esters based on magnetic solid-phase extraction (MSPE). The real samples were first preconcentrated by Fe 3 O 4 @void@C-MIPs, subsequently extracted by eluent and finally determined by GC-MS after magnetic separation. Several variables affecting the extraction efficiency of the analytes, including the type and volume of the elution solvent, amount of adsorbent, extraction time, desorption time and pH of the sample solution, were investigated and optimized. Validation experiments indicated that the developed method presented good linearity (R 2 >0.9961), satisfactory precision (RSD<6.7%), and high recovery (86.1-103.1%). The limits of detection ranged from 1.6ng/L to 5.2ng/L and the enrichment factor was in the range of 822-1423. The results indicated that the novel method had the advantages of convenience, good sensitivity, and high efficiency, and it could also be successfully applied to the analysis of PAEs in real samples. Copyright © 2016. Published by Elsevier B.V.

  3. Cloud point extraction coupled with microwave-assisted back-extraction (CPE-MABE) for determination of Eszopiclone (Z-drug) using UV-Visible, HPLC and mass spectroscopic (MS) techniques: Spiked and in vivo analysis.

    Science.gov (United States)

    Kori, Shivpoojan; Parmar, Ankush; Goyal, Jony; Sharma, Shweta

    2018-02-01

    A procedure for the determination of Eszopiclone (ESZ) from complex matrices i.e. in vitro (spiked matrices), as well as in vivo (mice model) was developed using cloud point extraction coupled with microwave-assisted back-extraction (CPE-MABE). Analytical measurements have been carried using UV-Visible, HPLC and MS techniques. The proposed method has been validated according to ICH guidelines and legitimate reproducible and reliability of protocol is assessed through intraday and inter-day precision UV-Visible techniques, corresponding to assessed linearity range. The coaservate phase in CPE was back extracted under microwaves exposure, with isooctane at pre-concentration factor ~50 when 5mL of sample solution was pre-concentrated to 0.1mL. Under optimized conditions i.e. Aqueous-Triton X-114 4% (w/v), pH4.0, NaCl 4% (w/v) and equilibrium temperature of 45°C for 20min, average extraction recovery has been obtained between 89.8 and 99.2% and 84.0-99.2% from UV-Visible and HPLC analysis, respectively. The method has been successfully applied to the pharmacokinetic estimation (post intraperitoneal administration) of ESZ in mice. MS analysis precisely depicted the presence of active N‑desmethyl zopiclone in impales as well as in mice plasma. Copyright © 2018 Elsevier B.V. All rights reserved.

  4. Simple and fast analysis of tetrabromobisphenol A, hexabromocyclododecane isomers, and polybrominated diphenyl ethers in serum using solid-phase extraction or QuEChERS extraction followed by tandem mass spectrometry coupled to HPLC and GC.

    Science.gov (United States)

    Li, Jian; Chen, Tian; Wang, Yuwei; Shi, Zhixiong; Zhou, Xianqing; Sun, Zhiwei; Wang, Dejun; Wu, Yongning

    2017-02-01

    Two simplified sample preparation procedures for simultaneous extraction and clean-up of tetrabromobisphenol A, α-, β-, and γ-hexabromocyclododecane and polybrominated diphenyl ethers in human serum were developed and validated. The first procedure was based on solid-phase extraction. Sample extraction, purification, and lipid removal were carried out directly on an Oasis HLB cartridge. The second procedure was a quick, easy, cheap, effective, rugged, and safe-based approach using octadecyl-modified silica particles as a sorbent. After sample extraction and cleanup, tetrabromobisphenol A/hexabromocyclododecane was separated from polybrominated diphenyl ethers by using a Si-based cartridge. Tetrabromobisphenol A and hexabromocyclododecane were then detected by high-performance liquid chromatography coupled to tandem mass spectrometry, while polybrominated diphenyl ethers were detected by gas chromatography coupled to tandem mass spectrometry. The results of the spike recovery test using fetal bovine serum showed that the average recoveries of the analytes ranged from 87.3 to 115.3% with relative standard deviations equal to or lower than 13.4 %. Limits of detection of the analytes were in the range of 0.4-19 pg/mL except for decabromodiphenyl ether. The developed method was successfully applied to routine analysis of human serum samples from occupational workers and the general population. Extremely high serum polybrominated diphenyl ethers levels up to 3.32 × 10 4 ng/g lipid weight were found in occupational workers. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Online turbulent flow extraction coupled with liquid chromatography-tandem mass spectrometry for high throughput screening of anabolic steroids in horse urine.

    Science.gov (United States)

    Shin, Hyun Du; Suh, Joon Hyuk; Kim, Junghyun; Cho, Hyun-Deok; Lee, Su Duk; Han, Kwan Seok; Wang, Yu; Han, Sang Beom

    2017-10-25

    A high throughput method for simultaneous screening of anabolic steroids and their metabolites (4-esterendione, trenbolone, boldenone, oxandrolone, nandrolone, methandrostenolone, testosterone, 1-androstendione, ethisterone, normethandrolone, methyltestosterone, 16β-Hydroxystanozolol, epitestosterone, bolasterone, norethandrolone, danazol, stanozolol and androstadienone) in equine urine by online turbulent flow extraction coupled with liquid chromatography-tandem mass spectrometry was developed. The use of turbulent flow chromatography could simplify pretreatment of horse urine, which has complex matrices as well as high viscosity. The urine was extracted by mixed-mode cation exchange solid phase extraction, and hydrolyzed using β-glucuronidase/arylsulfatase. Then, the sample was automatically loaded on the TurboFlow Cyclone extraction column for removal of further matrix, followed by separation on a fused core C18 column before MS/MS detection. Optimization and validation of the method were discussed in detail. All analytes were rapidly detected within 10min with high sensitivity (picogram to nanogram per milliliter level), and no interference was observed. The linearity range was from 0.1-10ng/mL for nine steroids and 1.0-50ng/mL for the others, with correlation of coefficient values over 0.995. Precision and accuracy ranged from 0.1 to 14.5% and 1.7 to 12.4%, respectively. The developed method was successfully applied to the analysis of anabolic steroids in horse urine after administration of a model drug. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Analysis of iminosugars and other low molecular weight carbohydrates in Aglaonema sp. extracts by hydrophilic interaction liquid chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Rodríguez-Sánchez, S; García-Sarrió, M J; Quintanilla-López, J E; Soria, A C; Sanz, M L

    2015-12-04

    A method by hydrophilic interaction liquid chromatography coupled to tandem mass spectrometry (HILIC-MS(2)) has been successfully developed for the simultaneous analysis of bioactive iminosugars and other low molecular weight carbohydrates in Aglaonema leaf extracts. Among other experimental chromatographic conditions, mobile phase eluents, additives and column temperature were evaluated in terms of retention time, resolution, peak width and symmetry provided for target carbohydrates. In general, narrow peaks (wh: 0.2-0.6min) with good symmetry (As: 0.9-1.3) and excellent resolution (Rs>1.8) were obtained for iminosugars using an acetonitrile:water gradient with 5mM ammonium acetate in both eluents at 55°C. Tandem mass spectra were used to confirm the presence of previously detected iminosugars in Aglaonema extracts and to tentatively identify for the first time others such as miglitol isomer, glycosyl-miglitol isomers and glycosyl-DMDP isomers. Concentration of total iminosugars varied from 1.35 to 2.84mgg(-1) in the extracts of the different Aglaonema samples analyzed. To the best of our knowledge, this is the first time that a HILIC-MS(2) method has been proposed for the simultaneous analysis of iminosugars and other low molecular weight carbohydrates of Aglaonema sp. extracts. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. [Determination of deoxynivalenol in grain and its products by solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Huang, Juan; Chen, Guosong; Zhang, Xiaoyan; Shen, Chongyu; Lü, Chen; Wu, Bin; Liu, Yan; Chen, Huilan; Ding, Tao

    2012-11-01

    A method was established for the determination of deoxynivalenol (vomitoxin) in grain and its products based on solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was firstly extracted by acetonitrile-water (84:16, v/v). The extract was then cleaned-up by an HLB solid phase extraction cartridge. The separation was carried out on a Phenomenex Kinetex C18 column (100 mm x4. 6 mm, 2.6 microm) with a gradient elution using 0.3% per hundred ammonia solution-acetonitrile as mobile phases. The analysis of deoxynivalenol was performed under electrospray negative ionization mode. The limit of detection (LOD, S/N= 3) and the limit of quantification (LOQ, S/N = 10) were 20 microg/kg and 50 microg/kg, respectively. A good linearity (r > 0.99) was achieved for the target compound over the range of 20-1000 pg/L. The recoveries at the three spiked levels (50, 100, 500 microg/kg) in the blank matrices such as flour, barley, soybean, rice, cornmeal, cassava and wheat, were varied from 75.6% to 111.0% with the relative standard deviations no more than 13. 0%. The method is accurate, efficient, sensitive and practical. The cost of pretreatment is obviously reduced by replacing immunoaffinity columns and Mycosep columns with HLB columns which have the same purification effect.

  8. Ultrasound Assisted Synthesis of 5,9-Dimethylpentadecane and 5,9-Dimethylhexadecane – the Sex Pheromones of Leucoptera coffeella

    Directory of Open Access Journals (Sweden)

    Fritz Duus

    2007-08-01

    Full Text Available Racemic 5,9-dimethylpentadecane and 5,9-dimethylhexadecane, the major and minor constituents, respectively, of the sex pheromone of Leucoptera coffeella, have been synthesized from citronellol in 56-58% overall yield through six steps. Ultrasound irradiation efficiently supported tosylation of alcohols (two steps as well as the subsequent cross coupling reactions with the pertinent Grignard reagents (also two steps.

  9. Extraction of Glycyrrhizic Acid from Glycyrrhiza uralensis Using Ultrasound and Its Process Extraction Model

    Directory of Open Access Journals (Sweden)

    Jiangqing Liao

    2016-10-01

    Full Text Available This work focused on the intensification of extraction process of glycyrrhizic acid (GA from Glycyrrhiza uralensis using ultrasound-assisted extraction (UAE method. Various process parameters such as ultrasonic power, ultrasonic frequency, extraction temperature, and extraction time which affect the extraction yield were optimized. The results showed that all process parameters had exhibited significant influences on the GA extraction. The highest GA yield of 217.7 mg/g was obtained at optimized parameters of 125 W, 55 kHz, 25 °C, and 10 min. Furthermore, the extraction kinetics model of this process was also investigated based on Fick’s first law available in the literature. Kinetic parameters such as equilibrium concentration (Ce and integrated influence coefficient (λ for different ultrasonic powers, ultrasonic frequencies, and extraction temperatures were predicted. Model validations were done successfully with the average of relative deviation between 0.96% and 4.36% by plotting experimental and predicted values of concentration of GA in extract. This indicated that the developed extraction model could reflect the effectiveness of the extraction of GA from Glycyrrhiza uralensis and therefore serve as the guide for comprehending other UAE process.

  10. Electromembrane extraction of amino acids from body fluids followed by capillary electrophoresis with capacitively coupled contactless conductivity detection

    Czech Academy of Sciences Publication Activity Database

    Strieglerová, Lenka; Kubáň, Pavel; Boček, Petr

    2011-01-01

    Roč. 1218, č. 37 (2011), s. 6248-6255 ISSN 0021-9673 R&D Projects: GA ČR GAP206/10/1219 Institutional research plan: CEZ:AV0Z40310501 Keywords : electromembrane extraction * biological samples * capillary electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.531, year: 2011

  11. Simultaneous determination of platinum group elements and rhenium in rock samples using isotope dilution inductively coupled plasma mass spectrometry after cation exchange separation followed by solvent extraction

    International Nuclear Information System (INIS)

    Shinotsuka, Kazunori; Suzuki, Katsuhiko

    2007-01-01

    A simple and precise determination method for platinum group elements (PGEs) and Re in rock samples was developed using isotope dilution coupled with inductively coupled plasma mass spectrometry (ID-ICP-MS). Cation exchange separation was employed for simplicity, because it is applicable to group separation and simultaneous isotopic measurement in contrast with the widely used anion exchange separation which entails separate elution. However, its application to ID-ICP-MS has been limited due to spectral interferences from impurities retained in the PGE fraction even after ion chromatography. To overcome this limitation, solvent extraction using N-benzoyl-N-phenylhydroxylamine (BPHA) in chloroform was successfully applied for further purification. After the examination of optimum experimental parameters in cation exchange separation and solvent extraction using synthetic PGE solution, the established procedure was applied to the determination of PGEs and Re in some geochemical reference materials. The obtained results agreed well with the literature data determined using the different digestion methods (NiS fire assay and the use of a high-pressure asher) within the analytical uncertainties of each other. Significant difference in reproducibility between Ru, Ir, Pt and Os group, and Pd and Re group was observed in the results for BHVO-2 and JA-2. By considering the error factors affecting analytical reproducibility, we concluded that the difference is ascribed to the sample heterogeneity of minor minerals enriched in Ru, Ir, Pt and Os

  12. Rapid and sensitive determination of phytosterols in functional foods and medicinal herbs by using UHPLC-MS/MS with microwave-assisted derivatization combined with dual ultrasound-assisted dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Sun, Jing; Zhao, Xian-En; Dang, Jun; Sun, Xiaoyan; Zheng, Longfang; You, Jinmao; Wang, Xiao

    2017-02-01

    In this work, a hyphenated technique of dual ultrasound-assisted dispersive liquid-liquid microextraction combined with microwave-assisted derivatization followed by ultra high performance liquid chromatography tandem mass spectrometry has been developed for the determination of phytosterols in functional foods and medicinal herbs. Multiple reaction monitoring mode was used for the tandem mass spectrometry detection. A mass spectrometry sensitive reagent, 4'-carboxy-substituted rosamine, has been used as the derivatization reagent for five phytosterols, and internal standard diosgenin was used for the first time. Parameters for the dual microextraction, microwave-assisted derivatization, and ultra high performance liquid chromatography tandem mass spectrometry were all optimized in detail. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect, extremely low limits of detection (0.005-0.015 ng/mL) and limits of quantification (0.030-0.10 ng/mL) were achieved. The proposed method was compared with previously reported methods. It showed better sensitivity, selectivity, and accuracy. The matrix effect was also significantly reduced. The proposed method was successfully applied to the determination of five phytosterols in vegetable oil (sunflower oil, olive oil, corn oil, peanut oil), milk and orange juice (soymilk, peanut milk, orange juice), and medicinal herbs (Ginseng, Ganoderma lucidum, Cordyceps, Polygonum multiflorum) for the quality control of functional foods and medicinal herbs. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Response of the rf-extraction-wing balcony and floor, and the storage ring to forced and ambient vibration excitation and coupling to tunnel/basemat

    International Nuclear Information System (INIS)

    Jendrzejczyk, J.A.; Wambsganss, M.W.; Smith, R.K.; Rosas-Velez, P.

    1993-08-01

    To ensure successful operation of the APS, vibration of the storage ring quadrupole magnets must be limited to very low levels for frequencies >10 Hz. There will be many sources of vibration, such as pumps, fans, compressors, generators, and other rotating and reciprocating machinery when the APS is operational. In general, such vibration sources are isolated from the structural components and base foundations by vibration dampers and isolators. Pumps are typically mounted on seismic isolators, which are massive bases with response frequencies of <10 Hz, and fans are mounted with elastic-type isolators to minimize vibration coupling. The attenuation of expansion/isolation joints is a very important factor in predicting the response of the storage ring basemat to the various excitation sources. Several 75-hp pumps are located on the balcony of the rf extraction wing, which is close to the storage ring basemat. The pumps per se may prove to be a vibration excitation source of concern. Additional pumps will be placed in the RF extraction building and could add to the vibration levels. If the dynamic unbalance force of the pump motor, and the efficiency of the associated expansion joints were known, one could predict the response of the storage ring basemat. This information would also be useful in determining the placement of additional pumps. This report discusses vibration tests and measurements that were performed on July 28, 1993, in the rf extraction building. The purpose of the investigation was to study the efficiency of two specific expansion joints: (1) the joint that separates a structural column pad from the extraction wing floor, and (2) the joint that separates the extraction wing floor from the roof of the storage ring tunnel. A small electrodynamic exciter, with a maximum RMS force output of ∼0.5 lb at the frequencies of interest, was used

  14. Extraction of hyaluronic acid (HA) from rooster comb and characterization using flow field-flow fractionation (FlFFF) coupled with multiangle light scattering (MALS).

    Science.gov (United States)

    Kang, Dong Young; Kim, Won-Suk; Heo, In Sook; Park, Young Hun; Lee, Seungho

    2010-11-01

    Hyaluronic acid (HA) was extracted in a relatively large scale from rooster comb using a method similar to that reported previously. The extraction method was modified to simplify and to reduce time and cost in order to accommodate a large-scale extraction. Five hundred grams of frozen rooster combs yielded about 500 mg of dried HA. Extracted HA was characterized using asymmetrical flow field-flow fractionation (AsFlFFF) coupled online to a multiangle light scattering detector and a refractive index detector to determine the molecular size, molecular weight (MW) distribution, and molecular conformation of HA. For characterization of HA, AsFlFFF was operated by a simplified two-step procedure, instead of the conventional three-step procedure, where the first two steps (sample loading and focusing) were combined into one to avoid the adsorption of viscous HA onto the channel membrane. The simplified two-step AsFlFFF yielded reasonably good separations of HA molecules based on their MWs. The weight average MW (M(w) ) and the average root-mean-square (RMS) radius of HA extracted from rooster comb were 1.20×10(6) and 94.7 nm, respectively. When the sample solution was filtered through a 0.45 μm disposable syringe filter, they were reduced down to 3.8×10(5) and 50.1 nm, respectively. Copyright © 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Determination of nonylphenol isomers in landfill leachate and municipal wastewater using steam distillation extraction coupled with comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry

    Science.gov (United States)

    Zhang, Caixiang; Eganhouse, Robert P.; Pontolillo, James; Cozzarelli, Isabelle M.; Wang, Yanxin

    2012-01-01

    4-Nonylphenols (4-NPs) are known endocrine disruptors and by-products of the microbial degradation of nonylphenol polyethoxylate surfactants. One of the challenges to understanding the toxic effects of nonylphenols is the large number of isomers that may exist in environmental samples. In order to attribute toxic effects to specific compounds, a method is needed for the separation and quantitation of individual nonylphenol isomers. The pre-concentration methods of solvent sublimation, solid-phase extraction or liquid–liquid extraction prior to chromatographic analysis can be problematic because of co-extraction of thousands of compounds typically found in complex matrices such as municipal wastewater or landfill leachate. In the present study, steam distillation extraction (SDE) was found to be an effective pre-concentration method for extraction of 4-NPs from leachate and wastewater, and comprehensive two-dimensional gas chromatography (GC × GC) coupled with fast mass spectral data acquisition by time-of-flight mass spectrometry (ToFMS) enhanced the resolution and identification of 4-NP isomers. Concentrations of eight 4-NP isomers were determined in leachate from landfill cells of different age and wastewater influent and effluent samples. 4-NP isomers were about 3 times more abundant in leachate from the younger cell than the older one, whereas concentrations in wastewater effluent were either below detection limits or <1% of influent concentrations. 4-NP isomer distribution patterns were found to have been altered following release to the environment. This is believed to reflect isomer-specific degradation and accumulation of 4-NPs in the aquatic environment.

  16. Determination of occluded oxygen, nitrogen and hydrogen in zircalloy-4 by vacuum extraction coupled to gas chromatography

    International Nuclear Information System (INIS)

    Vega, O.; Imakuma, K.

    1983-01-01

    The technique of vacuum extraction at high temperatures was used for the liberation of gases from zircalloy-4 samples; oxygen, nitrogen and hydrogen were quantitatively analysed by gas chromatography. Two different sets of zircalloy-4 samples were examined. The results for O 2 , N 2 and H 2 quantitative analyses satisfy the requirements for the characterization of the zircalloy-4 quality. (C.L.B.) [pt

  17. Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

    Directory of Open Access Journals (Sweden)

    Đurović-Pejčev Rada

    2016-01-01

    Full Text Available A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME in combination with liquid-solid sample preparation (LS was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl content was perfor-med using 100 μm polydimethyl-siloxane (PDMS fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS was used for detection and quantification, obtaining relative standard deviation (RSD below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 μg kg-1 of each herbicide. Limits of detection (LOD were less than 1.2 μg kg-1 for all the studied herbicides. [Projekat Ministarstva nauke Republike Srbije, br. TR31043 i br. III43005

  18. Method validation for determination of metals in Vitis labrusca L. grapevine leaf extracts by inductively coupled plasma mass spectrometry (ICP-MS

    Directory of Open Access Journals (Sweden)

    LIANE V.V. BOKOWSKI

    Full Text Available ABSTRACT Vitis labrusca L. is the main species used for wine and juice production in Brazil. The grapevine leaves can be used both as functional foods and as cheapest sources for the extraction of phenolic compounds. Besides the antioxidant activity, grapevine leaves exhibited significant anti-inflammatory activity. Therefore, the aim of this study was to develop and validate an analytical methodology to determine the metals selenium (96Se, chromium (53Cr, nickel (62Ni, cadmium (111Cd and lead (206Pb in 30 samples of grapevine leaf extracts (Vitis labrusca, Bordo cultivar using inductively coupled plasma mass spectrometry (ICP-MS. To obtain the grapevine leaf extracts the samples were milled, weighed and digested in microwave oven with nitric acid. The method showed linearity, precision, accuracy and limits of quantification and detection acceptable for INMETRO protocol validation of analytical methods. Therefore, the method using ICP-MS was developed and validated to determine metals concentrations in grapevine leaves of Vitis labrusca L. and the proposed method could be applied in routine analytical laboratory.

  19. Ultra-trace determination of Persistent Organic Pollutants in Arctic ice using stir bar sorptive extraction and gas chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Lacorte, S; Quintana, J; Tauler, R; Ve